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A new rapid and simple method for simultaneous determination of azoxystrobin, acetamiprid and metalaxyl in tomatoes has been developed and validated. The separation and quantification of investigated pesticides was performed by reverse-phase HPLC with diode-array detection. Pesticide residues were extracted with acetone and purified by liquid‒liqui...

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... [33] This showed quantitative performance of Orbitrap-MS methods is between 78% and 100% compared with LC-MS/MS. [82] Several factors can avoid or reduce the matrix effects for correct quantitation, that is, matricmatched standard, [50,95] the internal standard method, [37,96] the standard addition methods, [95] changing the chromatographic and mass spectrometric conditions. The effects of matrix matching differ between spices, and even when two spices of the same kind are used, the ion suppression or amplification of the MS signal for one spice does PANDEY ET AL. [102] In 2007 WHO developed a guideline for assessing the quality of herbal medicines regarding contaminants and residues to determine biological, chemical, and radio-nuclear contaminants as well as pesticide residues. ...
... [33] This showed quantitative performance of Orbitrap-MS methods is between 78% and 100% compared with LC-MS/MS. [82] Several factors can avoid or reduce the matrix effects for correct quantitation, that is, matricmatched standard, [50,95] the internal standard method, [37,96] the standard addition methods, [95] changing the chromatographic and mass spectrometric conditions. The effects of matrix matching differ between spices, and even when two spices of the same kind are used, the ion suppression or amplification of the MS signal for one spice does PANDEY ET AL. [102] In 2007 WHO developed a guideline for assessing the quality of herbal medicines regarding contaminants and residues to determine biological, chemical, and radio-nuclear contaminants as well as pesticide residues. ...
Article
Medicinalplantsafetyisarisingchallengeworldwideduetothecontinuedoveruse ofpesticidestotheirmaximumresiduelimits.Duetothehighdemandformedicinal plants, theirproduction isbeing increasedandsometimesprotectedbypesticide use.Theanalysisoftheseresiduesrequiresrobustanalyticalmethodstoensurethe safetyandqualityofmedicinalplants.Developingeffectivesamplepreparationfor detectingpesticidesischallenging,duetotheirdiversenatures,classes,andphysicochemical characteristics.Hence, existingtechniquesandstrategiesareneededto improve the reliabilityof the results. The reviewdiscusses thecurrent stateof samplepreparationtechniques, analyticalmethods, and instrumental technologies employed in pesticide residue analysis in medicinal plants. It highlights the challenges, limitations, andadvancements inthe field, providing insights intothe analytical strategies used to detect and quantify pesticide residues. Reliable, accessible, affordable, andhigh‐resolutionanalytical procedures areessential to ensure that pesticide levels inmedicinal plants are effectively regulated. By understanding thecomplexitiesof pesticide residueanalysis inmedicinal plants, this reviewarticleaims tosupport theconservationofmedicinal plant resources, promotepublichealth,andcontributetothedevelopmentofsustainablestrategies for ensuring thesafetyandqualityofmedicinal plants inNepal. The findingsof thisreviewwillbenefitresearchers,policymakers,andstakeholders involvedinthe conservationofmedicinalplantresourcesandthepromotionofpublichealth. KEYWORDS analytical techniques,medicinalplants,pesticides, samplepreparation, toxicity
... Thus, pesticides monitoring has become a public health issue in view of the growth of the levels agrochemicals in the hive products. This study was developed with modification QuEChERS EN 15662 and validated according to the European Union SANTE/2015/11945 guidelines a multiresidue method for the quantification 28 pesticides from different chemical group (acylalanine, benzilate, carbamate, dicarboximide, juvenile hormone mimic, neonicotinoid, organochlorine, organophosphorous, oxadiazine, oxime carbamate, pyrethroid, pyridinecarboxamide and triazole) in beeswax (Valverde & Pihlström, 2017). Beeswax samples were extracted by modified QuEChERS method and analyzed by GC-MS/MS. ...
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Proceeding about meeting of food engineering event of 2019 for celebrating world food day.
