超高效液相色谱-串联质谱法测定蔬菜中9种氨基甲酸酯类农药残留

Determination of nine kinds of carbamate pesticide residues in vegetables by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry

目的 建立同时测定蔬菜中9种氨基甲酸酯类农药残留的超高效液相色谱-串联质谱分析方法。方法 蔬菜样品粉碎后用乙腈超声提取,经过QuEChERS(快速、简单、低廉、有效、稳定、安全的预处理方法)分离净化后通过Xbridge C18色谱柱(2.1 mm×100 mm,1.8μm),以0.05%甲酸的水溶液-乙腈为流动相进行梯度洗脱,采用电喷雾离子源(ESI)和多反应监测(MRM)模式进行质谱分析,对样品前处理和仪器条件进行优化,探究方法的各项特征指标。结果9种氨基甲酸酯类农药在5~100μg/L浓度范围内线性关系良好,相关系数的平方(r2)均大于0.997 0,加标回收率为86.1%~95.1%,相对标准偏差(RSD)为3.5%~7.2%(n=6),方法检出限为0.000 5 mg/kg~0.02 mg/kg。结论 超高效液相色谱-串联质谱法可以快速、简单、准确的同时测定蔬菜中9种氨基甲酸酯类农药残留,具有稳定性好、灵敏度高等优点。

Objective To establish a method for simultaneous determination of nine carbamate pesticide residues in vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry.Methods After crushing,the vegetable samples were extracted with acetonitrile,separated and purified by QuEChERS method(fast,simple,cheap,effective,stable and safe pretreatment method),and then passed through XBridge C18 chromatographic column(2.1 mm×100 mm,1.8 μm).The gradient elution was carried out with 0.05% formic acid and acetonitrile aqueous solution as mobile phase,mass spectrometry was carried out with electrospray ion source(ESI) and multi reaction monitoring(MRM) mode,sample pretreatment and instrument conditions were optimized,and various characteristic indexes of the method were explored.Results The nine carbamate pesticides showed good linear relationship in the range between 5-100 μg/L,and the squares of correlation coefficients(r2) were all greater than 0.997 0.The recoveries were 86.1%-95.1%,the relative standard deviation(RSD) was 3.5%-7.2%(n=6),and the detection limit of the method was 0.000 5-0.02 mg/kg.Conclusion The established method by ultra-high performance liquid chromatography-tandem mass can be used for rapid,simple and accurate simultaneous determination of nine carbamate pesticide residues in vegetables.It has the advantages of good stability and high sensitivity.