超高效液相色谱--串联质谱法测定水样中吡虫啉及其代谢物残留

Rapid Determination of Imdacloprid and Its Five Metabolites in Environmental Water by Direct Injection-ultra Performance Liquid Chromatography—triple Quadrupole Mass Spectrometry

建立了一种简便、直接进样的超高效液相色谱—串联质谱(UPLC-MS/MS)快速测定水样中吡虫啉及其5种代谢物检测方法。环境水样经0.22μm滤膜过滤后,滤液直接定量分析。结果表明:水样中吡虫啉、吡虫啉胍、吡虫啉脲、烯式吡虫啉、5-羟基吡虫啉、6-氯烟酸的在2~100μg/L范围内相关系数(r)均大于0.999,线性关系良好,方法检出限为0.05~0.35μg/L;实际水样在低、中、高3种加标水平下,平均加标回收率为70.0%~100%,相对标准偏差在2.6%~8.0%。本方法分析速度快、灵敏度高,重现性好,适用于水中吡虫啉及其5种代谢物的快速测定。

A simple and direct injection method for the rapid determination of imidacloprid and its five metabolites in water samples by UPLC-MS/MS was developed.The environmental water sample was filtered by a 0.22μm filter membrane,and the filtrate was directly quantitatively analyzed.The results showed that the correlation coefficients(r)of imidacloprid,imidaclopridine,imidacloprilurea,eneimidacloprid,5-hydroxy-imidacloprid and 6-chloronicotinic acid in water samples were all greater than 0.999 in the range of 2-100μg/L,and the detection limits of the method were 0.05-0.35μg/L.The average recoveries of water samples were 70.0%~100%and the relative standard deviations(RSD)were 2.6%~8.0%under three spiked levels.This method is rapid,sensitive and reproducible for the rapid determination of imidacloprid and its five metabolites in water.