固相萃取净化-超高效液相色谱-串联质谱法检测茶叶中胺菊酯  

Determination of Tetramethrin in Tea Samples by Solid Phase Extraction and Liquid Chromatography-tandem Mass Spectrometry

作　　者：叶美君[1] 潘胜东[2] 杜颖颖[1] 李文萃[1] 陆小磊[1] 刘相真 YE Mei-jun;PAN Sheng-dong;DU Ying-ying;LI Wen-cui;LU Xiao-lei;LIU Xiang-zhen(Hangzhou Tea Research Institute,CHINA COOP,Hangzhou 310016,China;Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals,Ningbo 315010,China)

机构地区：[1]中华全国供销合作总社杭州茶叶研究院,浙江杭州310016 [2]宁波市疾病预防控制中心,浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010

出　　处：《中国茶叶加工》2021年第4期53-59,共7页China Tea Processing

基　　金：浙江省基础公益研究计划项目(LGC19C200005)。

摘　　要：文章建立了一种基于固相萃取净化-超高效液相色谱-串联质谱法检测茶叶中胺菊酯残留的方法。茶叶样品加入2 g氯化钠,20 mL乙腈(1%醋酸)匀浆提取2次,经石墨化碳黑-氨基复合固相萃取小柱净化,C_(18)色谱柱分离,超高效液相色谱-串联质谱进行定量分析。结果表明,胺菊酯在2.5~400μg/L浓度范围内呈现良好的线性关系,相关系数r^(2)=0.9983方法检出限(LOD)为2.5μg/kg,方法定量限(LOQ)为8.0μg/kg。在8.00μg/kg、30.0μg/kg和100.0μg/kg三个加标水平下,方法回收率为88.88%~109.87%,相对标准偏差(RSD)均小于10%。所建方法简便、快速、灵敏和准确,适用于日常茶叶样品的痕量分析。A method was developed for the determination of tetramethrin residues in dry tea by liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)coupled with solid phase extraction(SPE).Tea samples were firstly extracted with 20 mL acetonitrile(1%HAc)and 2 g NaCl for 2 times by homogenous,and then purified by Carb-NH_(2) SPE column,finally analyzed by UPLC-MS/MS in SRM mode using C_(18) column for separation.The results indicated that tetramethrin showed good linearity in range of 2.5~400μg/L with the correlation coefficient of 0.9983.The limit of detection(LOD)was 2.5μg/kg and the limit of quantity(LOQ)was 8.0μg/kg.The spiked recoveries of tea samples were in the range of 88.88%~109.87%at the three concentrations of 8.00μg/kg、30.0μg/kg and 100μg/kg,respectively,while the relative standard deviations(RSDs)were all less than 10%.The proposed method,which proved to be simple,fast,sensitive,and accurate,can be used for trace analysis of tetramethrin in tea samples.

关 键 词：茶叶 胺菊酯 固相萃取 超高效液相色谱-串联质谱法 痕量分析 

分 类 号：O657.72[理学—分析化学] S571.1[理学—化学]