Article

A rapid method for the determination of mycotoxins in edible vegetable oils by ultra-high performance liquid chromatography-tandem mass spectrometry

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Abstract

An analytical method based on a QuEChERS procedure (quick, easy, cheap, effective, rugged and safe) has been developed for the determination of mycotoxins (α-zearalenol and zearalenone, and aflatoxins B1, B2, G1 and G2) in edible oils. The analysis was performed by ultra-high performance liquid chromatography coupled to triple quadrupole analyser (UHPLC-QqQ-MS/MS). The method was fully validated and the quantification limit is 0.5 μg kg ⁻¹ for aflatoxins and 1 μg kg ⁻¹ for α-zearalenol and zearalenone. Suitable recoveries were obtained at low concentration levels (0.5–25 μg kg ⁻¹ for aflatoxins and 1–25 μg kg ⁻¹ for α-zearalenol and zearalenone), ranging from 80 to 120%. Intra and inter-day precision values were also evaluated and relative standard deviation was lower than 20%. The expanded uncertainty, U, was also evaluated ant it was below 32% at 25 µg kg ⁻¹ . The validated method has been applied to monitor the presence of mycotoxins in 194 samples belonging to different types of edible oils (olive oil, sunflower oil, soy oil and corn oil). Zearalenone was detected in 25% of the analysed samples at concentrations up to 25.6 μg kg ⁻¹ , and aflatoxin G1 and G2 in 3% and 14% of the samples at a maximum concentration of 1.9 and 6.8 μg kg ⁻¹ respectively.

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... Thus, the validity, confirmation, detection, and determination of contaminants are significant issues that must be considered. The Food and Agriculture Organization of the United Nations (FAO) has estimated that >25 % of all agricultural products are contaminated with mycotoxins and that aflatoxins (AFs) are the most common among them (Hidalgo-Ruiz et al., 2019). The four types of AFs (AFG1, AFB1, AFG2, and AFB2) are secondary metabolites that are produced by fungi, including Aspergillus parasiticus and A. flavus, which vastly contaminate agricultural products (Yu et al., 2019). ...
... In addition to the soil, harvesting, and packaging conditions of oilseeds, several studies have highlighted the contamination of vegetable oils by mycotoxins because of certain storage conditions, including high temperatures and relative humidity, which are considered ideal and favorable for fungal reproduction and mycotoxin production (European Food Safety Authority (EFSA, 2020). The presence of mycotoxins affects oil quality (Bahrami et al., 2016;Bhat and Reddy, 2017;Hidalgo-Ruiz et al., 2019). The contaminant levels in edible oil depend on the raw materials used during production, which are often stored for weeks under unacceptable conditions; this may lead to mold growth and mycotoxin production, including AFs. ...
... LOQs for AFs ranged from 0.2 to 0.4 μg kg − 1 , whereas LODs ranged from 0.07 to 0.11 μg kg − 1 (Table 2), indicating the adequate sensitivity and fitness of purpose. The method sensitivity concerning the LOQ of the targeted AFs was similar to that proposed by Hidalgo-Ruiz et al. (2019) and ranged between 0.5 and 1.0 μg kg − 1 using ultra HPLC-MS/MS, which was performed to determine AFs in edible vegetable oils. LOQs in this study was also comparable to those reported in other recent studies; one study determined the occurrence of AFs in Table 1 Aflatoxins G1, B1, G2 and B2 fraction profile by gel permeation chromatography (GPC), μg kg -1 . ...
Article
Aflatoxins (AFs) are among the most toxic contaminants that are present in nuts, grains, seeds, and spices. This study developed a selective and reliable method to determine AFs in edible vegetable oils. In addition, the health risk assessments of AFs owing to the consumption of contaminated edible vegetable oils were estimated using the margin of exposure (MOE) approach in Egyptians. Size exclusion chromatography was performed for the selective extraction of AFs from oils. AFs were quantified via precolumn derivatization, followed by high-performance liquid chromatography with a fluorescence detector (HPLC-FLD). The method was tested for validation parameters and was found to fit its selective and intended use. The limit of quantification (LOQ) values for AFG1, AFB1, AFG2, and AFB2 were 0.3, 0.3, 0.4, and 0.2 µg kg⁻¹, respectively; the corresponding values for the limit of detection (LOD) were 0.08, 0.08, 0.11, and 0.07 µg kg⁻¹, respectively. The test method was applied to determine AFs in 90 randomly collected edible vegetable oil samples from 4 Egyptian governorates. The results showed that 5.6% of the samples were contaminated with AFB1 (average concentration, 3.56 ± 2.50 µg kg⁻¹). The estimated daily intakes of AFB1 from sunflower, corn, and mixed oils were 0.00047, 0.00571, and 0.30384 ng kg⁻¹ body weight (bw) day⁻¹, respectively, and the corresponding MOE values were 361,702, 29,750, and 560 ng kg⁻¹ bw day⁻¹, respectively. The MOE results suggested that the situation represents a health concern regarding the consumption of mixed oils and that essential measures should be taken to protect public health. However, no harmful effects from the consumption of sunflower and corn oils were observed. This is the first study to investigate AFs in edible vegetable oils and assess their health risk in Egypt.
... Virgin olive oils can be contaminated by mycotoxins and because of chemical and thermal stability of these toxins, the contaminations remain during food processing such as cooking and frying (Afzali et al. 2012;Agriopoulou et al. 2020). Literature review supports the presence of mycotoxins in olive and olive oil (Daradimos et al. 2000;Papachristou and Markaki 2004;Finoli et al. 2005;Roussos et al. 2006;Ghitakou et al. 2006;Cavaliere et al. 2007;Ferracane et al. 2007;Ben Rejeb et al. 2009;Bao et al. 2010;Markaki 2010;Alamprese 2014;Nabizadeh et al. 2018;Hidalgo-Ruiz et al. 2019). Presence of AFs in olive and consequently extracted oil may raise consumer concerns regarding safety of these products; therefore, monitoring of these contaminants is important. ...
... I 2 which measures statistical heterogeneity was obtained 94.96% for AFB 1 in olive oil with P value of \ 0.05 which shows the highly severe heterogeneity (Higgins and Thompson 2002). Studies with the prevalence value of zero for aflatoxin B 1 were excluded from meta-analysis (Zhao et al. 2017a;Nabizadeh et al. 2018;Hidalgo-Ruiz et al. 2019;Yu et al. 2019). Length of the line in the forest plot is inversely related to the sample size. ...
... Conversely, OTA was reported in 88% of olive oil from different origin of producers and marketplaces in Greece (Papachristou and Markaki 2004). When olives are deposited for a couple of days in environments which support the mold growth, mycotoxin contamination may occur (Ben Rejeb et al. 2009;Alamprese 2014;Tantaoui-Elaraki et al. 2018;Hidalgo-Ruiz et al. 2019). Issues related to quality control, inappropriate production technologies, hot climate and improper storage conditions support the growth of mold and development of mycotoxins, resulting in the more frequent incidence of mycotoxin contamination of food in developing countries (Agriopoulou et al. 2020). ...
Article
Olive oil can be contaminated by fungal toxins; therefore, it is necessary to monitor the incidence of mycotoxins in this oil. In the present study, the pooled prevalence of detectable aflatoxin B1 (AFB1) in olive oil was evaluated using systematic review and meta-analysis approach from 1 January 1991 to 31 December 2020 (30 years study). The search was conducted via electronic databases involving Scopus, Web of Science, PubMed, Agris and Agricola. Synonyms were collected from combination of the MESH, Agrovoc and free text method. After screening and selection process of primary researches, full texts of eligible researches (46 studies) were evaluated and data of the nine studies as included researches were extracted. Random effect model was used to estimate the pooled prevalence of AFB1 in olive oil and weighing model of Dersimonian–Laired was applied. Summary measure of mycotoxin prevalence was estimated using Metaprop module of STATA and 95% confidence interval (CI) were calculated using the Binomial Exact Method. Pooled prevalence of AFB1 in olive oils were 32% (95% CI 8–56%) which means that 68% of olive oil were free of detectable contaminants of AFB1. Due to controversy over the results of primary studies, future researches and consequent subgroup analysis based on the main variables affecting the aflatoxins contamination in olive oil are recommended to achieve the conclusive results.
... Oil is an important ingredient used in the preparation of foods [8], with edible oils being processed from various grains, such as soybean, rapeseed, sunflower seed, peanut, and olive [9]. The processed edible oils can easily become contaminated by mycotoxins originating in the seed before the crop has been harvested to produce their oils [10]. Oil from olives (Olea europaea L.) is a major product of the west coast USA, Turkey, Spain, Greece, Italy, and Morocco. ...
... Contamination by aflatoxins (AFs) and ochratoxin A (OTA) is common in olive oil [4]. Hidalgo-Ruiz et al. [10] reported that 153 olive oil samples in Spain were contaminated by zearalenone (ZEA; 0.6-21.1 µg/kg), aflatoxin G1 (AFG1; 1.1-6.8 µg/kg), and aflatoxin G2 (AFG2; 0.8-1.9 ...
... The QuEChERS procedure was modified from [8,10]. Briefly, 2 g of oil sample was added to 2 mL of Milli-Q water and mixed for 1 min using a vortex mixer. ...
Article
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The prevalence of mycotoxins is often increased by the climatic conditions prevailing in tropical regions. Reports have revealed the contamination of mycotoxins in some types of vegetable oil. However, vegetable oil is one of the essential ingredients used in food preparation. Thus, this study determined the occurrence of multi-mycotoxins in six types of vegetable oils commercially available in Thailand to assess the consumer health risk. In total, 300 vegetable oil samples (olive oil, palm oil, soybean oil, corn oil, sunflower oil, and rice bran oil) collected from various markets in Thailand were analyzed for the presence of nine mycotoxins, namely, aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2), beauvericin (BEA), ochratoxin A (OTA), zearalenone (ZEA), fumonisin B1 (FB1), and fumonisin B2 (FB2) using a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based procedure and a triple quadrupole mass spectrometer equipped with an electrospray ionization source. The incidences of mycotoxin contamination varied among the different types of oil samples. AFB1, AFB2, ZEA, FB1, and FB2 were most frequently found in contaminated samples. AFB2, BEA, ZEA, FB1, and FB2 contaminated olive oil samples, whereas AFB1, AFB2, AFG2, and OTA contaminated palm oil samples. AFB1, AFB2, and ZEA were found in soybean oils, whereas ZEA, FB1, and FB2 contaminated corn oil samples. AFB1 and AFG1 contaminated sunflower oil samples, whereas AFB1, AFB2, AFG1, and OTA were detected in rice bran oil samples. However, the contamination levels of the analyzed mycotoxins were below the regulatory limits.
... This hypothesis is strengthened by the detection of aflatoxins and ochratoxin A in olive oil. However, in most of the studies, aflatoxins are detected at low concentrations or traces, more sensitive analytical methods with low LODs show considerable more positive samples (Bircan, 2006;Cavaliere et al., 2007;Hidalgo-Ruiz et al., 2019;Nabizadeh et al., 2018;Papachristou & Markaki, 2004;Waqas et al., 2021;Zhang & Xu, 2019). Also, ochratoxin A could be successfully detected in 44 of 50 olive oil samples with a maximum concentration of 1.03 μg/kg (Papachristou & Markaki, 2004). ...
... To our knowledge, there are no data concerning the contamination of mycotoxins in olive mill solid residue itself. In olive pomace oil, aflatoxin G2 was found in levels up to 6.8 μg/kg (Hidalgo-Ruiz et al., 2019). However, Aspergillus flavus strains producing aflatoxin B1 in vitro and Aspergillus niger strains producing ochratoxin A in vitro could be isolated from olive cake made of spoiled olives (Roussos et al., 2006). ...
