基质分散固相萃取和超高效液相色谱-串联质谱法测定水果、蔬菜中的11种杀菌剂

目的 建立水果、蔬菜中11种杀菌剂的基质分散固相萃取-液相色谱-串联质谱分析方法。方法 样品中的杀菌剂经乙腈提取,以PSA、石墨化炭黑和C18为吸附剂的基质分散固相萃取净化,最后用C18柱分离,以乙腈和0.05%甲酸水为流动相,经电喷雾离子源(ESI+)电离,多反应监测(MRM)模式串联质谱检测。结果 腐霉利的检测线性范围为10~500ng/ml,检出限为10μg/kg,其余10种杀菌剂的检测线性范围1.0~50ng/ml,检出限为1μg/kg;11中杀菌剂的平均加标回收率在80.3%~115.6%之间,相对标准偏差在3.9%~11.2%之间。结论 该方法前处理简单、快速、有效、准确灵敏、稳定和安全,适合于水果蔬菜中11种杀菌剂的检测。

Determination of 11 fungicides in fruits and vegetables by matrix dispersive solid phase extraction and UPLC-MS/MS method

Objective To develop a method for determination of 11 fungicide residues in fruits and vegetables by matrix dispersive solid phase extraction and UPLC-MS/MS.Methods The fungicides in fruits and vegetables were extracted with acetonitrile,purified with matrix dispersive solid phase extraction using PSA,GCB and C18 as adsorbents.The sample solution was separated on PhenomenexC18 (150mm×3.0mm,size 1.7 μm) with gradient elution using acetronitrile-0.05% formic acid as mobile phase and detected by MS/MS using positive electrospray ionization (ESI+) under the multiple reaction monitoring(MRM).Results The linear range of procymidone was 10~500ng/ml with the limit of detection (LOD) of 10μg/kg.The linear ranges of other ten fungicide were 1.0~50ng/ml and all the LODs were 1μg/kg.The average recoveries were in the range of 80.3%-115.6%,with relative standard deviations (RSD) of 3.9%~11.2%.Conclusion The method is simple,time-saving,accurate and sensitive.It is suitable for detection of 11 fungicides residue in fruits and vegetables.