GC-MS/MS法和LC-MS/MS法对玉竹根茎和白茅根茎中224种农药多残留的测定

目的：建立玉竹根茎及白茅根茎中农药多残留的检测方法。方法：以乙腈为溶剂，高速匀浆提取，检测方法：气相色谱-串联质谱法，采用DB17MS弹性石英毛细管柱（30 m×0.25 mm×0.25 μm），电子轰击电离源（EI）；液相色谱-串联质谱法，采用十八烷基硅烷键合硅胶柱（CORTECSTM UPLC C₁₈，2.1 mm×150 mm，1.6 μm），以0.1%甲酸（含5 mmol·L^-1甲酸铵）溶液和95%乙腈（含5 mmol·L^-1甲酸铵、0.1%甲酸）溶液为流动相，电喷雾电离源（ESI），正离子模式下多反应监测（MRM）。结果：224种农药质量浓度在1~100ng·mL^-1范围内线性关系良好，相关系数在0.99以上的占95%，高、中、低三水平回收率试验（0.01、0.1、0.5 mg·kg^-1）98%的回收率在67.5%~121.0%之间，RSD在1.9%~20.8%之间。结论：本方法能快速有效地检测玉竹根茎和白茅根茎中的农药多残留，为其他药用植物中的农残检测提供借鉴。

Objective: To establish a method for the determination of pesticide residues in fragrant solomonseal rhizome and cogongrass rhizome.Methods: The samples were extracted with acetonitrile by high speed homogenizer. GC-MS/MS analysis was performed on a DB17MS(30 m×0.25 mm×0.25 μm) capillary column with electron impact(EI) source.An LC-MS/MS analysis was performed on a CORTECSTM UPLC C₁₈(2.1 mm×150 mm,1.6 μm) column with isocratic elution of 0.1% formic acid(containing 5 mmol·L^-1 ammonium formate) and 95% acetonitrile(containing 5 mmol·L^-1 ammonium formate and 0.1% formic acid).Electrospray ionization(ESI) source was applied by positive ionization in multiple reaction monitoring(MRM) modes.Results: The calibration curves of 224 pesticide residues showed good linearity in the ranges of 1-100 ng·mL^-1 with 95% of correlation coefficients above 0.99. The average recoveries at spiked levels of 0.01,0.1,0.5 mg·kg^-1 for all target compounds in the range of 67.5%-121.0% were 98% with relative standard deviations of 1.9%-20.8%.Conclusion: The method is fast,accurate and highly sensitive for the screening and confirmation of pesticide residues in fragrant solomonseal rhizome and cogongrass rhizome,which provides a basis for the pesticide residues control of other medicinal plants.