Article
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Among the most important agro-industrial activities in the Mediterranean basin, olive oil production has a high impact on the economy of many Mediterranean countries. However, olive oil extraction generates huge quantities of byproducts, including leaves, pomace residues, stones and wastewater, which have severe environmental impacts mainly because of their phytotoxicity and great organic content. Olive oil byproducts are regarded as inexpensive and abundant raw materials rich in bioactive compounds with high and varied health-related activities. Several phenolic compounds and terpenoids were recovered from olive byproducts using different conventional and advanced extraction methods due to their potential to be used in food, packaging, pharmaceutical, and cosmetic industries. Recently, the use of olive byproducts and their functional compounds to enhance the functional properties of packaging systems was investigated as a sustainable strategy for food preservation, fostering the sustainability of the olive-oil chain, and promoting circular economy. In this framework, the main goals of this review are to summarize the main bioactive compounds in olive byproducts, to review the main advancements in their extraction, purification, and characterization, and finally to discuss their applications in food packaging systems as well as safety-related aspects.
... However, the occurrence of mycotoxins is one of the chemical hazards that potentially threatens the safety of these products. In this regard, aflatoxins B 1 , G 1 , B 2 and G 2 in the peanut and coconut oils and zearalenone (ZEN) in maize germ oil have raised more concerns than other mycotoxins (Hidalgo-Ruiz et al., 2019;Van Duijn, 2014). ...
... Maize oil samples were artificially spiked with 50, 100 and 200 µg/l of ZEN which are 0.125, 0.250 and 0.500 times the maximum limit set by the European Commission for refined maize oil (400 µg/kg), respectively (Hidalgo-Ruiz et al., 2019). Aliquots of maize oil (~ 200 ml) were then removed and processed by three different cooking techniques, including microwaving, deep-frying and oven-cooking. ...
Article
Mycotoxins are one of the most common types of chemical hazards related to edible oils. Although the refining process can remove such contaminations, they may still be present in the final oils due to defects during the refining steps. In addition, most oils produced in local manufactories are not refined and as such may be contaminated with mycotoxins. However, the effect of various cooking methods on the stability of mycotoxins in edible oils has rarely been studied. Hence, this study evaluated the impact of microwave, deep frying and oven cooking on the degradation of spiked zearalenone (50, 100 and 200 μg/l) in maize oil. Measurements were done by high performance liquid chromatography-fluorescence detection. The results showed that the majority of treatments, including time-temperature combinations of frying (130-190 °C for 2.5 and 5 min), oven cooking (110-230 °C for 2.5 and 5 min) and exposure time of microwave (2.5, 5 and 10 min) reduced zearalenone levels. Microwave cooking of samples containing 200 μg/l of zearalenone for 10 min showed the highest degradation of the toxin (~ 38%) following first order kinetics. The extent of destruction achieved by frying and oven cooking was also dependent on the initial concentration of zearalenone. These findings can be helpful to evaluate the chemical safety of edible oils or foods prepared by them.
... The AFG1 values range from 0 to 3.50 ng/g for peanut oils produced in Bobo Dioulasso with an average of 0.70 ng/g. For peanut oils produced in Ouagadougou-Saaba, values range from 0 to 2.37 ng/g with an average of 0. 39 average of 0.17 ng/g. The AFG1 was not detected in cottonseeds oils produced in Ouagadougou-Pabré. ...
... Maximum levels of mycotoxins in food and feed not to be exceeded have been accepted but vary from country to country [38]. However, there are no legal limits for aflatoxins in all edible oils, although they have been set in oilseeds, i.e. 2.0 µg/kg for AFB1 and 4.0 µg/kg for the sum of the four aflatoxins (B1+B2+G1+G2) [39]. In view of their hazard to the health of the consumer, it is possible to eliminate them. ...
Article
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Aim: The study aim was to assess aflatoxin and moisture levels in edible oils produced and consumed in Burkina Faso to know the impact on consumer health. Methodology: A total of 61 samples of refined cottonseeds oils and crude peanut oils were collected from Ouagadougou, Bobo Dioulasso and surrounding areas. Aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2) were determined by HPLC and moisture by differential weighing after oven drying. Results: The moisture content of peanut oils were ranged from 0.06 to 0.18% and cottonseeds oils from 0.02 to 0.17%. The moisture average is 0.13% for peanut oils and 0.08% for cottonseeds oils (P<0.05). The moisture of all oils is lower and conform to the Codex Alimentarius standard. AFB1, AFB2, AFG1 and AFG2 were identified in 86.89% of the oil samples analyzed. The proportion of samples contaminated with AFB1 is 57.38%, 59.02% for AFB2, 42.62% for AFG1 and 65.57% for AFG2. The AFB1 average of peanut oils is 6.21 ng/g while that of cottonseeds oils is 0.03 ng/g.The AFB2 average of peanut oils is 0.89 ng/g against 0.04 ng/g for cottonseeds oils (P<0.05). The AFG1 average of peanut oils is 0.54 ng/g and 0.08 ng/g for cottonseeds oils (P<0.05). The AFG2 average of peanut oils was 0.66 ng/g against 0.64 ng/g for cottonseeds oils. AFG2 had the highest proportion of all oils while AFB1 has the highest concentration and proportion in peanut oils. The 72.13% samples analyzed in this study comply with the European Community standard for aflatoxin B1 level maximum in oilseeds. Conclusion: Aside from the moisture content that comply with the standard, aflatoxins are present at varying levels and can negatively impact the consumer health. It is important to strengthen the monitoring and production system in order to have quality oil.
... A previous extraction method based on QuEChERS method has been tested for the determination of mycotoxins in nuts (Hidalgo-Ruiz et al., 2019). Whereas the LC-MS procedure has been the same, the extraction procedure was slightly modified. ...
Article
A method was developed for the determination of 6 mycotoxins (α-zearalenol and zearalenone, and aflatoxins B1, B2, G1 and G2) in nuts. For that purpose, a QuEChERS based method (quick, easy, cheap, effective, rugged and safe) procedure has been used as well as ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS). Peanuts was selected as representative matrix after checking several matrices (almonds, hazelnuts, peanuts, pistachios and walnuts). Thus, a quantification strategy of mycotoxins in nuts has been stablished using only one matrix. The method was also fully validated and the quantification limit was set at 0.5 μg kg⁻¹ for the four aflatoxins and 1 μg kg⁻¹ for α-zearalenol and zearalenone. Appropriate recoveries were obtained at low concentration levels (0.5, 10 and 25 μg kg⁻¹), ranging from 80 to 120%. Intra and inter-day precision values, expressed as relative standard deviation, were lower than 20%. Expanded uncertainty was also estimated and it was below 42%. To check the applicability of the method, it has been applied to 36 samples of different types of nuts, such as almonds, hazelnuts, peanuts, pistachios and walnuts. Aflatoxin G2 was detected in 40% of the analysed samples at concentrations up to 6.3 μg kg⁻¹.
... A similar procedure to HPLC, UHPLC or UPLC is also used on the column to improve the resolution of AFB 1 . Hidalgo et al. [100] developed a new analytical method by coupling UHPLC to a triple quadrupole analyzer (UHPLC-QqQ-MS/MS), which was well validated and applied to monitor mycotoxins, including AFB 1 , in 194 samples of edible vegetable oil. ...
Article
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Contamination of agricultural products and foods by aflatoxin B1 (AFB1) is becoming a serious global problem, and the presence of AFB1 in edible oil is frequent and has become inevitable, especially in underdeveloped countries and regions. As AFB1 results from a possible degradation of aflatoxins and the interaction of the resulting toxic compound with food components, it could cause chronic disease or severe cancers, increasing morbidity and mortality. Therefore, rapid and reliable detection methods are essential for checking AFB1 occurrence in foodstuffs to ensure food safety. Recently, new biosensor technologies have become a research hotspot due to their characteristics of speed and accuracy. This review describes various technologies such as chromatographic and spectroscopic techniques, ELISA techniques, and biosensing techniques, along with their advantages and weaknesses, for AFB1 control in edible oil and provides new insight into AFB1 detection for future work. Although compared with other technologies, biosensor technology involves the cross integration of multiple technologies, such as spectral technology and new nano materials, and has great potential, some challenges regarding their stability, cost, etc., need further studies.
... spectrometric (MS) detection [11,12]. For example, highperformance liquid chromatography (HPLC) coupled with fluorescence [13,14] or MS detection [15,16] have been described for ZEA detection. Although chromatographic analysis is very accurate and reproducible, its practical use is limited by its high cost and sluggishness. ...
Article
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The development of a bioluminescent immunosensor is reported for the determination of zearalenone (ZEA) based on a peptide mimetic identified by phage display. The peptide mimetic GW, with a peptide sequence GWWGPYGEIELL, was used to create recombinant fusion proteins with the bioluminescent Gaussia luciferase (GLuc) that were directly used as tracers for toxin detection in a competitive immunoassay without the need for secondary antibodies or further labeling. The bioluminescent sensor, based on protein G–coupled magnetic beads for antibody immobilization, enabled determination of ZEA with a detection limit of 4.2 ng mL⁻¹ (corresponding to 420 μg kg⁻¹ in food samples) and an IC50 value of 11.0 ng mL⁻¹. The sensor performance was evaluated in spiked maize and wheat samples, with recoveries ranging from 87 to 106% (RSD < 20%, n = 3). Finally, the developed method was applied to the analysis of a naturally contaminated reference matrix material and good agreement with the reported concentrations was obtained. Graphical abstract
... (classified within fatty fish, lean fish, or crustaceans). This approach has been previously reported for emerging contaminants, for instance in foodstuff (Díez et al., 2016;Hidalgo-Ruiz et al., 2019;Tao et al., 2018) and wine (Berset et al., 2017). Both matrix-specific variations of extraction efficiencies (recovery) and ionization (LC-MS matrix effects) should be compensated in our case since matrix-matched curves are submitted to the entire procedure, rather than adding native analytes and internal standards post extraction. ...
Article
Freshwater and marine seafood products purchased in Montreal, Canada, were screened for diverse veterinary drug residues including sulfonamides and potentiators, macrolides, lincosamides, nitrofurans, nitroimidazoles, amphenicols, quinolones and fluoroquinolones, one triphenylmethane dye and its leuco-metabolite, and tetracyclines. QuEChERS extraction ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was validated in three model matrices (fatty fish, lean fish, and shrimp edible meat). Method detection limits were in the range of 0.002–3 μg/kg, and the accuracy of matrix-matched extracted calibrants was generally within acceptance criteria. The aquaculture or wild-caught samples of pangasius (basa), cod, salmon, sole, tilapia, trout, white shrimp and giant tiger prawn originated from Canada, China, India, Southeast Asia (Indonesia, Thailand, Vietnam), and other regions worldwide. Overall, 38 % of the tested fish and shrimp samples had detectable residues of at least one veterinary drug or metabolite, and 25 % were not compliant to Canadian guidelines. Leucomalachite green was detected across various sample types (detection frequency: 13 %; maximum: 0.9 μg/kg). Other detected compounds (2–11 % of samples) included tetracycline (maximum: 36 μg/kg), 4-epi-oxytetracycline (18 μg/kg), oxytetracycline (13 μg/kg), metronidazole (13 μg/kg), sulfamethazine (4.8 μg/kg), sulfamethoxazole (4.2 μg/kg), trimethoprim (0.59 μg/kg), florfenicol (0.27 μg/kg), flumequine (0.21 μg/kg), enrofloxacin (1.6 μg/kg), and ofloxacin (0.52 μg/kg).