... The LOQ, understood as the lowest concentration of the compound that produces an SNR of 10:1, was usually determined. Nevertheless, it is important to indicate that the SNR is a secondary calculated value and the quantification accuracy of the proposed NMR method must be evaluated by the absolute integrated intensity of the signal, setting the LOQ as the lowest concentration of HEDP that generates suitable precision and accuracy values [43]. Following the latter statement, the calculated LOQ for a sample at 0.01% w/v concentration ranged from 0.01% w/v, for one minute of analysis (116 scans) to 0.003% w/v for 60 min of analysis (4745 scans). ...
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Etidronic acid (1-hydroxyethylidene-1,1-diphosphonic acid, HEDP) is a common antioxidant additive used as detergent in the processing plants of agri-food industry for fruit and vegetable washing processes before commercialization. In the present work, and for the first time, a quick and reliable alternative to standard established methods for HEDP quantitation study has been performed in vegetable-washing processes applying ³¹P NMR. The proposed quantitative nuclear magnetic resonance method has been fully validated in water with different analysis times including a novel validation of the limits of detection and quantification depending on the target expected concentration, which results in considerable cost and time savings in those samples containing high concentrations of the compound. The limits of quantification (LOQs) ranged from 0.017% w/v for one minute of analysis (116 scans) to 0.003% w/v for 60 min of analysis (4745 scans). Additional validation parameters have been evaluated such as quantification procedure (comparing internal vs. external calibration), working range (from 0.01% to 0.05% w/v), recovery (95.0%–105.4%) and intra- and inter-day precision (from 0.9 to 4.3%) at 0.01 and 0.05% w/v. The developed method has successfully been applied for the determination of HEDP in 10 samples of agri-food processing industrial waters used for the cleaning of fruits and vegetables prior to their commercialization, providing adequate results and obtaining HEDP concentrations between 0.003 and 0.050% w/v.
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Disulfoton is highly toxic insecticide and acaricide. Food safety requires analysis of disulfoton and its five metabolites (disulfoton-sulfoxide, disulfoton-sulfone, demeton-S, demeton-S-sulfoxide, and demeton-S-sulfone). However, simultaneous determination of disulfoton and its metabolites in agro-products was not established, and the limits of quantification (LOQs) of reported methods could hardly meet the requirement of maximum residue limits (MRLs) set by some countries or organizations. In the present study, disulfoton and its five metabolites in seven agro-products (maize, oat, rice, pea, asparagus, milk and chicken) were extracted according to a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure and simultaneously determined with a liquid chromatograph tandem-mass spectrometer. The method was accurate and reliable after optimization of several key parameters (chromatographic columns, mobile phase, and clean-up sorbents). The sensitivity of the proposed method was greatly improved through the concentration process. Matrix effects for six analytes in different matrices were evaluated, and matrix-matched calibration standards were used to compensate these matrix enhancement or suppression effects. Under optimal conditions, the developed method showed satisfactory linearity with coefficients of determination (R²) > 0.9919. The limits of detection (LODs) for all target analytes in different agro-products ranged from 0.01 to 1.68 µg/kg, while the LOQs were 5 µg/kg for disulfoton, and 1 µg/kg for its each metabolite. At three fortification levels, the mean recoveries were in the range of 71.3–114.4% with relative standard deviations (RSDs) < 16%. Analysis of 70 market samples showed a trace amount of disulfoton and/or its metabolites in 10% samples. In conclusion, the developed method exhibited both high sensitivity and accuracy, and is suitable and practical for the simultaneous determination of trace levels of disulfoton and its five metabolites in agro-products of plant and animal origin.
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The present study aimed to evaluate the Strata-X® sorbent, commonly used in cartridges, through analysis by high-performance liquid chromatography coupled with mass spectrometry. Due to the different physical-chemical characteristics of the compounds, different conditions of chromatography and mass analysis were necessary. The developed methods were validated in terms of selectivity, linear range, linearity (coefficient of determination, r²), the limit of detection (LOD), the limit of quantification (LOQ), accuracy (recovery, %), and precision (RSD, %). The results allowed us to select efficient extraction methods, using methanol acidified to pH 2 with formic acid, to elute the herbicides 2,4-D and dicamba in both sorbent materials. Besides, the Strata-X® sorbent was efficient in the sorption of analytes; thus, we indicate it for potential use in air sampling as an alternative to XAD-2.
