摘要
目的以QuEChERS-SPE为前处理方法,UHPLC-MS/MS为检测仪器,建立瓜蒌中156种农药残留的快速筛查检测方法。方法采用1%冰乙酸乙腈溶液提取样品,以无水硫酸镁(Mg SO4)为脱水剂,经Mg SO4、丙基乙二胺(PSA)、C18混合净化剂简单净化,再通过SPE小柱(Waters Prime HLB,3 m L,60 mg)进一步净化,Waters Cortecs C18+柱(100 mm×2.1 mm,1.6μm)分离,采用UHPLC-MS/MS多反应监测(MRM)模式进行定性和定量分析。结果 156种农药在5~200μg·L-1内线性关系良好(r>0.995),平均回收率范围为74.9%~116.4%,RSD为1.0%~5.6%,方法的检出限为0.02~20μg·kg^(-1),定量限为0.06~50μg·kg^(-1)。结论该方法简单、准确、灵敏度高,适合于瓜蒌中多农药残留的同时筛查测定。
OBJECTIVE To develope a multi-residue analytical method for the determination of 156 kinds of pesticide residues in Trichosanthis Fructus by QuEChERS-SPE-UHPLC-MS/MS. METHODS The samples were extracted with acetonitrile containing 1% acetic acid, dehydrated by Mg SO4, simply purified by a mixed cleaning agents of Mg SO4, PSA, and C18, and further cleaned by SPE column（Waters Prime HLB, 3 m L, 60 mg）, separated on a Waters Cortecs C18＋ column（100 mm×2.1 mm, 1.6 μm） and detected by UHPLC-MS/MS with positive and multiple reaction monitoring mode（MRM）. RESULTS The results of all the 156 kinds pesticides showed good linearity in the range of 5-200 μg·L-1（r0.995）. The average recoveries ranged from 74.9% to 116.4%, with the relative standard deviations（RSDs） from 1.0% to 5.6%, the limits of detection（LODs） of the method were among 0.02-20 μg·kg^（-1）, and the limits of quantification（LOQs） were among 0.06-50 μg·kg^（-1）. CONCLUSION The method is simple, accurate and sensitive, can be used for the determination of multi type pesticides in Trichosanthis Fructus.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2018年第1期17-23,共7页
Chinese Journal of Modern Applied Pharmacy
基金
"重大新药创制"国家科技重大专项(2014ZX09304307-002)
山东省中医药科技发展计划项目(2015-160)