... One of the challenges for researchers to confront in the determination of mycotoxins in cashew nuts is the high fat content and limitation of mycotoxins at trace levels (Cunha et al., 2018;Hidalgo-Ruiz et al., 2019a). In recent years, several analytical methods have been developed to solve the mentioned problems in which mass spectrometry (MS) detection has widely used owing to its high selectivity and sensitivity (Dong et al., 2019;Giang and Thien, 2020;Wang et al., 2018). ...
Article
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The rising demand in cashew-nut consumption has become a concern worldwide due to mycotoxin-contamination-related health risks. Here, we optimized an analytical method for the measurement of 18 mycotoxins in commercial cashew nuts from Vietnam. We hypothesized that nuts contained more additives also consisted of higher mycotoxin concentration. The UPLC–MS/MS system based on the QuEChERS protocol was utilized for evaluating different solid phase extraction materials. Best analyte resolution was obtained using MeOH in combination with NH4F. Moreover, performance of the C18-MAX-MCX extraction materials was most outstanding, resulting in >70% recoveries and <13% RSD in most compounds. Fumonisin B1 remarkably varied among food of different seasoning techniques in which those nuts containing the most additives also consisted of highest toxin. Yet no significant difference in deoxynivalenol concentration was detected. Additive compositions, preservation conditions, and heat-resistance attribute were key factors to the occurrence of mycotoxin in cashew nuts.
... However, most commonly used methodes require sample preparation (extraction and clean up), steps to separate the mycotoxins from the oil. The liquid-liquid extraction or partitioning (LLE) (Idris et al., 2010;Majerus et al., 2009;Zhu et al., 2015), solid-phase extraction (SPE) (Drzymala et al., 2015;Ferracane et al., 2007;Han et al., 2019), immune-affinity columns (IAC) (Karunarathna et al., 2019;Yang et al., 2011), multifunctional cleanup columns , IAC combined with dispersive liquid-liquid microextraction (DLLME) (Afzali et al., 2012), Quick, Easy, Cheap, Effective, Rugged, and Safe (QuECh-ERS) (Hidalgo-Ruiz et al., 2019;Sharmili et al., 2016;Zhao, Wan, et al., 2017), and gel permeation chromatography (GPC) (Qian et al., 2015) are frequently reported among literature. A food sample preparation technique depends on mycotoxin's characteristics, food matrix type, and detection technique (Alshannaq & Yu, 2017). ...
Article
Background: Edible vegetable oils usually make up at least 30% of the human daily diet, provide calories and essential fatty acids for the body, and make food palatability. However, edible oils are susceptible to mycotoxins as a severe threat to human health. Oilseeds are prone to contamination with various mycotoxins if stored for a long time in inappropriate storage conditions such as high temperature and humidity, which can eventually be transmitted to the extracted oil. Scope and approach: This review intends to summarize the studies published to date regarding the prevalence, toxicity, and methods used to detect and decontaminate the main mycotoxins in edible vegetable oils. Key findings and conclusions: Among the 14 types of oils discussed in the current review, the main mycotoxins in oils were aflatoxins, zearalenone, ochratoxin A, trichothecenes, fumonisins, and Alternaria toxins with a predominance of aflatoxins. Mycotoxins' prevalence varied in different edible oils depending on the type of oil, geographical area, analysis method, and oilseeds' storage conditions. A broad range of methods was used to detect mycotoxins in oils, while the most applied was the HPLC coupled with fluorescence detection, followed by HPLC coupled with tandem mass spectrometry, gas chromatography, enzyme-linked immunosorbent assay, aptamer, and surface plasmon resonance. The lowest detection limit with excellent sensitivity and selectivity was associated with LC-MS/MS, although it depends on the sample preparation method. Moreover, mycotoxins decontamination techniques for edible oils were alkaline electrolyzed water, irradiation, magnetic adsorbents, and enzymatic methods, while the most effective method was alkaline electrolyzed water.
... Sample preparation is of primary importance in mycotoxin determination because it affects every chromatographic determination. The most common solvents used for the extraction of mycotoxins from foodstuff are methanol-water and acetonitrile-water [26,28,30]. In addition, other solvents, such as acetone [31,32], ethyl acetate [33,34] and chloroform [35,36], are also used for mycotoxin extraction. ...
Article
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Penicillium spp. are emerging as producers of mycotoxins and other toxic metabolites in nuts. A HPLC-MS/MS method was developed to detect 19 metabolites produced by Penicillium spp. on chestnuts, hazelnuts, walnuts and almonds. Two extraction methods were developed, one for chestnuts and one for the other three nuts. The recovery, LOD, LOQ and matrix effect were determined for each analyte and matrix. Correlation coefficients were always >99.99%. In walnuts, a strong signal suppression was observed for most analytes and patulin could not be detected. Six strains: Penicillium bialowiezense, P. brevicompactum, P. crustosum, P. expansum, P. glabrum and P. solitum, isolated from chestnuts, were inoculated on four nuts. Chestnuts favored the production of the largest number of Penicillium toxic metabolites. The method was used for the analysis of 41 commercial samples: 71% showed to be contaminated by Penicillium-toxins. Cyclopenin and cyclopenol were the most frequently detected metabolites, with an incidence of 32% and 68%, respectively. Due to the risk of contamination of nuts with Penicillium-toxins, future studies and legislation should consider a larger number of mycotoxins.
... Table 6 clearly shows that HPLC and liquid chromatography with tandem mass spectrometry (LC-MS/MS) are the most commonly used methods for the determination of mycotoxins in separate matrices (38-41, 43, 44). For the pretreatment method, the QuEChERS procedure (quick, easy, cheap, effective, rugged and safe) seems to be the most commonly used technique (9,39,(43)(44)(45)(46). However, all these methods listed in Table 6 are suitable for the determination of several mycotoxins in either vegetable oil samples or sauce samples. ...
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A solid phase extraction-high-performance liquid chromatography-tandem Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS) method was established for the determination of 12 mycotoxins (ochratoxin A, ochratoxin B, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, HT-2 toxin, sterigmatocystin, diacetoxysciroenol, penicillic acid, mycophenolic acid, and citreoviridin) in edible oil, soy sauce, and bean sauce. Samples were extracted by 80:20 ( v:v ) acetonitrile-water solution, purified by PRiME HLB column, separated by aQ C18 column with mobile phase consisting of 0.5 mmol/L ammonium acetate-0.1% formic acid aqueous solution and methanol. The results showed that the limits of detection (LODs) and limits of quantification (LOQs) of 12 mycotoxins were 0.12–1.2 μg/L and 0.40–4.0 μg/L, respectively. The determination coefficients of 12 mycotoxins in the range of 0.20–100 μg/L were > 0.998. The average recoveries in soy sauce and bean sauce were 78.4–106.8%, and the relative standard deviations (RSDs) were 1.2–9.7% under three levels, including LOQ, 2× LOQ and 10 × LOQ. The average recoveries in edible oil were 78.3–115.6%, and the precision RSD ( n = 6) was 0.9–8.6%. A total of 24 edible oils, soy sauce and bean sauce samples were analyzed by this method. AFB1, AFB2, sterigmatocystin and mycophenolic acid were detected in several samples at concentrations ranging from 1.0 to 22.1 μg/kg. The method is simple, sensitive, and rapid and can be used for screening and quantitative analysis of mycotoxin contamination in edible oil, soy sauce, and bean sauce.
... On the other hand, there might be some adverse effects of these synthetic nutraceuticals depending upon their manufacturing material. The nutraceuticals contain mycotoxins, pesticides, and heavy metal residues while manufacturing the supplementation from coffee beans (89), legumes (90), herbal plants (91), edible vegetable oil (92), and green tea (93). The present research is therefore focused on the biological methods (biofortified food consumption) to overcome the Zn deficiency in humans. ...
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... Conventional approaches, including high-performance liquid chromatography (HPLC) [7,8] and HPLC-tandem mass spectrometry (HPLC-MS/MS) [5,6], have been widely used for AFB 1 detection in nuts and dried fruits, but generally these methods need expensive instruments, highly skilled personnel, and complex pretreatment steps, making them difficult to use for real-time, fast and in-field detection. In addition to instrumental methods, immunoassays have proven to be effective in routine diagnostic applications for type-B aflatoxins. ...
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Type-B aflatoxins (AFB1 and AFB2) frequently contaminate food, especially nuts and fried figs, and seriously threaten human health; hence, it is necessary for the newly rapid and sensitive detection methods to prevent the consumption of potentially contaminated food. Here, a lateral flow aptasensor for the detection of type-B aflatoxins was developed. It is based on the use of fluorescent dye Cy5 as a label for the aptamer, and on the competition between type-B aflatoxins and the complementary DNA of the aptamer. This is the first time that the complementary strand of the aptamer has been used as the test line (T-line) to detect type-B aflatoxins. In addition, the truncated aptamer was used to improve the affinity with type-B aflatoxins in our study. Therefore, the lengths of aptamer and cDNA probe were optimized as key parameters for higher sensitivity. In addition, binding buffer and organic solvent were investigated. The results showed that the best pair for achieving improved sensitivity and accuracy in detecting AFB1 was formed by a shorter aptamer (32 bases) coupled with the probe complementary to the AFB1 binding region of the aptamer. Under the optimal experimental conditions, the test strip showed an excellent linear relationship in the range from 0.2 to 20 ng/mL with a limit of detection of 0.16 ng/mL. This aptamer-based strip was successfully applied to the determination of type-B aflatoxins in spiked and commercial peanuts, almonds, and dried figs, and the recoveries of the spiked samples were from 93.3%−112.0%. The aptamer-complementary strand-based lateral flow test strip is a potential alternative tool for the rapid and sensitive detection of type-B aflatoxins in nuts and dried figs. It is of help for monitoring aflatoxins to avoid the consumption of unsafe food.
... Mycotoxins can be present in low moisture foods such as nuts (Wang et al., 2018b), dried fruits (Fanelli et al., 2017;Ozturkoglu-Budak, 2017), cereals (Habschied et al., 2019;Spanic et al., 2020), cereal products (Abia et al., 2017;Generotti et al., 2017), oilseeds (Mohammed et al., 2018), feeds (Lee et al., 2015), and fermented products such as beer (Peters et al., 2017;Mastanjević et al., 2018) and some types of tea (Wang et al., 2018a). Mycotoxin presence is also observed in foods of animal origin such as dairy products (Anelli et al., 2019;Vaz et al., 2020), meat (Al Khalaileh, 2018;Meucci et al., 2019), eggs (Jurisic et al., 2019), and breast milk (Cantú-Cornelio et al., 2016;Arcella et al., 2017); fruits such as apples (Li et al., 2020), fruit juices (Kalagatur et al., 2018;Pallarés et al., 2019) and wines (He et al., 2019); and vegetable oils (Hidalgo-Ruiz et al., 2019). ...
Article
Mycotoxins are secondary metabolites produced by some fungal species, mainly from the genera Alternaria, Aspergillus, Fusarium, and Penicillium. Mycotoxins can be found in raw materials and processed foods. High intake of mycotoxins in short time periods will generate outbreaks of mycotoxicosis distinguished by physical discomfort or even death. Chronic consumption of mycotoxins can cause several important illnesses. Due to the substantial health risk of mycotoxin intake, several organisations have recommended the maximum allowable limits in foods. Since differences in the values suggested across organisations affect the risk of populations ingesting these compounds, the criteria must be unified. Mycotoxins are generally highly thermostable. Operations commonly applied during food processing such as frying and roasting have variable effects in reducing the mycotoxin content. The use of probiotics to transform mycotoxins into minor toxic compounds is a promising alternative reduction measure. The complete elimination of mycotoxins in foods appears practically impossible. Therefore, good agronomic practices are essential to avoid the growth of mycotoxin-producing fungi in raw materials. Global climate change is a relevant issue due to the changes in rainfall, humidity, and temperature patterns worldwide could stimulate the growth of fungi in broader regions, thus increasing the risk of mycotoxin presence in foods and subsequent consumption. Therefore, increasing research and development in innovative methods for the elimination or reduction of mycotoxins in foods is essential.
