通过式固相萃取结合高效液相色谱-串联质谱法测定石斛中9种农药残留

Determination of Nine Pesticides Residues in Dendrobii Caulis by Pass-through Solid Phase Extraction Cleanup and Liquid Chromatography-tandem Mass Spectrometry

目的建立了通过式固相萃取结合高效液相色谱-串联质谱法测定石斛栽培过程可能使用的9种农药。方法样品用0.1%甲酸乙腈提取,上清液经通过式固相萃取小柱Oasis PRIME HLB净化,Waters HSS T3-C_(18)色谱柱(2.1×100 mm,1.8μm)分离后,采用串联质谱正离子多反应监测模式(MRM)进行测定。结果结果显示9种农药在各自的质量浓度范围内线性良好,相关系数r均大于0.99,平均加标回收率在72.1%~98.5%之间,RSD为3.1%~10.4%。结论该方法前处理操作快速简单、检测灵敏度高、结果测定准确,适用于种植石斛过程9种农药残留量的质量安全检测和控制。

OBJECTIVE A method was developde for determination of nine possible pesticides used in the cultivation process of Dendrobii Caulis by Pass-through Solid Phase Extraction Cleanup and Liquid Chromatography-tandem Mass Spectrometry.METHODS The analyses were extracted by acetonitrile solution(contain 0.1%formic acid)and purified by Oasis PRIME HLBsolid phase extraction column.Separation was performed on Waters HSS T3-C_(18)column(2.1×100 mm,1.8μm),Determination using tandem mass spectrometry positive ion multi reaction monitoring(MRM)mode.RESULTS Results showed that there were good linear relationships for the ninepesticides in their respective concentration with correlation coefficients greater than 0.99,The mean recoveries ranged from 78.9%to 102.4%,and the relative standard derivations(RSDs)were within 3.1%-10.4%.CONCLUSION The proposed method to be simple,sensitive and reliable,and Suitable for quality and safety testing and control of 9 pesticide residues during the process of planting Dendrobium.