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目的建立N-丙基乙二胺(PSA)-高效液相-三重四极杆串联质谱(HPLC-QQQ-MS/MS)法测定浙贝母中有机磷等12种农药残留的方法,并收集主产地浙江等地20批浙贝母样品进行农药残留测定。方法浙贝母样品加乙腈提取,过PSA柱净化,采用LC-QQQ-MS/MS方法在多反应监测(MRM)模式下测定,内标法定量。结果 12种农药成分在相应的测定范围内线性关系良好,相关系数在0.998 6~0.999 8,12种农药在90、300、900 ng/mL 3个添加水平下,加样回收率范围为68.1%~108.0%,RSD为1.1%~6.1%,各农药的检出限在0.08~1.0μg/kg。结论该方法可应用于浙贝母药材中12种农药残留成分的同时检测。浙贝母药材农药残留量甚微,符合安全性要求。
Objective To establish a method for the determination of 12 organophosphorus pesticides residues in Fritillaria cirrhosae by high performance liquid chromatography-tandem mass spectrometry (HPLC-QQQ-MS / MS) Zhejiang and other places of origin 20 batches of Fritillaria samples for determination of pesticide residues. Methods The Fritillaria cirrhosa samples were extracted with acetonitrile and purified by a PSA column. The content of the Fritillaria cirrhosa samples was determined by MR-LC-QQQ-MS / MS and quantified by internal standard method. Results The linear relationship of 12 pesticide components in the corresponding range was good with a correlation coefficient of 0.998 6 to 0.999. The recoveries of 12 pesticides at 90, 300 and 900 ng / mL were 68.1% ~ 108.0%, RSD was 1.1% ~ 6.1%, and the detection limit of each pesticide was 0.08 ~ 1.0μg / kg. Conclusion The method can be applied to the simultaneous determination of 12 pesticide residues in Fritillaria cirrhosa. Fritillaria medicinal herbs residues are small, in line with safety requirements.