基质固相分散-超高效液相色谱-串联质谱法检测蔬菜中残留的苯甲酰脲类和双酰肼类杀虫剂

建立了基质固相分散技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中苯甲酰脲类杀虫剂(除虫脲、灭幼脲、杀铃脲、氟苯脲、氟虫脲、氟啶脲、氟铃脲)和双酰肼类杀虫剂(甲氧虫酰肼、虫酰肼)的方法。蔬菜样品经中性氧化铝和石墨化炭黑研磨,乙酸乙酯淋洗,洗脱液浓缩定容后,经超高效液相色谱分离,分别在正、负离子多反应监测(MRM)模式下用电喷雾电离串联质谱测定,外标法定量。结果表明,9种杀虫剂在1～100 μg/L质量浓度范围内有良好的线性关系(R2≥0.99);在1、5、10、100 μg/kg 4个加标水平上的回收率为78.5%～112.8%;相对标准偏差为2.3%～10.2%,检出限为0.5～1.0 μg/kg。该方法操作简便快速,样品和溶剂用量少,检出限低,可满足蔬菜中苯甲酰脲类和双酰肼类杀虫剂同时检测的要求。

Determination of benzoylurea and bishydrazide pesticide residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry with matrix solid phase dispersion

A method for the determination of nine pesticides including benzoylureas (diflubenzuron,chlorobenzuron,triflumuron,teflubenzuron,flufenoxuron,chlorfluazuron,hexaflumuron) and bishydrazides (methoxyfenozide,tebufenozide) in vegetables was developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with matrix solid phase dispersion.The sample was graphitized with neutral alumina as dispersant and carbon black as purifying,and eluted with ethyl acetate.The separation was achieve...