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
祝子铜 1雷美康 1姜芝英 1黄超群 2叶有标 1陈玉娇 1韩超3
作者信息
- 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
- 折叠
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 100.0 μg/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.
Abstract
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 100.0 μg/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Key words
plant-derived product/highly polar fungicide/high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/isotopically labelled internal standard method引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据