... In recent years, more and more modern analytical instrumental methods (i.e., high performance liquid chromatography (HPLC) (Hidalgo-Ruiz et al., 2019), liquid chromatography-tandem mass spectrometry (LC-MS) (Schlegel and Elsinghorst, 2020;Yang et al., 2020), ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) (Manizan et al., 2018;Huang et al., 2022a) and etc.) have been used in the simultaneous detection of multiple mycotoxins. Although these methods have high sensitivity and reliable analytical results, they rely on sophisticated and expensive instruments, cumbersome sample pretreatment, long period detection and specialized personnel, which restrict their application for rapid detection in the field (Mahmoudi- Moghaddam et al., 2019). ...
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A dual-target aptamer functionalized probes (DTAFP) was applied for the detection of aflatoxin B1 (AFB1) and zearalenone (ZEN) simultaneously, which has not been reported. Meanwhile, two functional materials for signal amplification of the DTAFP were synthesized: 1) a three-dimensional molybdenum disulfide-reduced graphene oxide (MoS2-rGO) as a favorable loading interface; 2) a double-probes gold nanoparticles (AuNPs) modified by Thionin (Thi) and 6-(Ferrocenyl) hexanethiol (FC6S) as distinguishable and non-interfering signals. Mycotoxins on the electrode surface release into solution under the function of the DTAFP, leading a reduction of the differential peak impulse in signal response. Under the optimum conditions, the aptasensor exhibited a detection range of 1.0 pg mL−1–100 ng mL−1 for AFB1 and ZEN, with no observable cross reactivity. In addition, the aptasensor performed excellent stability, reproducibility, specificity, and favorable recovery in the detection of edible oil. This work demonstrated a novel method for the construction of a simple, rapid, and sensitive aptasensor in the detection of multiple mycotoxins simultaneously.
... PSA exhibited a good performance for the vast majority of analytes ( Figure 1b) but was unable to recover other important mycotoxins, such as AFB1 and AFG1. The moderate affinity of PSA with polar compounds may explain low recoveries for aflatoxins, being consistent with other works based on oily matrices [29,30]. Similarly, extraction with C18 was efficient for most compounds and only some low-polarity mycotoxins showed recoveries out of the range set, like ZAN (150%) and β-ZEL (155%). ...
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Cannabidiol (CBD) food supplements made of Cannabis sativa L. extracts have quickly become popular products due to their health-promoting effects. However, potential contaminants, such as mycotoxins and pesticides, can be coextracted during the manufacturing process and placed into the final product. Accordingly, a novel methodology using ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was developed to quantify 16 mycotoxins produced by major C. sativa fungi, followed by a post-target screening of 283 pesticides based on a comprehensive spectral library. The validated procedure was applied to ten CBD-based products. Up to six different Fusarium mycotoxins were found in seven samples, the most prevalent being zearalenone (60%) and enniatin B1 (30%), both found at a maximum level of 11.6 ng/g. Co-occurrence was observed in four samples, including one with enniatin B1, enniatin A and enniatin A1. On the other hand, 46 different pesticides were detected after retrospective analysis. Ethoxyquin (50%), piperonyl butoxide (40%), simazine (30%) and cyanazine (30%) were the major residues found. These results highlight the necessity of monitoring contaminants in food supplements in order to ensure a safe consumption, even more considering the increase trend in their use. Furthermore, the developed procedure is proposed as a powerful analytical tool to evaluate the potential mycotoxin profile of these particular products. Key Contribution: The first multi-class analysis of CBD-based supplements regarding mycotoxins and pesticide residues using high-resolution mass spectrometry techniques.
... Hepatocellular carcinoma (HCC) causes liver cancer and in developing countries is the third highest source of cancer deaths, with a 16-32 times greater risk of mortality [16]. About 25,,000 new incidences of liver cancer are reported globally each year, which might be related to the consumption of peanuts and maize contaminated with AFs: people with HBV (hepatitis B virus) are particularly susceptible to this [17]. ...
Article
Contamination of edible oils with aflatoxins (AFs) is a universal issue due to the detrimental effects of aflatoxins on human health and the fact that edible oils are a major source of fungal growth, particularly storage fungi (Aspergillus sp.). The objective of this study was to assess aflatoxin B1 (AFB1) in edible oil used in fried food in order to determine the risk of cancer from AFB1 exposure through cooked food using the FAO/WHO's and EFSA's margin of exposure (MOE) quantitative liver cancer risk approaches. Using Mycosep 226 columns and HPLC-FLD, 100 samples of cooking oils (soybean, canola, and sunflower oil) from different food points were analyzed for contamination with aflatoxins. Of all the samples tested, 89% were positive for total aflatoxins and AFB1, with 65% indicating AF concentrations beyond permitted levels. Canola oil was found to contain higher levels of AFB1 and AFs than soybean and sunflower oil. Almost 71 percent of canola oil samples (range of 54.4-281.1 µg/kg) were contaminated with AF levels higher than the proposed limits of the European Union (20 µg/kg). The consumption of canola oil samples used in fried foods had MOE values that were significantly lower as compared to sunflower and soybean oils, indicating that risk reduction is feasible. Additionally, compared to soybean and sunflower oil, canola oil exhibited a greater threat of liver cancer cases linked to AFB1 exposure (17.13 per 100,000 males over 35 and 10.93 per 100,000 females over 35). Using a quantitative liver cancer approach, health risk valuation demonstrated that males and females over the age of 35 are at significant risk of developing liver cancer. The health risk assessment exposed that the males and female over the age of 35 are at considerable risk of liver cancer by using a quantitative liver cancer approach. The innovation of this study lies in the fact that no such study is reported related to liver cancer risk evaluation accompanied with AFB1 exposure from consumed edible oil. As a result, a national strategy must be developed to solve this problem so that edible oil products are subjected to severe regulatory examination.
... An ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method based on the QuEChERS procedure, including the dispersive solid phase extraction (dSPE) step with a C18 sorbent, has been developed for the determination of mycotoxins (α-zearalenol (α-ZEL), ZEN, and AFB 1 , aflatoxin B 2 (AFB 2 ), aflatoxin G 1 (AFG 1 ), and aflatoxin G 2 (AFG 2 )) in edible oils (Hidalgo-Ruiz et al., 2019). In contrast with the common trend of including as many mycotoxins/commodities as possible, the work by Hildago-Ruiz et al. (2019) addresses a scientifically sound target and is dedicated to only one commodity, while including a wide range of representative types, namely different types of olive oils (extra virgin olive oil, olive oil, lampante olive oil and refined olive oil), two types of pomace oil, two types of sunflower oil, soy oil, and maize oil. ...
Article
This review summarises developments on the analysis of various matrices for mycotoxins that have been published in the period from mid-2018 to mid-2019. Analytical methods to determine aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes, and zearalenone are covered in individual sections. Advances in sampling strategies are also discussed in a dedicated section. In addition, developments in multi-mycotoxin methods – including comprehensive mass spectrometric-based methods as well as simple immunoassays – are also reviewed. This critical review aims to briefly present the most important recent developments and trends in mycotoxin determination as well as to address limitations of the presented methodologies.
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Mycotoxins are the most widely studied biological toxins, which contaminate foods at very low concentrations. This review describes the emerging extraction techniques and the current and alternatives analytical techniques and methods that have been used to successfully detect and identify important mycotoxins. Some of them have proven to be particularly effective in not only the detection of mycotoxins, but also in detecting mycotoxin-producing fungi. Chromatographic techniques such as high-performance liquid chromatography coupled with various detectors like fluorescence, diode array, UV, liquid chromatography coupled with mass spectrometry, and liquid chromatography-tandem mass spectrometry, have been powerful tools for analyzing and detecting major mycotoxins. Recent progress of the development of rapid immunoaffinity-based detection techniques such as immunoassays and biosensors, as well as emerging technologies like proteomic and genomic methods, molecular techniques, electronic nose, aggregation-induced emission dye, quantitative NMR and hyperspectral imaging for the detection of mycotoxins in foods, have also been presented.
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Multiple mycotoxins may co-occurred in a single product and cause serious threats to public health. Herein, a multiplex immunochromatographic assay (mICA) was developed based on novel α-Fe2O3 nanocubes (FNCs) as signal tags for the simultaneous detection of deoxynivalenol (DON) and aflatoxins B1 (AFB1). The FNCs with eminent water-dispersibility and stability were synthesized by a one-step hydrothermal process, which can rapidly label monoclonal antibodies (mAbs) to form FNCs-mAb probe. Under optimal experimental conditions, the visual limit of detection for DON and AFB1 were 0.18 ng/mL and 0.01 ng/mL, respectively, which were at least 2-fold improvement compared with the traditional gold nanoparticles based mICA. Furthermore, DON and AFB1 residual in mung bean, millet and corn were successfully detected by the proposed biosensor, and the average recovery rates were 93.3%–128.3%. Thus, this work indicated that the developed FNCs-mICA provided a sensitive, rapid and reliable on-site simultaneous detection of multiple mycotoxins.
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Worldwide, contamination of mycotoxins in certain aliments (including cereals, edible oil, unprocessed milk, pistachios, ginger, and other products) has, in recent years, raised serious concerns. Due to their toxicity, the maximum acceptable levels for mycotoxins are standardized and checking their occurrence in foodstuffs is essential to ensure food safety and customer protection. In terms of mycotoxins detection techniques, having a series of advantages such as high sensitivity, rapidity, ease of use, and simultaneous identification of several mycotoxins, immunoassay-based methods have been significantly developed. Furthermore, on-site detection and chromatography-based techniques provide sensitivity, accuracy, and selectivity in the determination of mycotoxins. Also, some new and modified mycotoxin compounds are identified by tandem mass spectrometric detectors. In order to organize the knowledge status, improve detection efficiency and motivate new research, this review focuses on research published in on mycotoxins detection techniques in the edible oils.
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Aflatoxins are secondary metabolites produced by Aspergillus fungi, and aflatoxin B1 (AFB1) is the most potent carcinogen among these compounds. As one of the most widely distributed hazardous chemicals in nature, it can be introduced into the human body via the food chain, thereby posing a threat to human health. Therefore, improving the detection level of AFB1 has become a critical control point for food safety, medical examination, import and export inspection, and quarantine diagnosis. Herein, we designed a magnetic beads (MBs)-based flow cytometry fluorescence immunoassay (FCMFI). In this assay, we developed a magnetic bead modified with BSA–AFB1 to form a competitive immune pattern in the sample solution with free AFB1. A secondary antibody labeled with fluorescein isothiocyanate (FITC) binds to the above targets to provide a signal for the fluorescent immunoassay. Changes in fluorescence intensity received by the flow cytometer can be used to quantify the AFB1 content. In this work, the limit of detection (LOD) of FCMFI was 0.2034 μg/L for AFB1 in the buffer, and the limit of quantitation (LOQ) was 0.5659 μg/L. We also optimized some reaction conditions. Under the best conditions, the developed FCMFI method could analyze AFB1 efficiently with considerable sensitivity. The developed FCMFI was verified by comparing with the colorimetric indirect enzyme linked immunosorbent assay (id-ELISA), and commercial kit. The results show that the FCMFI method has excellent performance features, such as high sensitivity and low LOD. Hence, the convenience and reliability of the developed AFB1 detection method were fully demonstrated.
