Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment

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  • ISSN
    1944-0057

Publications in this journal

  • [Show abstract] [Hide abstract]
    ABSTRACT: In 2010 the European Commission placed a limit on the amount of free formaldehyde in carrageenan and processed Eucheuma seaweed (PES) of 5 mg kg(-1). Formaldehyde is not used in carrageenan and PES processing and accordingly one would not expect free formaldehyde to be present in carrageenan and PES. However, surprisingly high levels up to 10 mg kg(-1) have been found using the generally accepted AOAC and Hach tests. These findings are, per proposed reaction pathways, likely due to the formation of formaldehyde when sulphated galactose, the backbone of carrageenan, is hydrolysed with the strong acid used in these conventional tests. In order to minimise the risk of false-positives, which may lead to regulatory non-compliance, a new high-performance liquid chromatography (HPLC) method has been developed. Initially, carrageenan or PES is extracted with 2-propanol and subsequently reacted with 2,4-dinitrophenylhydrazine (DNPH) to form the chromophore formaldehyde-DNPH, which is finally quantified by reversed-phase HPLC with ultraviolet light detection at 355 nm. This method has been found to have a limit of detection of 0.05 mg kg(-1) and a limit of quantification of 0.2 mg kg(-1). Recoveries from samples spiked with known quantities of formaldehyde were 95-107%. Using this more specific technique, 20 samples of carrageenan and PES were tested for formaldehyde. Only one sample had a detectable content of formaldehyde (0.40 mg kg(-1)), thus demonstrating that the formaldehyde content of commercial carrageenan and PES products are well below the European Commission maximum limit of 5 mg kg(-1).
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Shiitake mushrooms (Lentinula edodes) cultivated on bed-log are known to accumulate radiocesium. Since the Fukushima-Diichi nuclear power plant accident, the violation rate has been higher for log-cultivated shiitake than that for agricultural products or other foodstuffs. When testing shiitake mushrooms for radionuclide contamination, the validation of the sampling plan can be severely compromised by the heterogeneous contamination within shiitake lots. Currently, few data are available on the statistical properties of the radiocesium contamination of log-cultivated shiitake. In this paper, shiitake lots contaminated by radiocesium were identified, and the distribution of the radiocesium concentration within the lots was investigated. The risk of misclassifying shiitake lots was predicted from the operating characteristic curve generated from Monte Carlo simulations and the performance of various sampling plans was evaluated. Our study provides useful information for deciding an acceptable level of misclassification risk.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: The Food Contact Notification (FCN) programme was authorised by the US Food and Drug Administration (USFDA) Modernization Act of 1997. Manufacturers may file FCNs for food contact substances (FCSs) not already authorised or pre-sanctioned by the USFDA by demonstrating a reasonable certainty of no harm for their intended uses. The Division of Food Contact Notifications (DFCN) 10-year Retrospective Assessment Group was formed to collect and develop metrics associated with the first decade of the FCN Programme and determine the extent selected aspects of the review process contributed to the effective FCN. Comparative analysis of 924 FCNs revealed that 76% become effective, 23% were withdrawn and 1% received a not accepted status. The focus of the Group was to identify factors impacting the likelihood of an FCN becoming effective.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Two decades ago differences in the geographic distribution of distinct trichothecene mycotoxins in wheat and barley were first recorded. The different toxicological properties of deoxynivalenol (DON), nivalenol (NIV) and their acetylated derivatives require careful monitoring of dynamics of these mycotoxins and their producers. The phylogenetic species concept has become a valuable tool to study the global occurrence of mycotoxin producing Fusarium species. This has revolutionized our views on the terrestrial distribution of trichothecene -producing Fusaria in the context of agronomics, climatic conditions and human interference by global trade and exchange of agricultural commodities. This paper presents an overview of the dynamics of the different trichothecene-producing Fusarium species as well as their chemotypes and genotypes across different continents. Clearly not one global population exists, but separate ones can be distinguished, sometimes even sympatric in combination with different hosts. A population with more pathogenic strains and chemotypes can replace another. Several displacement events appear to find their origin in the inadvertent introduction of new genotypes into new regions: 3-acetyl-DON producing F. graminearum in Canada; 3-acetyl-DON producing F asiaticum in Eastern China; 15-acetyl-DON F. graminearum in Uruguay and NIV producing F asiaticum in southern USA.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: The emerging trend towards high-resolution mass spectrometry alternatives was evaluated by the application of Orbitrap mass spectrometry for the determination of acrylamide in coffee samples. The high resolving power of the Orbitrap mass spectrometer provided the high selectivity and sensitivity that enabled quantitative analysis of acrylamide in complex matrices, such as coffee. Several sample preparation methods and scanning modes of the mass spectrometer (full MS, t-SIM, t-MS2) were assessed in order to optimise parameters of the analytical method. The final procedure involved the extraction of acrylamide with acetonitrile, solid phase extraction with dispersive PSA and amino columns, and the detection by ultra-performance liquid chromatography coupled to a hybrid quadrupole-Orbitrap mass spectrometer (HPLC-Q-Orbitrap) operated in targeted MS2 scanning mode. The repeatability of the method at the lowest calibration level (10 μg kg(-1)), expressed as relative standard deviation, was 7.8% and the average recovery of acrylamide was 111%. The proposed method was applied to the determination of acrylamide in 22 samples of roasted coffee obtained from the Latvian retail market. Acrylamide concentration in coffee samples was in the range of 166-503 μg kg(-1).
