Method Validation for Pesticide Residues on Rice Grain in Aceh Besar District, Indonesia Using Gas Chromatography-Electron Capture Detector (GC-ECD)

Agus Winarsih, R. Idroes, Utari Zulfiani, M. Yusuf, M. Mahmudi, S. Saiful, S. A. Rahman
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引用次数: 3

Abstract

Analysis of pesticide residues in rice in Aceh Besar District using the Gas Chromatography – Electron Capture Detector (GC-ECD) method has been carried out. This study aims to validate the analytical method and determine the pesticide residue levels of Dichlorvos, Dimethoate, Bifenthrin, and λ-Cyhalothrin in rice samples. Rice samples in branded rice were taken from the Districts of Want Jaya, Indrapuri, Darussalam, Suka Makmur, Simpang Tiga, Kuta Baro, and ground using a grinder. The powder sample was extracted by the QuEChERS method and analyzed by GC-ECD. The results of the linearity test have met the requirements with the coefficient of determination (R2), which is an average of 0.98. The LOD values ranged from 0.013 to 0.017 mg/kg, while the LOQ ranged from 0.022 to 0.079 mg/kg. The results of precision and reproducibility (% RSD, n = 6) show the values of 0.56 - 1.26% and 1.14 - 2.19%, respectively, and the accuracy value (%Recovery) shows the results of 99.71 - 101.84%, with an RSD value of 2.42 - 3.59%, meet the requirement of 20%. The results of the analysis of the sample showed that sample A had a large %Recovery value in the Dichlorvos analyte, namely 139.10%, with the calculation that the Dichlorvos analyte contained 0.0206 mg/Kg. This value has not passed the MLR set by the European Food Safety Authority, which is 0.2 mg/Kg. In the other rice samples, no pesticide residue analytes were detected. The calculation of %Recovery of each analyte in the spiked sample ranged from 80-101%, which indicated that the pesticide residue analysis carried out had good accuracy, namely the requirement of 70-120%.
气相色谱-电子捕获检测器(GC-ECD)检测印尼亚齐Besar地区稻米中农药残留的方法验证
采用气相色谱-电子捕获检测器(GC-ECD)方法对亚齐贝萨尔地区大米中的农药残留进行了分析。本研究旨在验证分析方法,并测定水稻样品中敌敌畏、乐果、联苯菊酯和氰氯氰菊酯的农药残留量。品牌大米中的大米样本取自旺查亚、因德拉普里、达鲁萨兰国、苏卡Makmur、辛邦提加和库塔巴罗等地区,并使用研磨机研磨。粉末样品采用QuEChERS法提取,GC-ECD分析。线性检验结果符合要求,决定系数(R2)平均为0.98。检出限为0.013 ~ 0.017 mg/kg,检出限为0.022 ~ 0.079 mg/kg。精密度和重现性(% RSD, n = 6)分别为0.56 ~ 1.26%和1.14 ~ 2.19%,准确度(%回收率)为99.71 ~ 101.84%,RSD值为2.42 ~ 3.59%,满足20%的要求。对样品的分析结果表明,样品A在敌敌畏分析物中具有较大的%回收率值,为139.10%,计算敌敌畏分析物中敌敌畏含量为0.0206 mg/Kg。该数值未超过欧洲食品安全局设定的最大容许量(MLR),即0.2 mg/Kg。在其他大米样本中,没有检测到农药残留。加标样品中各分析物的回收率计算范围为80 ~ 101%,说明所进行的农药残留分析具有较好的准确度,即70 ~ 120%的要求。
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