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In this article we describe a new and simple analytical method based on the Quick, Easy, Cheap, Effective, Rugged and Safe technique followed by dispersive solid-phase extraction clean-up with C18 and Lipifiltr® and LC–HRMS for simultaneously extracting six phthalate diesters and six of their metabolites (phthalate monoesters) from highly consumed seafood species. The method was validated for seafood with high and low lipid contents. Apparent recoveries were up to 79% for all compounds. Matrix effect values ranged from –8 to –48% for all compounds in both types of matrices. Method limits of detection were 1–25 ng g–1 dry weight (d.w.) for most compounds. Five seafood species were analysed using this method, and several phthalate diesters and monoesters were successfully quantified. Phthalate diesters were found at concentrations of up to 982 ng g–1 (d.w.) and phthalate monoesters were found at concentrations of up to 178 ng g–1 (d.w.).
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Mass spectrometry (MS) is widely used in food safety area, being fully implemented both in routine analysis and research laboratories. Indeed, MS is considered as an essential tool for the monitoring of food contamination. Continuous improvements in the instrumentation resulted in a breakthrough in analytical chemistry and consequently in food sciences. The advances in MS enabled the development of reliable, reproducible and robust new methodologies allowing for rapid and accurate screening analysis. The present review compiles the last advances (2015-2019) in MS aimed at the monitoring of, among others, microbiological contamination as well as pesticide and veterinary drug residues in food. Different MS techniques are discussed including matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), hyphenated techniques, ion mobility spectrometry-MS (IMS-MS) and ambient mass spectrometry (AMS) in addition to high resolution mass spectrometry (HRMS), whose implementation was an step forward in food safety since it allows for performing retrospective analysis.
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A green sample preparation method based on aqueous extraction followed by dispersive solid phase extraction (d-SPE) with in situ derivatization (ISD) was developed for the determination of aflatoxins (AFs) in traditional Chinese medicines (TCMs). AFs in TCMs were extracted by alkaline aqueous solution and converted to substituted coumaric acids. Then, mixed-mode anion exchange (MAX) sorbent was used to isolate and enrich the substituted coumaric acids. During the elution by acetonitrile/trifluoroacetic acid solution, AFs were reconstructed and in situ derivatized. Several parameters affecting the procedure were evaluated. The developed preparation method coupled with high performance liquid chromatography-fluorescence detection was successfully applied for AFs determination in TCMs. The limit of detection (LOD) reached 10 pg/mL for AFs. Good linearity was obtained in three orders of magnitude with correlation coefficients ranging from 0.9996 to 0.9999. The relative recoveries of the method were between 72.7% and 114.5% with intra- and inter-day relative standard deviations (RSDs) less than 9.5% and 10.1%, respectively. The method was successfully applied to determine AFs in 15 kinds of TCMs in China, with the results verified by IAC standard method.
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Due to increasing food safety standards, the analysis of mycotoxins has become essential in the food industry. In this work, we have developed a competitive upconversion-linked immunosorbent assay (ULISA) for the analysis of zearalenone (ZEA), one of the most frequently encountered mycotoxins in food worldwide. Instead of a toxin-conjugate conventionally used in competitive immunoassays, we designed a ZEA mimicking peptide extended by a biotin-linker and confirmed its excellent suitability to mimic ZEA by nuclear magnetic resonance (NMR) and surface plasmon resonance (SPR) analysis. Upconversion nanoparticles (UCNP, type NaYF4:Yb,Tm) served as background-free optical label for the detection of the peptide mimetic in the competitive ULISA. Streptavidin-conjugated UCNPs were prepared by click reaction using an alkyne-PEG-neridronate linker. The UCNP conjugate clearly outperformed conventional labels such as enzymes or fluorescent dyes. With a limit of detection of 20 pg mL-1 (63 pM), the competitive ULISA is well applicable to the detection of ZEA at the levels set by the European legislation. Moreover, the ULISA is specific for ZEA and its metabolites (α- and β-zearalenol) without significant cross-reactivity with other related mycotoxins. We detected ZEA in spiked and naturally contaminated maize samples using liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) as a reference method to demonstrate food analysis in real samples.
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The development of a multi-mycotoxins method using LC-MS/MS is necessary and it is clear that the development of such method involves many compromises in the choice of the different parameters. This review summarizes applications using conventional experimental designs and some recent studies using response surface methodology (RSM) as a mathematical modeling tool for the optimization of extraction procedures. The authors also discuss pros and cons of the different procedures. To our knowledge, it is the first review on experimental design for the development of multi-mycotoxin methods. This review could be useful in the development and optimization of LC-MS/MS methods with the aim of describing experimental design and variables (factors) that are likely to affect sensitivity and specificity.
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Argan fruit and argan oil are endemic products from Morocco and are like other oleaginous fruits with edible oils. However, there are no published data to indicate whether mycotoxin could contaminate argan kernels and edible argan oil. The study of the contamination of this product by mycotoxins is essential. In our study, all collected samples (argan fruits and argan oil) were stored for a long period (approximately 20 months) in conditions that were probably conducive to the development of molds. For quantitative analysis of mycotoxins, a sensitive ultraperformance liquid chromatography–tandem mass spectrometry method is proposed. Aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), aflatoxin G2 (AFG2), and ochratoxin A (OTA) were extracted using a modified QuEChERS method. The extracts were frozen overnight (−18 °C) to separate the majority of lipids and subjected to a cleanup step with C18 as dispersing material. The method was successfully validated in kernel powder and argan oil. Good linearity (0.125–20 μg/kg, R2 > 0.99), limits of quantification (0.45–0.8 μg/kg), recoveries (78–112%), and precision (<11%) were achieved for the five mycotoxins. Matrix-matched calibration curves were employed for accurate quantification. Using this method, no mycotoxins were found above the limit of quantification in any of the analyzed samples.
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Gel permeation chromatography (GPC) is herein used as size exclusion clean-up technique for highly sensitive and straightforward detection of Polycyclic Aromatic Hydrocarbons (PAHs) in olive oil samples. An advanced chromatographic system has been developed to isolate a series of PAHs with cancerogenic potential, including PAH4 (benzo(a)pyrene BaP, benzo(a)anthracene BaA, benzo(b)fluoranthene BbF and chrysene Chry) reported in the European Regulation. The system avails of two glass chromatographic columns and a switching valve, that allow removal of interfering analytes in olive oil without resorting to any preliminary extraction process. A seven-fold increase of the loaded sample amount versus conventional chromatographic systems (1g vs 0.150 g) has been pursued, as well as improved PAHs detection and quantification limits (LOD-LOQ for PAH4: 0.21-0.70 ng/g for BaA, 0.26-0.86 ng/g for Chry, 0.23-0.76 ng/g for BbF, 0.32-1.06 ng/g for BaP), in accordance with the continuous need of more and more reducing these limits in food analysis by the European Regulation. The protocol developed represents a highly innovative and efficient analytical method for organic pollutants in complex biological matrices as olive oil, that can have huge impact on technology for PAHs detection in food samples, being suitable for both industrial and small-scale laboratories.
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Traditional approaches to characterize edible oils such as chemical, chromatographic and light absorption techniques are laborious, expensive, and bulky to implement. This paper presents the electrochemical impedance spectroscopy of 13 types of edible oils, a rapid robust approach to characterizing the electrical behavior of oils without sample preparation. This is achieved through probing the oils via oscillating electric fields to capture oil-specific electrical behaviors. The principal component analysis discriminates the oil types well and establishes repetitive behavioral trends, perceived as electrical signatures. This data is applied in a case study of adulterated peanut oils to quantify adulteration via supervised machine learning with batch-wise leave-one-out implementation. The mean absolute errors and R² values measure 2.18–3.27 and 0.975–0.991 respectively across 4 test batches. This work provides an exemplar for the electrochemical study of edible oils, with potential for portable proof-of-value device configurations for rapid in situ analysis of edible oils and adulterated oils.
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Sample pretreatment is an important step in the detection and analysis of mycotoxins. However, conventional pretreatment methods are complex, time-consuming, and labor-intensive; moreover, they generate a large amount of organic waste that pollutes the environment. An environmentally friendly and automated pretreatment method is proposed. Without extraction using organic solvents in advance, aflatoxins in peanut oil are directly cleaned and concentrated by immunomagnetic beads with the aid of a reaction solution containing surfactant Tween-20. Under optimal conditions, the proposed pretreatment method requires 40 min to simultaneously pretreat 10-24 samples without any centrifugation or filtering steps, and virtually no organic waste was produced. This pretreatment step was coupled with ultra-performance liquid chromatography-fluorescence detection to develop an effective detection method. The recovery of spiked aflatoxins in peanut oils at different concentrations ranged from 91.6 to 100.8%, and the relative standard deviation was below 5.3%. This reliable method overcomes the drawbacks of conventional methods and offers great application prospects.
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The natural bioactive or nutraceuticals exhibit several health benefits, including anti-inflammatory, anti-cancer, metal chelation, antiviral, and antimicrobial activity. The inherent limitation of nutraceuticals or bioactive ligand(s) in terms of poor pharmacokinetic and other physicochemical properties affects their overall therapeutic efficiency. The excess of iron in the physiological compartments and its varying dynamic oxidation state [Fe(II) and Fe(III)] precipitates various clinical conditions such as non-transferrin bound iron (NTBI), labile iron pool (LIP), ferroptosis, cancer, etc. Though several natural bioactive ligands are proposed to chelate iron, the efficiency of bioactive ligands is limited due to poor bioavailability, denticity, and other related physicochemical properties. The present review provides insight into the relevance of studying the dynamic oxidation state of iron(II) and iron(III) in the physiological compartments and its clinical significance for selecting diagnostics and therapeutic regimes. We suggested a three-pronged approach, i.e., diagnosis, selection of therapeutic regime (natural bioactive), and integration of novel drug delivery systems (NDDS) or nanotechnology-based principles. This systematic approach improves the overall therapeutic efficiency of natural iron chelators to manage iron overload-related clinical conditions.
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Zearalenone (ZEN) is a universal mycotoxin contaminant in corn and its products. A surface-enhanced Raman scattering (SERS) based test strip was proposed for the detection of ZEN, which had the advantages of simplicity, rapidity, and high sensitivity. Core-shell [email protected] with embedded reporter molecules (4-MBA) were synthesized as SERS nanoprobe, which exhibited excellent SERS signals and high stability. The detection range of ZEN for corn samples was 10–1000 μg/kg with the limit of detection (LOD) of 3.6 μg/kg, which is far below the recommended tolerable level (60 μg/kg). More importantly, the SERS method was verified by HPLC in the application on corn samples contaminated with ZEN, and the coincidence rates were in the range of 86.06%–111.23%, suggesting a high accuracy of the SERS assay. Therefore, the SERS-based test strip with an analysis time of less than 15 min is a promising tool for accurate and rapid detection of ZEN-field contamination.
Article
This study is about the combination of magnetic solid phase extraction (MSPE) and high performance liquid chromatography-fluorescence detector (HPLC-FLD) for the pre-concentration and determination of Zearalenone (ZEA) in grain sample extracts. The novel sorbent (Fe3O4[email protected]), for selective and intelligent extraction of ZEA, was synthesized by doping Fe3O4 into the fibrous structure of hydroxyapatite nanoparticle (Fe3O4-HAP) and subsequently wrapping with molecularly imprinted polymers. The characteristic and morphology of magnetic particles were studied by infrared spectroscopy, vibrating sample magnetometer and scanning electron microscopy. The maximum adsorption capacity was 2.89 μg/mg. It could reach the adsorption equilibrium within 5 min. The adsorption isotherm of ZEA by the Fe3O4[email protected] were simulated. The results showed that the extraction process of ZEA with the sorbent accorded with Langmuir isotherm. The important factors affecting the extraction efficiency include elution solvent, washing solvent and the volume of them. After a serious of experiments, the optimum conditions were as follows: the volume of elution solvent was 4 mL of methanol and the washing solvent was acetonitrile-water 2:8(v/v). The calibration curve for ZEA was linear in the range of 10.00-300.00 μg/kg. The limit of detection and limit of quantitative was 2.00 μg/kg and 6.65 μg/kg, respectively. This method could provide a good reusability of 8 times and enough recoveries at three spiked levels (3, 5 and 8 ng/mL) ranging between 61.97% and 95.15% with the relative standard deviations of 1.94%∼7.44%. These results demonstrated that Fe3O4[email protected] could be used for separation, concentration and detection of ZEA from real samples.
