超高效液相色谱串联质谱法测定植物源性食品中杀螟丹的残留  

Determination of Cartap Residue in Plant-Based Foods by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：林凯旋 沈佳乐 王慧凯 林德民 沈炜 LIN Kaixuan;SHEN Jiale;WANG Huikai;LIN Demin;SHEN Wei(Zhejiang Chemical Products Quality Inspection Co.,Ltd.,Hangzhou,Zhejiang 310023,China)

机构地区：[1]浙江省化工产品质量检验站有限公司,浙江杭州310023

出　　处：《浙江化工》2024年第9期48-54,共7页Zhejiang Chemical Industry

摘　　要：利用三重四极杆液相色谱-质谱联用技术对不同植物源性食品中杀螟丹进行定性、定量分析,通过对杀螟丹提取和净化条件进行筛选与优化,建立了植物源性食品中杀螟丹快速、便捷、准确、高效的分析方法。色谱柱选择ZORBAX SB-C18(2.1 mm×100 mm,3.5μm),流动相为水(0.1%甲酸)和甲醇,梯度洗脱,流速为0.3 mL/min,采用多反应监测模式(MRM),电喷雾离子源(ESI)选择正离子模式,定量离子对为238.1/149.9。样品经2%乙酸乙腈提取,QuEChERS法净化,过膜后直接测定,外标法定量。结果表明,目标物在5~200 ng/mL范围内线性关系良好,决定系数(R2)=0.9992,样品加标回收率为72%~86%,精密度试验相对标准偏差为0.7%~6.3%。该方法适用性广、操作便捷、回收率好、精密度高,可用于植物源性食品中杀螟丹残留的测定。Using triple quadrupole liquid chromatography-mass spectrometry technology,qualitative and quantitative analysis of cartap in different plant-based foods was carried out.By screening and optimizing the extraction and purification conditions of cartap,a rapid,convenient,accurate and efficient analysis method for cartap in plant-based foods was established.The chromatographic column was ZORBAX SB-C18(2.1 mm×100 mm,3.5μm),the mobile phase was water(0.1%formic acid)and methanol,the gradient elution flow rate was 0.3 mL/min,the multi reaction monitoring mode(MRM)was used,the positive ion mode was selected for the electric spray ion source(ESI),and the quantitative ion pair was 238.1/149.9.The sample was extracted with 2%acetic acid acetonitrile,purified by QuEChERS method,directly measured after membrane filtration,and quantified by external standard method.The results showed that the linear relationship of the target substance was good within the range of 5~200 ng/mL,with a determination coefficient(R2)of 0.9992.The recovery rate of the sample spiked was 72%~86%,and the relative standard deviation of the precision test was 0.7%~6.3%.This method has wide applicability,convenient operation,good recovery rate,and high precision,and can be used for the determination of residual cartap in plant-based foods.

关 键 词：植物源 食品 杀螟丹 残留 三重四级杆液质联用仪 QUECHERS 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]