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: To this day, research for furan mitigation has mostly targeted the levels of food production and handling of prepared foods by the consumer. However, part of the furan concentrations found in commercially available food products might originate from chemical deterioration reactions during storage. A range of individual vegetable purées was stored at two different temperatures to investigate the effects of storage on the furan concentrations of shelf-stable, vegetable-based foods. After 5 months of storage at 35°C (temperature-abuse conditions), a general increase in furan concentrations was observed. The furan formation during storage could be reduced by storing the vegetable purées at a refrigerated temperature of 4°C, at which the furan concentrations remained approximately constant for at least 5 months. Following storage, the vegetable purées were briefly reheated to 90°C, to simulate the effect of the final preparation step before consumption. As contrary to storage, furan concentrations decreased as a result of evaporative losses. Both refrigerated storage and the reheating step prior to consumption showed the potential of mitigation measures for furan formation in vegetable-based foods (e.g. canned vegetables, ready-to-eat soups, sauces or baby foods). Next to furan, the vegetable purées were analysed for 2- and 3-methylfuran. Tomato was very susceptible to the formation of both alkylated derivatives of furan, as opposed to the other vegetables in this study. Methylfuran concentrations rapidly decreased during storage, which was contrary to the results observed for furan.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: A herbal food supplement advertised as a potency pill was screened for the presence of PDE5 inhibitors. The resulting signals were characterised by UV, LC-MS in ESI-negative mode, and NMR spectroscopy using 1D and 2D experiments. Several substances were identified, bearing the basic chemical structure of sildenafil, but were not supposed to exhibit PDE5 inhibition. These compounds may be process-related impurities or by-products of different reaction steps in the synthesis of PDE5 analogues. As they were found to be present in different capsules at different concentrations, this is an example of the unreliable quality of dietary supplements.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Ochratoxin A (OTA) is widely found in food and feed products as a mycotoxin contaminant. It is produced by Penicillium species and several Aspergillus species. The identification OTA detoxification microorganisms is believed to be the best approach for decontamination. In this study, we isolated ASAG1, a bacterium with the ability to degrade OTA effectively, from grain depot-stored maize. A 16S rDNA sequencing approach was used to identify this strain as Bacillus amyloliquefaciens ASAG1. The degradation of OTA was detected in both medium and cell-free extracts after incubation with a culture of B. amyloliquefaciens ASAG1 cells. Subsequently, a hydrolysed enzyme (carboxypeptidase) related to the enzymatic conversion of OTA was cloned from the B. amyloliquefaciens ASAG1 genome. Using the Escherichia coli Expression System, we successfully expressed and purified this carboxypeptidase. When this enzyme was incubated with the engineered recombinant E. coli cells, the concentration of OTA was dramatically degraded. Our data therefore indicate that the carboxypeptidase produced by B. amyloliquefaciens ASAG1 is likely responsible for the biodegradation of OTA.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Honey samples, originating from Australia, were purchased and analysed for targeted pyrrolizidine alkaloids (PA) using a new and rapid isocratic LC-MS/MS method. This isocratic method was developed from, and is comparable to, a gradient elution method and resulted in no loss of sensitivity or reduction in chromatographic peak shape. Isocratic elution allows for significantly shorter run times (6 min), eliminates the requirement for column equilibration periods and thus has the advantage of facilitating a high-throughput analysis which is particularly important for regulatory testing laboratories. In excess of two hundred injections are possible, with this new isocratic methodology, within a 24 hour period which is a > 50% improvement on all previously published methodologies. Good linear calibrations were obtained for all ten PAs and four pyrrolizidine alkaloid N-oxides (PANOs) in spiked honey samples (3.57-357.14 µg L(-1); R(2) ≥ 0.9987). Acceptable inter-day repeatability was achieved for the target analytes in honey with % RSD values (n = 4) less than 7.4%. Limits of detection (LOD) and limits of quantitation (LOQ) were achieved with spiked PAs and PANOs samples; giving an average LOD of 1.6 µg kg(-1) and LOQ of 5.4 µg kg(-1). This method was successfully applied to Australian and New Zealand honey samples sourced from supermarkets in Australia. Analysis showed that 41 of the 59 honey samples were contaminated by PAs with the mean total sum of PAs being 153 µg kg(-1). Echimidine and lycopsamine were predominant and found in 76% and 88%, respectively, of the positive samples. The average daily exposure, based on the results presented in this study, were 0.051 µg kg(-1) bw day(-1) for adults and 0.204 µg kg(-1) bw day(-1) for children. These results are a cause for concern when compared with the proposed EFSA (European Food Safety Authority), COT (Committee on Toxicity) and BfR (Bundesinstitut für Risikobewertung - the Federal Institute of Risk Assessment Germany) maximum daily PA intake limit of 0.007 µg kg(-1) bw day(-1).
