分散固相萃取-气相色谱-串联质谱法测定茉莉花茶中86种农药残留

Determination of 86 Pesticide Residues in Jasmine Tea by Dispersive Solid-Phase Extraction Combined with Gas Chromatography-Tandem Mass Spectrometry

以QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)法为前处理技术,优化净化吸附剂组合和用量,改进净化方式,并以气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)法为检测手段,建立茉莉花茶中86种农药残留筛查检测方法。样品用乙腈提取,提取液经饱和的氯化钠溶液萃取,取有机相,转移至装有混合吸附剂和有机滤膜的针筒中完成净化与过滤,GC-MS/MS测定,外标法定量。86种农药线性范围在5~400μg/kg之间线性关系良好,相关系数(r^2)在0.98以上,方法定量限为0.1~8.0μg/kg。当添加水平为80μg/kg时,91.8%的农药平均加标回收率在70.1%~116.0%之间,相对标准偏差为1.9%~11.4%。

A multi-residue method for the simultaneous determination of 86 pesticide residues in jasmine tea was developed based on optimized quick,easy,cheap,effective,rugged,and safe（QuEChERS） with an improved cleanup procedure using optimized sorbent mixture by gas chromatography-tandem mass spectrometry（GC-MS/MS）.Samples were extracted with acetonitrile,and the extracts were cleaned up by liquid-liquid extraction with saturated sodium chloride aqueous solution.Then,the organic phase was transferred into a cylinder filled with a hybrid adsorbent and an organic membrane filter for cleanup and filtration and determinated by GC-MS/MS with an external standard method.The linear range of the developed method was from 5 to 400 μg/kg with correlation coefficients（r^2） of more than 0.98.The limits of quantification（LOQs） for the tested pesticides were determinated to be in the range between 0.1 and 8.0μg/kg.The recoveries of 91.8% of the 86 pesticides at the spiked levels of 80 μg/kg ranged from 70.1% to 116.0%,with relative standard deviations（RSDs） between 1.9% and 11.4% for all the pesticides.