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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This article used QuEchERS method,known as to be quick,easy,cheap,effective,rugged and safe,to determinate 11 pesticides residues in vegetables.After extraction and cleanup,the samples were detected by GC/MS.The LOQ and average recovery ratio were 5.6~18.2μg/kg and 67.7%~102.3% respectively,while RSD was less than 10.6%.The results show the QuEchERS method can be used for the determination of organophosphorus pesticide residues in vegetables.
QuEChERS
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For improving extraction and purification of vegetable’s multiple pesticide residues in QuEChERS method, a gas chromatography method has been developed for determining 24 organophosphorus pesticide residues in vegetable. The pesticide residues were extracted from sample with 0.1% acetic acid in acetonitrile,separated by capillary column DB-1701 (30 m×0.32 mm×0.25 μm) and detected by FPD (P). In the range of 0.002~0.05 mg/kg, recoveries (n=6) are 79%~103.5%,and RSD are 1.1%~5.6%. The limits of EPN are 0.01 mg/kg,carbophenothion and triazophos are 0.004 mg/kg,and other 21 pesticides are 0.002 mg/kg. The method is very easy to operate, cheap for cost,excellent for purification,and has the advantages of good recovery,repeatability,and sensitivity.
QuEChERS
Repeatability
Carbamate
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QuEChERS
Selected ion monitoring
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Objective A modified QuEChERS method for simultaneous determination of 109 pesticide residues in potato using gas chromatography coupled with mass spectrometry was established and validated. Methods The pesticide residues were extracted from the potato samples with acetonitrile,and purified by dispersion solid phase extraction( d-SPE) using N-propyl ethlene diamine( PSA) as the adsorbent. The GC-MS analysis was carried out under selected ion monitoring mode and the quantification was performed using the external standard calibration. Results The limits of quantification( LOQ) for 109 pesticide were in the range of 0. 001-0. 010 mg / kg. The recoveries were between 72. 7% and 118. 7% with the RSD of 1. 1%-17. 3%. When using electron impact( EI) mode,most pesticides exhibited matrix enhancement effects in potato matrix. To ensure an accurate determination,the matrix-matched calibration was used for quantitation. The established method was successfully applied to the potato samples provided by European proficiency test in fruits and vegetables organized by European Union Reference Laboratory for Residues of Pesticides in Fruits and Vegetables,and 13 pesticides were detected with the concentration in the range of 0. 002-1. 669 mg / kg with the Z-scores in the range of- 1. 00 to 1. 00. Conclusion The method was simple,sensitive,accurate and suitable for the fast screening test for multi-residue pesticides in potato.
QuEChERS
Solid phase extraction
Selected ion monitoring
Residue (chemistry)
Matrix (chemical analysis)
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Tomato crop is frequently damaged by diseases, pests and abiotic stresses, resulting in lower yielding and loss of fruit quality. The intensive use of pesticides in tomatoes without observation of good agriculture practices and regulations has caused great concern with a probable final product contamination. The QuEChERS method of sample preparation was used for the determination of six pesticides (buprofezin, carbofuran, endosulfan-α, endosulfan-β, endosulfan sulfate and monocrotophos) in thirty three tomato samples collected from local market retailers. The method involved extraction with acetonitrile, liquid-liquid partition with addition of MgSO4 and NaCl followed by dispersive solid phase extraction using primary secondary amine sorbent and the analyses were carried out with a gas chromatography/mass spectrometry equipment by ion trap. Recovery studies for different pesticides ranged from 71 to 111% and the relative standard deviation (RSD) was below 15%. No pesticide residue was detected (> LOD) among the thirty three tomato samples analysed.