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Zearalenone (ZEN) has caused significant economic effects on swine production in China. There is growing concern that exposure to ZEN during pregnancy affects the health of the offspring due to changes in the development of the immune system. To assess the risks associated with maternal ZEN exposure, several immunological parameters were assessed in pregnant sows and their offspring. The main aim of the study was to determine if modified hallosite nanotubes (MHNTs) can be used to protect pigs against the adverse effects of ZEN. Eighteen pregnant sows (second parity Yorkshire sows) were randomly divided into three treatment groups: (1) basal diet (control group); (2) contaminated grain (instead of 50% mouldy corn); and (3) contaminated grain (instead of 50% mouldy corn) + 1% MHNTs. The pregnant sows were fed the different treated diets from days 35 to 70 of gestation. Dietary ZEN exposure decreased the organ coefficient and the mRNA expression levels of IFN-γ, TNF-α, and IL-10, and increased ZEN residues and IL-4 mRNA expression in the spleen of pregnant sows and neonatal piglets. Decreases in the serum IgA and IgG levels were observed in the pregnant sows. Maternal ZEN exposure decreased the organ coefficient and the mRNA expression levels of IFN-γ and IL-10, and increased IL-4 mRNA expression in the spleen of weaning piglets. Exposure to ZEN during pregnancy decreased the level of serum IgG in the weaning piglets. Maternal exposure to ZEN induced histopathological damage and oxidative stress in the spleens of pregnant sows and their piglets. The addition of MHNTs to ZEN-contaminated diets can mitigate the negative effects induced by ZEN in the swine.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: Citrinin, a fungal secondary metabolite of polyketide origin, is moderately nephrotoxic to vertebrates including humans. Citrinin is synthesized by condensation of acetyl-CoA and malonyl-CoA. Six genes involved in the citrinin biosynthesis, including pksCT, ctnA and ctnB, have been cloned in Monascus purpureus. pksCT gene encodes a polyketide synthase. ctnA is a regulatory factor. ctnB encodes an oxidoreductase. When the three genes were respectively disrupted, the disruption strains drastically decreased ctrinin production or barely produced citrinin. Ten new genes have been discovered in Monascus aurantiacus besides the above six genes. One of these gene displayed highest similarity to β-carbonic anhydrase gene from Aspergillus oryzae (74% similarity) and was designated ctnG. To learn more about the citrinin biosynthetic pathway, a ctnG-replacement vector was constructed to disrupt ctnG with the hygromycin resistance gene as the selection marker, then transformed into M. aurantiacus Li AS3.4384 by protoplast-PEG method. The citrinin content of three disruptants were reduced to about 50%, meanwhile pigment production decreased by 23%, respectively, over those of the wild-type strains. ctnG was deduced to be involved in the formation of malonyl-CoA as a common precursor of red pigments and citrinin. Therefore, the disruption of ctnG gene decreased citrinin and pigment production. M. aurantiacus Li AS3.4384 can produce higher concentrations of citrinin than other strains such as M. purpureus and M. ruber. Establishing the function of citrinin biosynthetic genes in M. aurantiacus is helpful in understanding the citrinin synthetic pathway and adopting some strategies to control contamination.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 12/2014;
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    ABSTRACT: A simple, rapid, reliable and economical mini-column (MC) method for the detection of tetracyclines residue (TCs) in chicken meat was developed. The method employs a commonly available Pasteur pipette which is tightly packed with silica gel and anhydrous sodium sulfate. Clean-up and detection of illegal levels can be achieved on the same column. Viewing the developed MC under a UV lamp revealed that TCs can be detected as a compact golden yellow fluorescent band at the junction between the anhydrous sodium sulfate and silica gel layers. Comparing the yellow band of control extracts with those fortified (100 ng mL(-1)) showed no overlap between analyte and impurities. The limit of detection (LOD) of the MC assay was 1 ng, indicating that chicken sample containing 10 µg TCs kg(-1) sample could be easily detected. Moreover, the intensity of the yellow band increased whenever TCs level in the extract increased. Evaluation utility of the method with blind samples as controls or samples fortified with total TCs at various levels indicated that about 90% of the total blank and spiked samples at levels below the permissible limits were assessed as accepted. The method can provide an alternative to microbial screening assays and could be used as an effective pre-screening technique in public health laboratories.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;
