Pesticide Residue Determination In Shahr-E-Rey Tomatoes Using Quechers Method
Mahboubeh YadolahiMehran BabriAmir AbdolahAmir Abdolah Mehrdad SharifAmin MousaviAmin Mousavi Khaneghah
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Abstract:
In this study, pesticide residues in tomato products from Shahr-e-Rey farms were measured and investigated by QuEChERS modified method. This method was on the base of the sample preparation in few steps and high speed. Measurement of pesticide residues was carried out by gas chromatograph with electron capture detector. In this study, most of the pesticides showed a recovery in the range of 70% – 120%. Limit of detection (LOD) and limit of quantification (LOQ) for all pesticides were lower than 0.50 and 1.90 µg/kg respectively. chlorpyrifos was detected in studied samples at average concentration 3.22 µg/kg, which was lower than the Maximum Residue Limits (MRLs) of national standard. Results showed that mentioned method is a very useful method for studying pesticides residues in tomato.Keywords:
QuEChERS
Residue (chemistry)
Electron capture detector
Maximum Residue Limit
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A rapid,simple and sensitive analysis method was developed for the simultaneous determination of 12 pesticides,including ethoprophos,phorate,chlorpyrifos-methyl,bis(2333-tetrachloropropyl) ether,malathion,chlorpyrifos,fipronil,methidathion,chlorfenapyr,triazophos,bifenthrin and fenpropathrin in wheat.The analysis of target compounds was performed by the modified QuEChERS sample preparation combined with GC-MS/SIM method.The sample was extracted with acetonitrile(1% acetic acid) in the triangle vase and cleaned up by C18 and aluminum oxide neutral.The results showed that the average recoveries of 12 pesticides at spiked levels of 0.025-1.0 mg/kg ranged from 76% to 108% with relative standard deviations of 0.4%-10.5%.The limits of quantitation(S/N=10) of 12 pesticides were in the range of 0.5-9.8 μg/kg,lower than maximum residue limits(MRLs) of EU.The developed method could meet the requirement of the multi-residues analysis.
Chlorfenapyr
QuEChERS
Methidathion
Bifenthrin
Phorate
Fipronil
Residue (chemistry)
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QuEChERS
Chlorfenapyr
Coumaphos
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A method of GC-MS coupled with QuEChERS was applied for simultaneous determination of 16 kinds of pesticide residues in wine.The sample was extracted with acidified acetonitrile.The extract was purified by QuEChERS method,using the mixture of N-propylethylenediamine,graphitized carbon black and C18 powder,and then separated on an Agilent HP-5MS column and detected by MS adopting EI-SIM.The linearity range of the mass concentration of 16 kinds of pesticides was 0.05-2.00 mg·L-1 with detection limits in the range of 0.006-0.060mg·kg-1.Tests for recovery were made by standard addition method,giving values of recovery in the range of 87.6%-105%,and RSD(n=6)in the range of 0.77%-6.9%.The method was used for analysis of pesticide residues in wine samples for import and export inspection.
QuEChERS
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The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with . The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.
QuEChERS
Sample Preparation
Residue (chemistry)
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The method for determination of 31 pesticide residues in vegetables was developed.The sample was extracted by 50mL actonitrile.The first 10mL aliquot of upper phase was concentrated and injected into the chromatograph for determination of 19 organophosphorus pesticide residues with flame photometric detector(FPD).The second 10mL aliquot of upper phase was purified by florisil solid phase extract(SPE) and injected into the chromatograph for determination of 12 pyrethroid pesticide residues with electron capture detector(ECD).The average recoveries of 31 pesticides ranged from 74.20%~103.5%,and the relative standard deviations(RSDs) were 0.48%~16.0%.The minimum detection limits were 0.001~0.020mg/kg.This method has the merits of simply,rapidty,high accuracy and precision.
Electron capture detector
Relative standard deviation
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QuEChERS method and GB method were used to pretreatment okra samples,the data of 24 kinds of pesticides including signal-to-noise ration,detection limit(S/N ≥3),signal value,linear range,linear equation,average recovery and relative standard deviation by LC-MS/MS were acquired.Contrast analysis indicated the QuEChERS method for the pretreatment had less interference detection,higher sensitivity,better accuracy and precision,and could achieve requirements of testing the trace analysis of various kinds of pesticide residues simulaneously.