Chapter
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For both quantitative and qualitative applications, mass spectrometry (MS) has evolved to become an effective analytical instrument. The first mass spectrometer was designed in 1912 and has since progressed from studying only small inorganic molecules to biological macromolecules, with virtually no mass constraints. Research in drug discovery, in general, depends considerably on MS technologies. The capability of mass spectrometry to analyze proteins and other biological materials is due to the advancements made by establishing soft ionization techniques that can turn biological molecules into ions, such as electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI). Consequently, MALDI has the benefit of generating peptide and protein single-charge ions, reducing spectral complexity. Regardless of the cause of ionization, a mass spectrometer's sensitivity is connected to the mass analyzer where ion separation occurs. Both quadrupole and flight time (ToF) mass probes are widely used and can be designed as QToF tandem mass spectrometric instruments combined. As the title suggests, tandem mass spectrometry (MS/MS) is the outcome of conducting two or more concurrent ion separations, typically integrating two or more mass analyzers. The development of high-resolution mass spectrometers resulted in the combination of a quadrupole and flight time Historically, this paper introduces mass spectrometry and describes the benefits and drawbacks of ESI and MALDI along with quadruple and ToF mass analyzers, including scientific mass analyzers. This paper is of an introductory nature and is intended for graduate and senior biochemistry students as well as chemists and biochemists who are not acquainted with mass spectrometry and want to learn the basics; it is not intended for professionals in mass spectrometry. Keywords: Mass spectroscopy, electrospray ionization, matrix-assisted laser desorption ionization, quadrupole, tandem mass spectrometry, proteomics, foodomics.
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Foodomics has recently emerged as a new discipline that studies food and nutritional products with modern analytical tools, including mass spectrometry (MS), to ensure food quality and safety. Foodomics is currently being used as a powerful tool in food authentication. It has been used to authenticate food items such as cereals, wine, honey, chocolates, and other commercial products. MS is the most suitable technique for authentication of food products because of its precise, accurate, and reproducible analytical power. MS-based techniques are nowadays extensively used for authentication of food and nutritional products. MS-based methods can detect various food components, including nutrients, additives, and toxic contaminants. Due to advancement in separation techniques, ionization and detectors in MS such as liquid chromatography tandem mass spectrometry, gas chromatography mass spectrometry, electrospray ionization tandem mass spectrometry, matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry, surface-enhanced laser desorption/ionization mass spectrometry, desorption electrospray ionization mass spectrometry, direct analysis in real-time mass spectrometry, extractive electrospray ionization mass spectrometry, and tandem-MS approaches have emerged as the method of choice for authentication of food products. This chapter discusses separation techniques and application of MS to analyze food products.
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In this work, based on a specific antibody was obtained from the Protein Data Bank (PDB), a library of the specific peptides of aflatoxin B1 (AFB1) was constructed by combining key amino acids, amino acid mutations and molecular docking. Then, the porous gold nanoparticles (porous AuNPs) were fabricated on the surface of a glassy carbon electrode (GCE). A novel, sensitive and no-label signal immunosensor was developed by signal enhancement with the specific peptide as the recognition element for the detection of AFB1 in cereals. Under the optimal conditions, the limit of detection (S/N=3) was 9.4×10⁻⁴ μg·L⁻¹, and the linear range was 0.01 μg·L⁻¹ to 20 μg·L⁻¹. The recovery results were 88.4%∼102.0%, which indicated an excellent accuracy. This sensor is an ideal candidate for screening the peptides of AFB1, and a novel immunosensor was used to detect AFB1 in cereals.
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A rapid screening method of 70 colorants for regulatory control in dyeable foods was established using ultra-high-performance liquid chromatography–hybrid quadrupole–Orbitrap mass spectrometry (UHPLC-Q/Orbitrap MS) with customized accurate-mass database and mass spectral library. A rapid, high-throughput, and simple sample pretreatment condition with low reagent consumption and high recovery was developed on the basis of ultrasound-assisted extraction and dispersion solid-phase extraction. Rapid screening was conducted by comparing the experimentally measured exact mass of the parent and fragment ions, the isotope pattern, and the retention time with the accurate-mass database and by matching the acquired MS/MS spectra against the mass spectral library. The performance of the method was evaluated in terms of linearity, limits of detection, limits of quantitation, recovery, repeatability, reproducibility, and matrix effect. The proposed method was applied for simultaneous analysis of 70 colorants in seven kinds of dyeable foods, and it exhibited great potential for broad, sensitive, and reliable.
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ABSTRAC Main group of contaminants including toxic compounds be formed during food processing and packaging (incidental group) and fungal toxins have been listed as critical challenge for food safety and human health. Because of absorption and transferring of these compounds into the human body and accumulation of them in different organs, several chronic diseases have been observed. The levels of these toxicants have been seriously monitored using analytical techniques. In this review, formation mechanism, toxicological effect and analytical methods of biogenic amines, furfural, hydroxymethylfurfural, polycyclic aromatic hydrocarbon, acrylamide, bisphenol A, nitrosamine and aflatoxin were discussed in different food samples.
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A new, green, and cost-effective magnetic solid-phase extraction of aflatoxins and ochratoxins from edible vegetable oils samples was developed using polydopamine-coated magnetic multi-walled carbon nanotubes ([email protected]3O4-MWCNTs) as the absorbent. [email protected]3O4-MWCNTs nanomaterials were prepared by chemical co-precipitation and in situ oxidation and self-polymerization of dopamine and was characterized. Factors affecting MSPE and the adsorption behavior of the adsorbent to mycotoxins were studied, and the optimal extraction conditions of MSPE and the complexity of the adsorption process were determined. Based on this, the magnetic solid-phase extraction-high-performance liquid chromatography-fluorescence detection method (MSPE-HPLC-FLD) was established for determining six mycotoxins [aflatoxin B1 (AFB1), AFB2, AFG1, and AFG2, and ochratoxin A (OTA) and OTB)] in vegetable oils. The recovery was 70.15%∼89.25%, and RSD was≤6.4%. [email protected]3O4-MWCNTs showed a high affinity toward aflatoxins and ochratoxins, allowing selective extraction and quantification of aflatoxins and ochratoxins from complex sample matrices.
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A sensitive and accurate multiple fluorescence immunoassay for the simultaneous quantitative detection of Zearalenone (ZEN) and Ochratoxin A (OTA) in single spot based on multicolor quantum dots labeling was developed for the first time. Two kinds of ZnCdSe/ZnS (core/shell) quantum dots (QDs) with maximum emission wavelengths at 520 nm (green) and 610 nm (orange-red) were selected as marking materials, respectively. The anti-ZEN-mAb-QDs and anti-OTA-mAb-QDs were designed as the immune fluorescent probes. Fluorescence was measured at the same excitation wavelength and two different emission wavelengths to determine each target. The procedure for QDs-based multiple fluorescence labeled immunosorbent assay (M-FLISA) was developed. The 50% inhibition concentrations (IC50) of ZEN and OTA were 0.034 and 1.17 ng/mL. Moreover, the limits of detection (LOD) for the simultaneous determination was 0.00015 and 0.049 ng/mL for ZEN and OTA, respectively. In addition, the recoveries ranged from 93.15 to 101.90% for ZEN and from 95.29 to 102.43% for OTA, with the coefficient variation (CV) of 2.70–8.86% and 3.51–6.22% respectively. There was a good correlation between the M-FLISA and high performance liquid chromatography (HPLC) results, which confirmed that the M-FLISA was suitable for the simultaneous quantitative detection of various mycotoxins.
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Plant nutraceuticals have currently been receiving international attention due to their potentially health-promoting effects when consumed as part of a varied diet, including antioxidant, anti-inflammatory, and anti-proliferative properties. These beneficial effects have been attributed to the presence of bioactive compounds naturally occurring in food or produced de novo through metabolic pathways. However, taken into account that nutraceuticals could be concentrated forms of the food or plants, it is probable to find undesirable substances utilized in crop protection, such as pesticides, and other contaminants (e.g. mycotoxins), which could be concentrated during the extraction process. Hence, this review will deepen into the bioactive compounds and health-promoting properties of plant nutraceuticals as well as the challenges related to safety issues because of the increase consumption of these products by population.
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A method for sensitive analysis of 19 anabolic steroids (AS) in animal oil using enhanced matrix removal lipid (EMR-Lipid) cleanup and ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. Oil samples were extracted with 20 mL of acetonitrile aqueous solution and purified using EMR-Lipid cartridges. The eluent was evaporated to dryness under nitrogen and analyzed by UHPLC-MS/MS using 0.1% formic acid-acetonitrile and 0.1% formic acid-water solutions as the mobile phase via gradient elution. The method effectively removed unwanted matrix co-extractives better than other extraction cleanup techniques while still delivering acceptable recovery results for most of the AS. The established quantification method showed AS recovery in the range of 72.9-110.7% with good precision (relative standard deviation < 15%).
Chapter
The contamination of crops can come from several sources, either natural or anthropogenic. There are substances that come from food processing processes such as materials that are in contact with food or environmental and/or ubiquitous contaminants, such as polycyclic aromatic hydrocarbons (PAHs), 3‐monochloropropane‐1,2‐diol (3‐MCPDs), mineral oils, or phthalates, among others. To control chemical contaminants present in the final commercial products, governments and international organizations have established maximum residue limits at toxicologically acceptable levels for all the contaminants present in oils or seeds as mycotoxins, PAHs, 3‐MCPDs, glycidyl esters, mineral oil hydrocarbons, phthalates, or pesticides. Several analytical methods have been developed for the determination of all the contaminants indicated earlier, being chromatographic methods the most widely used. In this chapter, chemical contaminants such as mycotoxins, PAHs, 3‐MCPDs, mineral oils, phthalates, and pesticides present in edible oils and oilseeds are studied. Furthermore, extraction, analytical techniques, and occurrence of them from 2010 is reviewed in the target matrices.
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How to achieve simultaneous and rapid detection of various mycotoxins in food has important practical significance in the field of food processing and safety. In this paper, a smartphone immunoassay system based on hydrogel microspheres has been constructed to quickly detect two mycotoxins at the same time. The rapid detection system was reflected in the following three processes: (1) rapid separation of free matter after direct competition reaction based on hydrogel solid-phase carrier particles; (2) rapid detection process based on efficient catalytic function of enzymes; (3) fast capture and analysis of images based on smartphone software. Ochratoxin A (OTA) and zearalenone (ZEN) are secondary toxic metabolites of fungi that can contaminate a wide range of foods and feeds. OTA and ZEN were used as detection model molecules to verify the feasibility of the intelligent rapid detection system. The entire detection process was within 30 min, and the results were analyzed in only 10 s. Detection limits of mycotoxins OTA and ZEN are 0.7711 ng L−1 and 1.0391 ng L−1. The recoveries of both mycotoxins ranged from 76.72 to 122.05%. This study provides a universal rapid detection method for on-site application of large-scale food security testing.Graphical abstract Schematic diagram of the construction of the smartphone detection system: The system is divided into three parts: detection, image capture and analysis, and result.