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    ABSTRACT: Mycotoxins including aflatoxins, deoxynivalenol, fumonisins and ochratoxin A are among the main fungal secondary metabolites detected as natural contaminants in South America in different commodities such as peanuts (aflatoxins), cereals (deoxynivalenol and fumonisins) or grapes (ochratoxin A). Different strategies including crop rotation, tillage practices, fungicide application and planting less susceptible cultivars are used in order to reduce the impact of these mycotoxins in both food and feed chains. The development of fungicide resistance in many fungal pathogens as well as rising of public concern on the risks associated with pesticide use led to the search for alternative environmentally friendly methods. Biological control of plant pathogens and toxigenic fungi offers an alternative that can complement chemical control in the frame of an integrated pest management to reduce the impact of mycotoxins in the food and feed chains. The advances made in Argentina on reducing the impact of toxigenic fungi and mycotoxins in peanut, grapes and cereals using the biocontrol strategy are summarised. Native bacteria, yeasts and filamentous fungi have been selected to evaluate them as potential biocontrol agents. Field trials showed that Bacillus subtilis RC 218 and Brevibacillus sp. RC 263 were effective at reducing deoxynivalenol accumulation in wheat. The application of Clonostachys rosea isolates on wheat stubble reduced Fusarium colonisation on the stubble. Bacillus amyloliquefaciens and Microbacterium oleovorans showed good activity to control both Fusarium verticillioides growth and the accumulation of fumonisins at pre-harvest stage in maize. Control of toxigenic Aspergillus flavus and aflatoxin accumulation in peanuts was achieved using a native atoxigenic Aspergillus flavus strain based on competitive exclusion of the toxigenic strains. Kluyveromyces thermotolerans strains were used as biocontrol agents to reduce the impact of Aspergillus section Nigri and ochratoxin A accumulation in grapes.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;
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    ABSTRACT: The use of cinnamon as a spice and flavouring agent is widespread throughout the world. Many different species of plants are commonly referred to as 'cinnamon'. 'True cinnamon' refers to the dried inner bark of Cinnamomum verum J. S. Presl (syn. C. zeylanicum) (Lauraceae). Other 'cinnamon' species, C. cassia (Nees & T. Nees) J. Presl (syn. C. aromaticum Nees) (Chinese cassia), C. loureiroi Nees (Saigon cassia), and C. burmannii (Nees & T. Nees) Blume (Indonesian cassia), commonly known as cassia, are also marketed as cinnamon. Since there is a prevalence of these various types of 'cinnamons' on the market, there is a need to develop a rapid technique that can readily differentiate between true cinnamon (C. verum) and other commonly marketed species. In the present study, coumarin and other marker compounds indicative of 'cinnamon' were analysed using DART-QToF-MS in various samples of cinnamon. This method involved the use of [M + H](+) ions in positive mode in addition to principal component analysis (PCA) using Mass Profiler Professional software to visualise several samples for quality and to discriminate 'true cinnamon' from other Cinnamomum species using the accurate mass capabilities of QToF-MS.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;
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    ABSTRACT: A sensitive and selective GC-MS method was developed and used to analyse human milk samples for both free and total bisphenol A (BPA). Total BPA was detected in 72 of the 278 human milk samples (25.9%) at concentrations from < 0.036 to 2.5 ng g(-1) with a geometric mean (GM) of 0.13 ng g(-1) and median of 0.11 ng g(-1), while free BPA was detected in fewer samples, 46 of the 278 samples (16.5%) at concentrations ranging from < 0.036 to 2.3 ng g(-1) with a GM of 0.11 ng g(-1) and median of 0.10 ng g(-1). Ratios of [free BPA]/[total BPA] for the positive samples ranged from 7.9% to 100% with a GM of 57.2% and median of 70.3%. Concentrations of free and total BPA in most samples were low with 0.39 and 0.65 ng g(-1) at the 95th percentile for free and total BPA, respectively, and they are also lower than those reported in other countries. Based on the low frequency of detection of free BPA in human milk samples, in general, dietary exposure to BPA for Canadian breast-fed infants is expected to be somewhat lower compared with exposure among formula-fed infants.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;
