液相色谱-质谱/质谱法测定植物源性产品中强极性杀菌剂三乙膦酸铝残留  

Determination of Highly Polar Fungicide of Fosetyl-aluminium in Plant-derived Product by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：祝子铜 雷美康 姜芝英 黄超群 叶有标 陈玉娇 韩超 ZHU Zitong;LEI Meikang;JIANG Zhiying;HUANG Chaoqun;YE Youbiao;CHEN Yujiao;HAN Chao(Comprehensive Technology Center of Quzhou Customs,Quzhou 324003,China;Technology Center of Hangzhou Customs District,Hangzhou 310016,China;College of Biology and Environmental Engineering,Zhejiang Shuren University,Hangzhou 310015,China)

机构地区：[1]衢州海关综合技术服务中心,浙江衢州324003 [2]杭州海关技术中心,浙江杭州310016 [3]浙江树人学院,生物与环境工程学院,浙江杭州310015

出　　处：《食品工业科技》2024年第3期235-241,共7页Science and Technology of Food Industry

摘　　要：采用液相色谱-质谱/质谱法结合同位素内标法测定番茄、甘蓝、葡萄、金针菇、大米、花生等植物源性产品中强极性农药三乙膦酸铝。通过对色谱、质谱条件和前处理优化,确定了最佳的实验条件。样品用乙腈进行提取,经HLB固相萃取小柱净化,采用AQ C18柱色谱柱分离,以甲醇和0.15%甲酸溶液为流动相进行梯度洗脱,流速为0.1~0.2 mL/min。质谱采用多反应监测负离子扫描模式,同位素内标标准曲线法定量。三乙膦酸铝在20.0~800.0 ng/mL范围内线性良好,决定系数为0.9904。三乙膦酸铝定量限为100.0μg/kg。对6种植物源性产品进行3个水平加标回收试验,平均回收率范围为69.6%~112.3%,相对标准偏差为1.0%~9.8%。该方法前处理简便,灵敏度高,能满足国内外标准法规对植物源性产品中三乙膦酸铝残留限量的要求。A method was developed for determination of highly polar fungicide fosetyl-aluminium in plant-derived product of tomato,cabbage,grape,flammulina velutipes,rice,peanut by using liquid chromatography-tandem mass spectrometry.The best experimental conditions were established by optimization of chromatogram,mass spectrum and pretreatment.Sample was extracted with acetonitrile and purified by HLB solid phase extraction cartridges.Separation was performed on the AQ C18 column.The mobile phase consisted of methanol and 0.15%formic acid solution.The sample was analyzed by gradient elution and the flow rate was 0.1~0.2 mL/min.The mass spectrometer was operated in the negative ion mode(ESI-)using select reaction monitoring(SRM).Isotopically labelled internal standard calibration curve was used for quantitative analysis.Results showed that there was a good linearity for fosetyl-aluminium in the range of 20.0~800.0 ng/mL with a determination coefficient(r2)of 0.9904.The limit of quantitation in the method was 100.0μg/kg.The average recoveries of fosetyl-aluminium at three levels were in the range of 69.6%~112.3%,the RSDs were 1.0%~9.8%.The method is simple and sensitive,and can meet the requirements of domestic and foreign standards and regulations on the residual limit of fosetyl-aluminium in plant-derived products.

关 键 词：植物源性产品 强极性杀菌剂 液相色谱-质谱/质谱法 同位素内标法 

分 类 号：TS207.3[轻工技术与工程—食品科学]