液相色谱串联质谱法测定黄瓜中苯醚菌酯残留量  

Determination of Bemystrobin Residues in Cucumber by Liquid Chromatography-tandem Mass Spectrometry

作　　者：张闯 王永芳 刘姗姗 潘红蕊 ZHANG Chuang;WANG Yong-fang;LIU Shan-shan;PAN Hong-rui(Tianjin Customs Industrial Product Safety Technology Center,Tianjin 300457,China;Tianjin Customs Animal and Plant Food Testing Center,Tianjin 300457,China)

机构地区：[1]天津海关工业产品安全技术中心,天津300457 [2]天津海关动植物食品检测中心,天津300457

出　　处：《化学试剂》2024年第12期103-108,共6页Chemical Reagents

摘　　要：首次建立液相色谱-串联质谱(LC-MS/MS)法测定黄瓜中苯醚菌酯残留量的方法。选择QuEChERS(快速、简单、便宜、高效、耐用、安全)前处理方法进行样品提取、净化,经C18色谱柱进行色谱分离和分析,以乙腈和0.1%甲酸水为流动相进行梯度洗脱,正离子(ESI+)多反应监测模式(MRM)监测,采用基质标准曲线外标法进行定量。结果表明在10~200μg/kg范围内线性关系良好,相关系数R 2>0.99。方法的定量限为10μg/kg,检出限为4μg/kg。在空白黄瓜基质中添加10、40、100μg/kg 3个浓度进行加标回收实验,回收率在76.6%~91.3%范围内,相对标准偏差在3.7%~8.3%范围内。检测方法简便、快速、准确、灵敏度高,适用于黄瓜中苯醚菌酯残留量的测定。A method for the determination of bemystrobin residues in cucumber by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established for the first time.QuEChERS(quick,simple,cheap,efficient,durable,and safe)pretreatment method was selected for sample extraction and purification.The chromatographic separation and analysis were performed on a C18 column.Acetonitrile and 0.1%formic acid water were used as the mobile phases for gradient elution.Positive ion(ESI^(+))multi-reaction monitoring mode(MRM)was employed,and the matrix standard curve external standard method was used for quantification.The results showed that the linear relationship was good in the range of 10~200μg/kg with the correlation coefficient R^(2)>0.99.The limit of quantification was 10μg/kg,and the detection limit was 4μg/kg.Three concentrations of 10,40,and 100μg/kg were added to the blank cucumber matrix for spiked recovery experiments.The recovery rates were in the range of 76.6%~91.3%,and the relative standard deviations were in the range of 3.7%~8.3%.The detection method is simple,rapid,accurate,and highly sensitive,which is suitable for the determination of bemystrobin residues in cucumber.

关 键 词：苯醚菌酯 液相色谱-串联质谱 黄瓜 QUECHERS ESI+ 

分 类 号：O657.63[理学—分析化学]