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    ABSTRACT: The quantification of allergens in food including baked food matrices is of great interest. The aim of the present study was to describe a non-immunologic method to quantify bovine β-casein using ultra performance liquid chromatography tandem triple quadrupole mass spectrometry (UPLC-TQ-MS/MS) in multiple reaction monitoring (MRM) mode. Eight of ten theoretical peptides from β-casein after tryptic digestion were compared and MRM methods were developed to determine 5 signature peptides. The peptide VLPVPQK was selected as the signature peptide for bovine β-casein because of the high sensitivity. A stable isotope-labeled internal standard was designed to adjust the instability of sample pretreatment and ionization caused by matrix effect. Using the present suspension digestion method, the native and denatured β-casein could be digested to release the signature peptide at the maximum extent. The UPLC-TQ-MS/MS method developed based on tryptic signature peptide led to a reliable determination of bovine β-casein allergen in baked food matrices at a low quantitation level down to 500 μg/kg with a satisfactory accuracy (< 8.9%) and recovery (98.8 ± 2.6-106.7 ± 3.0%).
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;
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    ABSTRACT: Palm kernel cake (PKC) is a useful source of protein and energy for livestock. Recently PKC has been used as an ingredient in poultry feed. Mycotoxin contamination of PKC due to inappropriate handling during production and storage has increased public concern for economic losses and health risks for poultry and humans. This concern has accentuated the need for the evaluation of mycotoxins in PKC. Furthermore, a method for quantifying mycotoxins in PKC has so far not been established. The aims of this study were therefore a) to develop a method for the simultaneous determination of mycotoxins in PKC and b) to validate and verify the method. An LC-MS/MS method using an electrospray ionisation interface (ESI) in both positive and negative ion-modes was developed for the simultaneous determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB1 and FB2), T-2 and HT-2 toxin in PKC. An optimum method using a 0.2 ml/min flow rate, 0.2% formic acid in aqueous phase, 10% organic phase at the beginning and 90% organic phase at the end of the gradient was achieved. The extraction of mycotoxins was performed using a solvent mixture of acetonitrile: water: formic acid (79:20:1, v/v) without further clean-up. The mean recoveries of mycotoxins in spiked PKC samples ranged from 81% to 112%. Limits of detection (LOD) and limits of quantification (LOQ) for mycotoxin standards and PKC samples ranged from 0.02 to 17.5 μg kg(-1) and 0.06 to 58.0 μg kg(-1), respectively. Finally, the newly developed method was successfully applied on PKC samples. The results illustrated that the method is efficient and accurate for the simultaneous multi-mycotoxin determination in PKC, which can be ideal for routine analysis.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014; 17:1-9. Impact factor 2.341.
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    ABSTRACT: In this work, a novel magnetic three-dimensional graphene nano-composite (3D-G@Fe3O4) with a high surface area was synthesised by a vacuum freeze-dried method. Due to its high surface area, specific three-dimensional nano-porous structure and excellent magnetic properties, it can be used as a magnetic solid-phase extraction adsorbent. Some chlorophenols in honey samples were enriched by this nanocomposite prior to their determination by HPLC with ultraviolet detection. Factors that affect the extraction efficiency, such as the amount of 3D-G@Fe3O4, extraction time, sample pH, ionic strength and desorption conditions were investigated and optimised. Under the optimum conditions, good linearity existed in the range of 10.0~1000.0 ng/g. The enrichment factors of the method for the analytes were in the range from 101 to 248. The limits of detection of the method (S/N = 3) were 1.0~1.5 ng/g. The recoveries of the method for the analytes at spiking levels of 100.0 and 400.0 ng/g were in the range of 93.2%~98.9%. The results showed that the proposed method is simple, reliable and sensitive. It will be a useful tool for the routine monitoring of chlorophenols in honey products.
    Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 11/2014;