QuEChERS
Linear range
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곡물류 모니터링 시료인 현미, 보리, 옥수수 3가지 작물을 대상으로 보편적으로 많이 사용되고 등록된 농약을 조사, 76종을 선정하여 QuEChERS AOAC Official 2007. 01. 법과 변형된 QuEChERS 법으로 LC-MS/MS를 이용하여 회수율 시험을 비교하였다. 1% acetic acid를 사용하여 추출하는 QuEChERS AOAC Official 2007. 01. 법의 0.05, 0.2 mg/kg 회수율 결과는 현미 32.4~139.0%, 보리 24.2~123.7%, 옥수수 29.0~117.2%였고, 그 중 sulfonylurea 계통인 azimsulfuron, ethoxysulfuron, flucetosulfuron, imazosulfuron에 대해 회수율이 낮게 나오는 문제가 있었으며, 이들 농약의 평균 회수율은 53.3%였다. 이런 문제를 해결하기 위해 QuEChERS 법의 추출용매를 1% formic acid가 함유된 acetonitrile 용매로 바꾼 결과, 0.05, 0.2 mg/kg 수준의 회수율은 현미 73.2~132.2%, 보리 80.9~136.8%, 옥수수 66.6~143.5%였으며 변이계수는 모두 10% 미만이었다. 문제시 되었던 sulfonylurea 계통의 농약의 회수율도 53.3%에서 90.5%로 증가하였다. 검출한계(limits of detection, LOD)와 정량한계(limits of quantification, LOQ)는 현미 0.24~1.92, 0.79~65.74 ng/g, 보리 0.12~21.12, 0.36~63.36 ng/g, 옥수수 0.28~100.8, 0.86~302.4 ng/g이었다. 변형한 QuEChERS 법을 모니터링 시료 현미, 보리, 옥수수에 적용하여 98개 시료를 분석한 결과 36개의 시료에서 26종의 농약이 검출되었다. 검출 농도가 가장 높은 농약은 tricyclazole로 1.17 mg/kg로 조사되었다. 변형한 QuEChERS법으로 전처리를 하여 질량분석기 뿐만 아니라 현재 많이 보급된 검출기인 ECD, NPD 및 UPLC에서도 분석이 가능한지 실험하였고, 현미, 보리, 옥수수의 평균 회수율은 ECD는 65.3~130.3%, NPD는 61.6~133.0%로 대부분의 농약들이 잔류농약 검색용을 목적으로 하는 다성분 분석의 기준인 70~130% 이내의 회수율과 30%의 미만의 변이계수 조건을 만족하였다. This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.
QuEChERS
Residue (chemistry)
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QuEChERS
Matrix (chemical analysis)
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Objective:To establish a method for determination of 31 pesticide residues in fruits and vegetables.Methods: Modified QuEChERS pretreatment method and a on-line GPC-GC-MS system were used for the rapid determination of 31 pesticide residues including organophosphorus,organochlorine,carbamate and pyrethroid etc.Results: The 31 pesticides were well separated and the detection limits of the method were 0.01 μg/kg～0.83 μg/kg,the recoveries were 72%～110% and the relative standard deviations were 1.6%～10%.Conclusion: The good sensitivity,precision,accuracy,simple operation and short analytical period of this method could satisfy the requirement of simultaneous determination of various pesticide residues.
QuEChERS
Carbamate
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The present study was the first attempt for determination and measurement of pesticide residues in tomatoes used in salad production plants in Isfahan, central Iran.A multiresidue method based on modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation, followed by Gas Chromatography Mass Spectrometry (GC-MS) was developed and validated for the determination of 15 pesticides (permethrin, primicarb, dichlorvos, diazinone, fenpropathrin, carbaryl, chlorpyrifos, malathion, chlortalonil, brompropilate, propargit, tetradifone, phosalone, iprodion and endosulfane) from different classes. The recovery yields ranged from 83.84 to 119.73%and the relative standard deviation (RSD) was below 20.54%. The limits of detection (LODs) were between 1.63to 10.5 mg/kg and the limits of quantifications (LOQs) were between 5.43to35 mg/kg. The method has been successfully applied to the analysis of 22 tomato samples obtained from salad production plants in Isfahan in Sep to Dec 2014.An amount of 31.81% of samples showed contamination above maximum residue levels (MRLs) with pesticides. In addition, 13.6% of samples had contamination with diazinone and 18.18% of samples with chlorpyrifos.A full consideration is essential for tomatoes used in salad and food productions. It suggests a need for revision of the current trend of supervision for tomatoes and other vegetables presented in wholesale markets. In all, the study confirms that pesticide residue determination in food products, especially in raw fruits and vegetables, is a very demanding task in public health safety and trade.
QuEChERS
Residue (chemistry)
Sample Preparation
Carbaryl
Maximum Residue Limit
Dichlorvos
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