QuEChERS-SPE-UHPLC-MS/MS测定瓜蒌中156种农药残留

Determination of 156 Pesticide Residues in Trichosanthis Fructus by QuEChERS-SPE-UHPLC-MS/MS

关键词:  QuEChERS  SPE  超高效液相色谱-串联质谱  农药残留  瓜蒌

Key words:  QuEChERS  SPE  UHPLC-MS/MS  pesticide residues  Trichosanthis Fructus

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（MgSO₄）为脱水剂，经MgSO₄、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 mL，60 mg）进一步净化，Waters Cortecs C₁₈+柱（100 mm×2.1 mm，1.6 μm）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5~200 μg·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0.02~20 μg·kg^-1，定量限为0.06~50 μg·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。

Abstract:

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 MgSO₄, simply purified by a mixed cleaning agents of MgSO₄, PSA, and C₁₈, and further cleaned by SPE column(Waters Prime HLB, 3 mL, 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(r<0.995). 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.