LC-MS/MS法测定蔬菜和水果中3种杀软体动物剂

Determination of Three Molluscicides in Vegetables and Fruits by LC-MS/MS

建立分散固相萃取,LC-MS/MS法同时检测蔬菜和水果中四聚乙醛、杀虫环、灭梭威3种杀软体动物剂的分析方法。样品经乙腈均质提取,提取液混合使用乙二胺-N-丙基硅烷粉(PSA)和C18吸附剂粉末进行净化;采用XBridgeTMC18(5.0μm;150 mm×2.1 mm)色谱柱分离,多反应监测模式(MRM)分析,外标法定量。结果表明,灭梭威和杀虫环在0.01 mg/L^0.50mg/L,四聚乙醛在0.10 mg/L^1.0 mg/L线性范围内具有良好的线性关系(r=0.999 1~0.999 5)加标浓度在0.010mg/L^0.050mg/kg之间,方法的回收率介于80.5%~101.5%;相对标准偏差(RSD,n=6)介于2.3%~7.5%;检出限均为0.010 mg/kg。该方法前处理简单,净化效果好,具有良好的灵敏度,回收率和重现性。

A method was developed for the analysis of metaldehyde, thiocyclam and methiocarb by LC-MS/MS. The analytes were extracted from the samples using acetonitrile,then purified with PSA＋C18 The three molluscicides were separated on a XBridgeTM C18 （5.0 μm, 150 mm×2.1 mm column） by gradient elution and quatified with exterual standard method by MS/MS under multiple reaction monitoring （MRM） mode. The result indicated that, the calibration curve showed a good linearities for thiocyelam and methioearb in 0.01mg/L-0.50 mg/L, for metaldehyde in 0.10 mg/L-1.00 mg/L （r=0.999 1-0.999 5）.The recoveries of three molluseicides were in the range of 80.5 %-101.5 % at spiked concentration of 0.01 mg/L-0.05 mg/kg with RSDs （n=6） of 2.3 %-7.5 %. The detection limits were all 0.010 mg/kg. The method showed simple preparation, good cleaning effect, high sensitivity and better repeatability.