Chawla Suchi, Patel Hemlatta K, Vaghela Kiran M, Pathan Firoz Khan, Gor Hetal N, Patel Anil R, Shah Paresh G
Pesticide Residue Laboratory, AINP on Pesticide Residues, Anand Agricultural University, Khetiwadi Road, Anand, Gujarat, 388110, India.
Anal Bioanal Chem. 2016 Jan;408(3):983-97. doi: 10.1007/s00216-015-9192-2. Epub 2015 Dec 10.
A method was developed and validated for the analysis of 87 pesticides in cotton and groundnut oil by GC with ECD and FPD detectors and LC-MS/MS. The extraction procedure based on QuEChERS followed by low-temperature freezing and dispersive cleanup steps was validated in two oil matrices for 87 pesticides of different classes. Linearity, expressed as coefficient of variation, was within the acceptable range. Of those tested, 77-83 and 77-89% pesticides showed recoveries within the acceptable range of 70-120% on LC-MS/MS in cottonseed oil and groundnut oil, respectively, at different spiking levels. In case of GC analysis, 63-65 and 53-82% pesticides showed recoveries within the acceptable range of 70-120% on GC in cottonseed oil and groundnut oil, respectively, at different spiking levels. The exceptions to these recoveries were the few organochlorines which consistently gave lower recoveries. Recovery factors can be employed while analysing these pesticides by this method as the results obtained were consistent in both oils. RSD was less than 20% for most of the pesticides. The calculated limit of quantitation (LOQ) for most of the pesticides satisfies the maximum residue level (MRL) requirements as per European Union (EU) guidelines and Food Safety and Standards Authority of India (FSSAI).
开发并验证了一种通过配备电子捕获检测器（ECD）和火焰光度检测器（FPD）的气相色谱仪以及液相色谱-串联质谱仪（LC-MS/MS）分析棉花和花生油中87种农药的方法。基于QuEChERS的萃取程序，随后进行低温冷冻和分散净化步骤，在两种油基质中针对87种不同类别的农药进行了验证。以变异系数表示的线性在可接受范围内。在不同加标水平下，分别在棉籽油和花生油中，经LC-MS/MS检测，77 - 83%和77 - 89%的农药回收率在70 - 120%的可接受范围内。在气相色谱分析中，在不同加标水平下，分别在棉籽油和花生油中，63 - 65%和53 - 82%的农药回收率在气相色谱分析中处于70 - 120%的可接受范围内。这些回收率的例外情况是少数有机氯农药，其回收率始终较低。由于在两种油中获得的结果一致，因此在通过该方法分析这些农药时可采用回收率因子。大多数农药的相对标准偏差（RSD）小于20%。根据欧盟（EU）指南和印度食品安全标准管理局（FSSAI），大多数农药计算得出的定量限（LOQ）满足最大残留限量（MRL）要求。
