Pesticide Residue and Food Quality Analysis Laboratory, University of Agricultural Sciences, Raichur 584 104, Karnataka, India.
Pesticide Toxicology Laboratory, Tamil Nadu Agricultural University, Coimbatore 641 003, Tamil Nadu, India.
Molecules. 2021 Mar 25;26(7):1837. doi: 10.3390/molecules26071837.
A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg for and 0.10 to 9.55 µg·kg (LOD) and 0.35 to 33.43 µg·kg (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDR) by spiking of mixed pesticides standards at 100 µg·kg recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.
建立了一种快速、灵敏、重现性好的同时测定和番茄中 77 种多类农药及其代谢物残留的气相色谱-串联质谱分析方法。方法采用乙腈提取,分散固相萃取净化,以正己烷-乙酸乙酯(95∶5,V/V)为洗脱剂,在优化的气相色谱-串联质谱条件下进行检测,内标法定量。结果表明,在 0.1910.91μg·kg 和 0.6336.34μg·kg 浓度范围内,和番茄中 77 种农药的方法检出限为 0.109.55μg·kg(LOD)和 0.3533.43μg·kg(LOQ),方法回收率为 75%~110%,相对标准偏差(RSD)小于 20%。方法精密度采用添加混合标准溶液的方式进行评价,在 100μg·kg 浓度水平下,相对标准偏差(RSDr)小于 20%,相对重复性(RSDR)小于 20%。基质效应在可接受范围内,除个别农药外,和番茄基质中均未观察到明显的基质增强或抑制效应。对 77 种农药的测量不确定度进行了评估,结果表明该方法适用于市售和田间蔬菜中多类农药残留的检测。