QuEChERS
Endosulfan
Solid phase extraction
Carbofuran
Selected ion monitoring
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A method was developed for the determination of 12 carbamate pesticide residues in sugarcane by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The residues in the samples were extracted by acetonitrile,cleaned up by developed QuEChERS method,and then analyzed by using HPLC-MS/MS in multiple reaction monitoring(MRM) mode via positive electrospray ionization.External standard method was used to determine the residue contents with a good linear relationship(r20.995).The limits of quantification(LOQ) were 0.03~0.19 μg/kg.The recoveries of carbamate pesticide residues at three levels of 10,50,and 100 μg/kg were from 81.3% to 108.1% with the relative standard deviations(RSDs) of 0.8%~4.7%(n=6) in sugarcane.The method is simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.This developed procedure is suitable for the determination of carbamate pesticide residues in sugarcane.
QuEChERS
Carbamate
Residue (chemistry)
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It is important to have a reliable method to analyze pesticides in tea, a beverage commonly consumed in Iran. A validated method was developed for the determination of 20 pesticides in tea based on QuEChERS sample preparation and capillary gas chromatography-quadrupole mass spectrometry in selective ion monitoring mode (GC-MS/SIM) using triphenyl methane (TPM) solution as an internal standard. We used fortified, extracted, and cleaned-up tea samples instead of calibration standards for quantitation, which substantially reduced adverse matrix-related effects and negative recovery affected by graphite carbon black (GCB) on pesticide analysis. The recovery of pesticides at 3 concentration (40, 60, and 240 ng/g) ranged from 79.5% to 111.4% (n = 3). The method had acceptable repeatability with RSDr < 20%. The limits of quantification (LOQ) for all pesticides were ≤20 ng/g. The analytical results of the proposed method were in good agreement with proficiency test results (FAPAS, 19116). The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline. The validated method was suitable for the analysis of pesticides in tea.
QuEChERS
Repeatability
Residue (chemistry)
Black tea
Matrix (chemical analysis)
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An ultra performance liquid chromatography(UPLC)-high resolution time of flight mass spectrometer(TOFMS) method was established for the simultaneous determination of dichlorvos,chlorpyrifos,omethoate,and dimethoate residues in vegetable.The QuEChERS method was used for sample pretreatment.The matrix-matched external standard calibration curves were used for the quantitative analysis.The calibration curves of 4 organic phosphorous pesticides were linear in concentration range from 10 ng/mL to 250 ng/mL with correlation coefficients above 0.99.The limit of detection was 0.25~0.40 μg/kg and the limit of quantification was 0.73~1.00 μg/kg.The spiked recoveries in vegetable ranged from 80% to 98%.The relative standard deviations of the method were between 2.4% and 9.7%.This method was simple,efficient and accurate.Therefore,it was practicable in the trace determination of dichlorvos,chlorpyrifos,omethoate,and dimethoate in vegetable.
Omethoate
QuEChERS
Dichlorvos
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A method using QuEChERS sample preparation followed by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESIMS/MS) was developed for quantitative determination of 14 pesticide residues in Indonesian green coffee beans. The European Standard Method EN 15662:2008 was modified to obtain an appropriate extraction and clean-up procedure for green coffee bean samples. Homogenous slurry samples were extracted with 1% acetic acid in acetonitrile and the extracts were cleaned up by a high pigment dispersive SPE. LC-ESI-MS/MS was operated in the MRM mode for two specific precursor-product ion transitions per target compound to obtain 4 identification points. Representative matrix-matched calibration curves were applied to compensate matrix effects. This method was validated according to the requirements of SANCO/12495/2011. Limits of detection (LODs) and limits of quantification (LOQs) were obtained in the ranges of 0.2-2.9 μg kg-1 and 0.8-9.7 μg kg-1 respectively, showing lower values than the maximum residu limits (MRLs) set by importing countries. The method was applied to determine 14 pesticide residues in 181 Indonesian green coffee bean samples that were taken from different regions. Some pesticide residues were found in these samples and detected to be higher than the MRLs.
QuEChERS
Sample Preparation
Matrix (chemical analysis)
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QuEChERS
Residue (chemistry)
Repeatability
Maximum Residue Limit
Matrix (chemical analysis)
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Citations (39)