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In urban, industrial, and agricultural areas, a vast array of contaminants may be found because they are introduced into the aquifers by different recharge sources. The emerging contaminants (ECs) correspond to unregulated contaminants, which may be candidates for future regulation depending on the results of research into their potential effects on health and on monitoring data regarding their occurrence. ECs frequently found in wastewater, such as acetaminophen, carbamazepine, primidone, and sulfamethoxazole, may be good indicators of the introduction of the reclaimed water to the aquifers. The resistance of the ECs to removal in wastewater treatment plants (WWTPs) causes them to be appropriate sewage markers. Plana de Castellón (Spain) is a coastal area that has been characterized by intensive citrus agriculture since the 1970s. Traditionally, in the southern sector of Plana de Castellón, 100% of irrigation water comes from groundwater. In recent years, local farmers have been using a mixture of groundwater and reclaimed water from wastewater treatment plants (WWTPs) to irrigate the citrus. The aims of the present study were: i) to assess the occurrences, spatial distributions, and concentrations of selected ECs, including 32 antibiotics, 8 UV filters, and 2 nonsteroidal anti-inflammatory drugs, in groundwater in a common agricultural context; ii) to identify the recharge (pollution) sources acting as the origin of the ECs, and iii) to suggest ECs as indicators of reclaimed water arrival in detrital heterogeneous aquifers. The obtained data provided relevant information for the management of water resources and elucidated the fate and behavior of emerging contaminants in similar contexts.
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This study highlights the development of a high peak capacity, high-throughput (HTP) approach for a target list of 62 organic contaminants in an environmental river water matrix on a HPLC conventional 400 bar system. Key separation metrics were evaluated (a) peak capacity, (b) total analysis time and (c) mobile phase consumption. An average peak width of 0.10 min with a total analyses time (inclusive of the column wash and re-equilibration) of 10 minutes showcased the parallel segmented flow (PSF) column technology HPLC-MS strategy for increased productivity and performance Comparable to UHPLC peak widths and analysis times, achieved at a significantly lower backpressure (<400 bar). The operation of the PSF in a narrow-bore scale format (internal diameter of 2.1 mm) resulted in a conservative HPLC scale total mobile phase consumption rate of 15 mL for the column separation; only 5.5 mL of that volume was exposed to the ion source per injection. Mobile phase consumption was higher compared to UHPLC, but on the other hand achieved higher peak capacity. Three representative compounds of differing retention and ionisation properties were studied in detail in terms of detection sensitivity (atrazine, diclofenac and fluazuron). The majority of the ion ratios for the standards in river water matrix were within ±30 % of the average ion ratios. The largest ion suppression occurred for atrazine (-25 % matrix effect), a pesticide notorious for poor ionization and poor peak shape issues. The lowest response transitions at 1 μg/L for the extracted ions in river water matrix of atrazine, diclofenac and fluazuron had signal to noise ratios ≥3, with the exception of diclofenac where 5 μg/L was the lowest calibration level. The peak area’s calibration curve slope and standard deviation in the detector’s response determination of limit of quantification (LOQ) were between 5.2 to 30.4 μg/L.
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In this study, several calystegines (A3, A5, B1, B2, B3, B4 and C1) have been determined in tomato. A simple extraction followed by a derivatization step with silylating agents has been performed prior to their analysis by gas chromatography coupled to high resolution mass spectrometry (GC-HRMS-Q-Orbitrap), which allowed the monitoring of several ions at accurate mass. The validation of the method has provided suitable values of linearity, trueness (73.7-120.0%) and precision (≤ 20.0%, except for calystegines B3 and B4 at 0.5 mg/kg). The limit of quantitation (LOQ) was set at 0.5 mg/kg for all analytes. The validated method was successfully applied to the analysis of nine different tomato varieties, and calystegines A3, A5, B2 and C1 were found at concentrations ranging between 0.65 mg/kg (C1) and 12.47 mg/kg (B2). Tomato varieties were classified according to their calystegines content applying an analysis of variance (ANOVA).