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Mycotoxins are a class of secondary metabolites produced by filamentous fungi that are harmful to humans and animals. Here, a multiplex immunochromatographic assay was reported, which is based on 25 nm colloidal gold for simultaneous qualitative detection of fumonisin B1 (FB1), deoxynivalenol (DON) and zearalenone (ZEN) in wheat and corn samples. After conditions optimization, the immunochromatographic strip has high sensitivity. The visual detection limits of the immunochromatographic test strips for FB1, DON and ZEN reached 60, 12.5 and 6 ng/mL, respectively. In addition, the immunochromatographic strip has high specificity, no reaction to each other, or no cross-reactivity with ochratoxin A (OTA) and aflatoxin B1 (AFB1). Furthermore, eighteen samples (including corn and wheat) were tested using the test strips and verified by liquid chromatography-mass spectrometry (LC-MS/MS). The results of strips were found to be consistent with those of liquid chromatography-mass spectrometry (LC-MS/MS). In short, this work demonstrates that the spherical colloidal gold-based immunochromatographic test strip we developed can be used to quickly and simultaneously monitor the existence of multiple mycotoxins in agricultural food samples.
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This study aimed to review fungal mycotoxins in foods, their roles and significance in human nutrition and health. This paper provided comprehensive information on the mycological quality and mycotoxin safety of foods. The review showed that moulds are multicellular fungi that form thin thread like structures called hyphae. They are widely distributed and found wherever moisture is present with adequate nutrients that can sustain their growth. Fungi are major spoilage of foods and feedstuffs. The proliferation of various fungi in agricultural products leads to reduction in yield and quality with significant economic losses. Fungi produce secondary metabolites which are referred to as mycotoxins which have been found to be present in most food substances. The mycotoxins are low weight metabolites which cause harm known as mycotoxicoses, in livestock, domestic animals and humans and therefore of public health significance. The production of mycotoxins is stimulated by certain environmental factors: ...
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In this study, 288 milk samples were collected randomly from individual farms in Qazvin province from March to February 2012, Iran. Samples were analysed for Aflatoxin M1 (AFM1) by ELISA; also the Aflatoxin B1 (AFB1) contamination in animal feed was determined at the same time as the sampling of raw milk. One hundred and sixty-three samples (56.59%) were found to contain AFM1 at various levels; the presence of AFM1 was detected in a concentration ranging between 0.01 and 0.22 ppb. In 113 (69.32%) of the 163 milk samples, AFM1 levels were found to be higher than the maximum tolerable limit (0.05 ppb) accepted by the European union/Codex Alimentarius Commission. The mean AFM1 contamination levels in milk in summer and winter were 0.08 and 0.18 ppb, respectively. The AFB1 contamination level in the winter feed (2.27 ± 1.76) was higher than from summer (0.83 ± 0.60) (P < 0.05).
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There are adverse impacts by the changing climate on the agricultural sector; Kenya’s back borne may exacerbate the challenges of ensuring food safety and security, and reducing poverty in Africa as a whole. Understanding how climate change scenarios will affect agriculture is essential in ensuring future food security. In this paper whose objective was to review the potential impact of climate change on important mycotoxins that contaminate maize in Kenya, it focused on climatic factors: temperature and relative humidity, which affect fungal infection of crops and mycotoxin production by these fungi. Aflatoxins are potent mycotoxins that cause immune weakening, cancer and even death. Aflatoxin contamination causes significant loss for farmers, businessmen, marketers and consumers of varied susceptible crops. Climate change alters the complex communities of aflatoxin-producing fungi. This includes changes in space, time and in the quantity of aflatoxin-producers. Generally, if the temperature increases in cool or temperate climates, the respective countries may become more susceptible to aflatoxins. However, tropical countries may become too inhospitable for conventional fungal growth and mycotoxin production. Although some regions can afford to control the environment of storage facilities to minimize post-harvest problems, this happens at high additional cost.
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Maize kernels are susceptible to infection by the opportunistic pathogen Aspergillus flavus. Infection results in reduction of grain quality and contamination of kernels with the highly carcinogenic mycotoxin, aflatoxin. To understanding host response to infection by the fungus, transcription of approximately 9000 maize genes were monitored during the host-pathogen interaction with a custom designed Affymetrix GeneChip® DNA array. More than 4000 maize genes were found differentially expressed at a FDR of 0.05. This included the up regulation of defense related genes and signaling pathways. Transcriptional changes also were observed in primary metabolism genes. Starch biosynthetic genes were down regulated during infection, while genes encoding maize hydrolytic enzymes, presumably involved in the degradation of host reserves, were up regulated. These data indicate that infection of the maize kernel by A. flavus induced metabolic changes in the kernel, including the production of a defense response, as well as a disruption in kernel development.
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Background The current study was carried out to provide a reference for the control of mycotoxin contamination in feed ingredients and complete feeds for swine. Methods A total of 55 feed ingredients, including 14 corn, 13 wheat bran, 11 soybean meal and 17 dried distillers grains with solubles (DDGS) as well as 76 complete swine feeds including 7 creep feeds, 14 starter feeds, 14 grower feeds, 18 grower-finisher feeds, 10 gestating sow feeds, and 13 lactating sow feeds were randomly collected from 15 swine farms located in the Beijing region of China from July to August 2011. Immunoaffinity clean-up, using High-Performance Liquid Chromatography (HPLC) in combination with UV or Fluorescence Detection, was used for quantitative analysis of aflatoxin B1 (AFB1), deoxynivalenol (DON), zearalenone (ZEA) and ochratoxin A (OTA) in the ingredients and complete feeds. Results DON and ZEA were the most prevalent mycotoxins found. DON was detected at percentages of 93, 92, 54, 100 and 97% with a mean level of 1.01, 0.44, 0.05, 1.36 and 0.65 ppm in the samples of corn, wheat bran, soybean meal, DDGS and complete feeds, respectively. The detected percentages of ZEA were 100, 100, 54, 100 and 100 with mean levels of 109.1, 14.9, 9.2, 882.7 and 58.9 ppb in the same samples. In the wheat bran and soybean meal samples, the content of all four mycotoxins were below the maximum limits set by Chinese regulations while the percentage of samples that exceeded regulatory limits were 7, 57 and 7% for corn, and 7, 14 and 3% for the complete feeds for AFB1, DON and OTA respectively. DDGS showed the most serious mycotoxin contamination and the percentage of samples that exceeded regulatory limits were 6, 88 and 41%, for AFB1, DON and ZEA, respectively. Conclusions This paper is the first to present data on the natural occurrence of AFB1, DON, ZEA and OTA in ingredients and complete feeds obtained from swine farms in China’s Beijing region. The data shows that feed ingredients and complete swine feeds obtained from these farms are most often contaminated with DON followed by contamination with AFB1 and ZEA.
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Organically produced spices and herbs were analyzed for determination of aflatoxin B1 (AFB1) by ELISA using immunoaffinity column. For this purpose 93 organic spices and 37 organic herbs were randomly selected from organic markets and organic shops in Turkey. AFB1 was detected in 58 organic spice and 32 organic herb samples. Among organic spice samples, the maximum value was detected in cinnamon sample (53 μ g/kg). AFB1 was not detected in thyme samples. AFB1 levels of 41 organic spice samples were above the EU regulatory limit (5 μ g/kg). Among organic herb samples the highest concentration of AFB1 (52.5 μ g/kg) was detected in a rosehip sample. AFB1 levels of 21 organic herb samples were above the regulatory limits of the European Union. These results showed that more stringent measures must be taken for the prevention of mold contamination in the production of organic spices and herbs.
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This paper describes a method for determination of 27 mycotoxins and other secondary metabolites in maize silage. The method focuses on analytes which are known to be produced by common maize and maize-silage contaminants. A simple pH-buffered sample extraction was developed on the basis of a very fast and simple method for analysis of multiple pesticide residues in food known as QuEChERS. The buffering effectively ensured a stable pH in samples of both well-ensiled maize (pH < 4) and of hot spots with fungal infection (pH > 7). No further clean-up was performed before analysis using liquid chromatography–tandem mass spectrometry. The method was successfully validated for determination of eight analytes qualitatively and 19 quantitatively. Matrix-matched calibration standards were used giving recoveries ranging from 37% to 201% with the majority between 60% and 115%. Repeatability (5–27% RSDr) and intra-laboratory reproducibility (7–35% RSDIR) was determined. The limit of detection (LOD) for the quantitatively validated analytes ranged from 1 to 739 µg kg−1. Validation results for citrinin, fumonisin B1 and fumonisin B2 were unsatisfying. The method was applied to 20 selected silage samples and alternariol monomethyl ether, andrastin A, alternariol, citreoisocoumarin, deoxynivalenol, enniatin B, fumigaclavine A, gliotoxin, marcfortine A and B, mycophenolic acid, nivalenol, roquefortine A and C and zearalenone were detected. Maize silage fed to cows can be contaminated with mycotoxins from pre- and post-harvest fungi. Several metabolites were detected by LC-MS/MS; including zearalenone and mycophenolic acid from Fusarium (red) and Penicillium (green) infections, respectively.
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Co-occurrence of Aflatoxins, Ochratoxin A, Fumonisins, and Zearalenone in Cereals and Feed, Determined by Competitive Direct Enzyme-Linked Immunosorbent Assay and Thin-Layer Chromatography Aspergillus, Penicillium , and Fusarium species frequently contaminate crops. For this reason mycotoxins such as aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FBs), and zearalenone (ZEA) are found in food and feed in a wide range of concentrations, depending on environmental and storage conditions. Consumption of mycotoxin-contaminated food and feed has been associated with acute and chronic poisoning and carcinoma. The aim of this study was to determine the incidence and co-occurrence of AFs (B 1 +B 2 +G 1 +G 2 ), OTA, FBs (B 1 +B 2 +B 3 ), and ZEA in 37 samples of cereals and feed randomly collected in 2007 from households of an endemic nephropathy (EN) area in Croatia. The mycotoxins were determined using the competitive direct ELISA test (CD-ELISA) in combination with thin-layer chromatography (TLC). The most frequent mycotoxin was ZEA (92%, mean 318.3 μg kg ⁻¹ ), followed by FBs (27%, 3690 μg kg ⁻¹ ), AFs (24.3%, 4.6 μg kg ⁻¹ ), and OTA (16.2%, 9.8 μg kg ⁻¹ ). Levels of AFs, ZEA, and FBs detected by CD-ELISA significantly correlated with the TLC results. However, only one OTA-positive sample was confirmed by TLC due to its high limit of detection. The levels of these mycotoxins were below the permissible limit for animal feed. Twenty-nine percent of cereals were contaminated with FBs, OTA, or ZEA in mass fractions above the permissible limit for humans. Co-occurrence of two toxins varied between 4.2% and 54% and of three between 4.2% and 7.6%. Prolonged co-exposure to AFs, OTA, FBs, and ZEA might increase the risk of various chronic diseases.
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A method was developed and validated in-house for the detection and quantification of patulin in apple juice concentrate using a charge coupled device (CCD) on thin-layer chromatography (TLC) plates. Samples were extracted with ethyl acetate and then cleaned-up by extraction with a sodium carbonate solution. The method showed a mean recovery of 95%. The quantification and detection limit were 14 microg l(-1) and 0.005 microg per spot, respectively. The CCD camera is sufficiently sensitive to detect changes in spot fluorescence intensity caused by small differences in mycotoxin concentration under homogeneous illumination from a UV light source. The results of validation confirmed the efficiency of the method, which is sensitive enough to be used to quantify patulin in apple juice by producers or for government monitoring/survey programs. The method was applied to the analysis of 16 apple juice concentrate samples and patulin levels ranged from 15 to 46 microg l(-1). This study demonstrated the applicability of the TLC-CCD technique as a tool for monitoring patulin in apple juice.
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The chemicals endosulfan-alpha, endosulfan-beta, endosulfan sulfate, endosulfan ether, endosulfan lactone, PCB-21, PCB-48, PCB-61, and PCB-136 have been determined in 100 serum samples from women living in agricultural areas of Almería (Spain). The study includes a surgically treated breast cancer patient and a matching group of women with no sign of estrogenic-dependent disease. The determination was performed by gas chromatography with electron capture detection (GC-ECD) and tandem mass spectrometry (GC-MS-MS). Recovery, precision, linear range, detection limit (LOD), and quantification limit (LOQ) were calculated for each pesticide as was the expanded uncertainty (U). The method was evaluated for our laboratory and could be applied to subsequent results with relevant quality-control data. Comparison of the results was performed. The advantage of MS-MS over ECD for determination of endocrine-disrupting compounds in complex matrices is presented. The most commonly encountered pesticide was endosulfan-alpha. Endosulfan-beta and the PCB-48 congener were detected at concentrations lower than their LOQ. Endosulfan sulfate, endosulfan ether, endosulfan lactone, PCB-21, PCB-61 and PCB-136 were not found in any of the serum samples analysed.
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The complex diet of ruminants, consisting of forages, concentrates, and preserved feeds, can be a source of very diverse mycotoxins that contaminate individual feed components. A number of mycotoxins are successfully inactivated by the rumen flora, whereas others pass unchanged or are converted into metabolites that retain biological activity. Hence, the barrier function of the rumen largely determines the susceptibility of dairy cows and other ruminant species towards individual mycotoxins. An impairment of this barrier function due to diseases or the direct antimicrobial effect of certain mycotoxins may increase absorption rates. The rate of absorption determines not only the internal dose and risk for adverse health effects, but also the excretion of mycotoxins and the biologically active metabolites into milk.
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In this study, 16 mycotoxins were analyzed in ten kinds of dried fruits and nuts sampled from four climate zones in China. The results showed that all 16 mycotoxins were detected at a contamination frequency of 124/253. The most frequent mycotoxin category detected was TCs with contamination levels ranging from <LOQ–473.16 μg/kg. Two samples contaminated with AFB1 at levels that exceeded the maximum limit of China and EU. Significant differences of AFB1, AFG1, AOH, AME and ENNs contamination among the four climate zones were found. Specifically, the ENNs contamination level was significantly higher of samples from the semiarid to semi-humid zone than the arid zone, the semiarid zone and the humid zone. In the 124 positive samples, 66 samples were detected with two to eight mycotoxins. To the best of our knowledge, this is the first study of mycotoxin occurrence and co-occurrence in dried fruits and nuts from China that also included the emerging mycotoxins, ENNs and BEA.
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A simple and rapid method for the simultaneous determination of eleven mycotoxins—aflatoxins B1, B2, G1, and G2; fumonisins B1, B2, and B3; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin—in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS, QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionization in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy, and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6%—82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil, and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.
Article
A simple and efficient method for determining multiple mycotoxins was developed using a QuEChERS (quick, easy, cheap, effective, rugged and safe) based extraction procedure in vegetable oils. High performance liquid chromatography tandem mass spectrometry (HPLC-MSMS) was used for the quantification and confirmation of 16 chemically diversified mycotoxins. Different extraction procedures were studied and optimized by spiking 16 analytes into blank matrix, and the extraction with 85% MeCN solution and C18 as cleaning sorbent allowed an efficient recovery of 72.8-105.8% with RSDs less than 7%. The limit of detection (LOD) ranged from 0.04 to 2.9 ng/g. The developed method was finally applied to screen mycotoxins in 62 vegetable oil samples. Zearalenone (ZEN), aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and α-zearalenol (α-ZOL) were detected, with maximum concentrations of 0.59 (AFG1) – 42.5 (ZEN) ng/g. The method developed has the advantages of high sensitivity, accuracy and selectivity, and it can be applied to the target screening of mycotoxins in real samples.
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Safety concerns pertaining towards fungal occurrence and mycotoxins contamination in agri-food commodities has been an issue of high apprehension. With the increase in evidence based research knowledge on health effects posed by ingestion of mycotoxins-contaminated food and feed by humans and livestock, concerns have been raised towards providing more insights on screening of agri-food commodities to benefit consumers. Available reports indicate majority of edible oil-yielding seeds to be contaminated by various fungi, capable of producing mycotoxins. These mycotoxins can enter human food chain via use of edible oils or via animals fed with contaminated oil cake residues. In this review, we have decisively evaluated available data (from the past decade) pertaining towards fungal occurrence and level of mycotoxins in various oil seeds and their edible oils. This review can be of practical use to justify the prevailing gaps, especially relevant to the research on presence of mycotoxins in edible plant based oils.
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The aims of the present study were to investigate the occurrence of aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2) in dairy cow feedstuff samples collected from four west provinces in Iran and estimate the corresponding concentrations of aflatoxin M1 (AFM1) in milk during winter and summer in 2014. A total of 160 feed samples consisting of corn silage (n = 40), alfalfa hay (n = 40), straw (n = 40) and barley (n = 40) were analyzed using high-performance liquid chromatography with a fluorescence detector method. AFB1, AFB2, AFG1 and AFG2 were detected in 82.5%, 69.37%, 43.12% and 41.87% of the feed samples, respectively. The concentration of AFB1 in 65% (26/40) and 10% (4/40) of corn silage and straw samples was higher than the European Union limit, respectively. Estimation of the total corresponding concentration of AFM1 in milk was evaluated as 20.16 and 35.68 ng/l during summer and winter, respectively.
Article
An interlaboratory study was performed on behalf of the UK Food Standards Agency to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatographic (LC) method for the determination of deoxynivalenol in a variety of cereals and cereal products at proposed European regulatory limits. The test portion was extracted with water. The sample extract was filtered and applied to an immunoaffinity column. After being washed with water, the deoxynivalenol was eluted with acetonitrile or methanol. Deoxynivalenol was quantitated by reversed-phase LC with UV determination. Samples of artificially contaminated wheat-flour, rice flour, oat flour, polenta, and a wheat based breakfast cereal, naturally contaminated wheat flour, and blank (very low level) samples of each matrix were sent to 13 collaborators in 7 European countries. Participants were asked to spike test portions of all samples at a range of deoxynivalenol concentrations equivalent to 200-2000 ng/g deoxynivalenol. Average recoveries ranged from 78 to 87%. Based on results for 6 artificially contaminated samples (blind duplicates), the relative standard deviation for repeatability (RSD r) ranged from 3.1 to 14.1%, and the relative standard deviation for reproducibility (RSDR) ranged from 11.5 to 26.3%. The method showed acceptable within-laboratory and between-laboratory precision for all 5 matrixes, as evidenced by HorRat values <1.3.
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Abstract Mycotoxins are toxic secondary metabolites produced by filamentous fungi that occur naturally in agricultural commodities worldwide. Aflatoxins, ochratoxin A, patulin, fumonisins, zearalenone, trichothecenes and ergot alkaloids are presently the most important for food and feed safety. These compounds are produced by several species that belong to the Aspergillus, Penicillium, Fusarium and Claviceps genera and can be carcinogenic, mutagenic, teratogenic, cytotoxic, neurotoxic, nephrotoxic, estrogenic and immunosuppressant. Human and animal exposure to mycotoxins is generally assessed by taking into account data on the occurrence of mycotoxins in food and feed as well as data on the consumption patterns of the concerned population. This evaluation is crucial to support measures to reduce consumer exposure to mycotoxins. This work reviews the occurrence and levels of mycotoxins in Portuguese food and feed to provide a global overview of this issue in Portugal. With the information collected, the exposure of the Portuguese population to those mycotoxins is assessed, and the estimated dietary intakes are presented.
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Background: Dapivirine is a non-nucleoside reverse transcriptase inhibitor designed to prevent HIV-1 viral replication and subsequent propagation. A sensitive method is required to quantify plasma concentrations to assess drug efficacy. Results: Dapivirine-spiked plasma was combined with acetonitrile containing deuterated IS and was processed for analysis. The method has an analytical measuring range from 20 to 10,000 pg/ml. For the LLOQ, low, mid and high QCs, intra- and inter-assay precision (%CV) ranged from 5.58 to 13.89% and 5.23 to 13.36%, respectively, and intra- and inter-day accuracy (% deviation) ranged from -5.61 to 0.75% and -4.30 to 6.24%, respectively. Conclusion: A robust and sensitive LC-MS/MS assay for the high-throughput quantification of the antiretroviral drug dapivirine in human plasma was developed and validated following bioanalytical validation guidelines. The assay meets criteria for the analysis of samples from large research trials.
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Mycotoxins are abiotic hazards produced by certain fungi that can grow on a variety of crops. Consequently, their prevalence in plant raw materials may be relatively high. The concentration of mycotoxins in finished products is usually lower than in raw materials. In this review, occurrence and toxicology of the main mycotoxins are summarised. Furthermore, methodological approaches for exposure assessment are described. Existing exposure assessments, both through contamination and consumption data and biomarkers of exposure, for the main mycotoxins are also discussed.
Article
A rapid, reliable and sensitive method was developed to determine 12 mycotoxins (deoxynivalenol, aflatoxins B1, B2, G1, G2 and M1, fumonisins B1 and B2, ochratoxin A, HT-2 and T-2 toxin and zearalenone) simultaneously in maize, walnuts, biscuits and breakfast cereals. The method is based on a single extraction step using acetonitrile/water mixture (80/20 v/v) followed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The selectivity of the MS/MS detection allowed the elimination of further clean up steps. Extraction, chromatographic and detection conditions were optimised in order to increase sample throughput and sensitivity. Matrix-matched calibration was used for quantification and recoveries of the extraction process ranged from 70.0% and 108.4%, with relative standard deviations lower than 25% in all the cases, when samples were fortified at 5 and 50 μg/kg. Limits of detection ranged from 0.01 to 2.1 μg/kg and limits of quantification ranged from 0.03 to 6.30 μg/kg, which were always below the tolerance levels of mycotoxins set by European Union in the matrices evaluated. Several samples were analysed and aflatoxins B1, B2, G1, G2 and T-2 toxin were detected in one maize sample, with concentrations lower than 6.0 μg/kg and deoxynivalenol was detected in a breakfast cereal at 42.1 μg/kg.
Article
A new analytical method for the rapid and simultaneous determination of five mycotoxins (zearelenone, deoxynivalenol, Fusarenon X, 15-acetyldeoxynivalenol and nivalenol) in breakfast cereals and flours by heart-cutting GC-MS has been developed and validated. Extraction was performed with MeCN, applying a modified QuEChERS (QUick, Easy, CHeap, Effective, Rugged and Safe) procedure, and the extracts were analyzed after a silylation of the analytes under study. Careful optimization of the parameters of Deans Switch device and GC-MS was achieved in order to attain a fast separation in SIM mode, allowing a total run time of only 8 min. Acceptable recoveries for all mycotoxins at two different spiking levels (20 and 100 microg/kg) were achieved with good repeatability (from 9 to 21%). LOD ranged from 2 to 15 microg/kg and LOQ ranged from 5 to 50 microg/kg, which were lower than the maximum limit legal established by the European Union (EU). The method developed was applied to commercial breakfast cereals and flours; among the mycotoxins studied, deoxynivalenol and zearalenone were the most predominant.
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laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs
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Determination of mycotoxins by HPLC
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Jerome Jeyakumar, J. M., Zhang, M., & Thiruvengadam, M. (2018). Determination of mycotoxins by HPLC, LC-ESI-MS/MS, and MALDI-TOF MS in Fusarium species-infected sugarcane. Microbial Pathogenesis, 123(April), 98-110. https://doi.org/10. 1016/j.micpath.2018.06.045.
Co-occurrence of aflatoxins, Fig. 2. (a) Extracted ion chromatogram of the lampante olive oil sample contaminated with 25
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