基质固相分散萃取-高效液相色谱串联质谱法(HPLC-MS-MS)同时测定茶叶中11种农药的残留量  

Simultaneous Determination of 11 Kinds of Pesticide Residues in Tea by HPLC-MS-MS

作　　者：刘妍慧[1,2] 于常红[3] 刘岩[4] 刘健[1,2] 张婷[4] 

机构地区：[1]中国海洋大学环境科学与工程学院,山东青岛266100 [2]中国海洋大学海洋环境与生态教育部重点实验室,山东青岛266100 [3]青岛大学医学院,山东青岛266071 [4]山东省科学院海洋仪器仪表研究所山东省海洋环境监测技术重点实验室,山东青岛266001

出　　处：《茶叶科学》2014年第3期271-278,共8页Journal of Tea Science

基　　金：青岛市科技发展计划项目(13-1-3-129-nsh);山东省自然科学基金(ZR2013DL008);山东省高等学校科技计划项目(J11LF20);山东省优秀中青年科学家科研奖励基金(BS2011YY001)

摘　　要：建立了茶叶中3类11种农药的分散固相萃取-高效液相色谱串联质谱（HPLC-MS-MS）的检测方法。茶叶样品以乙腈-乙酸（体积比99∶1）提取,以PSA为净化剂基质固相分散萃取,然后通过C18色谱柱,以甲醇/水（含甲酸铵）溶液进行梯度洗脱,采用电离喷雾电离方式（ESI＋）,通过多反应监测（MRM）定量。结果表明：11种农药的分析时间约为20 min,在0～500 ng·mL-1范围内线性相关,相关系数大于0.9995,方法检测限为0.1～1.7μg·kg-1。测定了茶叶样品中11种农药的残留量,加标回收率为62.4%～114.8%（添加水平分别为10～400μg·kg-1）,相对标准偏差（RSD）为3.28%～19.34%。选取了5个不同类型的茶叶样品,检测其中11种农药的残留量,检出结果差异较大。其中绿茶中11种农药的检出量为1.7～339.4μg·kg-1,加标回收率为86.1%～104.1%,相对标准偏差（RSD）均小于20%（n=6）。本方法准确、灵敏、简单、快速、安全,能满足茶叶样品中多种农药残留分析的要求。A method for rapid determination of 11 kinds of pesticide residues in tea samples by matrix solid-phase disperse extraction and high performance liquid chromatography and tandem mass spectrometry was proposed. The pesticide residues in tea sample were firstly extracted by a mixture of V（acetonitrile）∶V（acetic acid）=99∶1, and the extract was solid-phase disperse purified by PSA and then separated on a Waters Xterra MS C18 column with a gradient system of a mixture of methanol and water with ammonium formate. Multi-reaction monitoring （MRM） was employed for quantitative determination. Eleven pesticide residues could be detected within 20 min. The linear range of 11 pesticide residue was 0-500 ng·mL-1 and the limits of detection were between 0.1-1.7μg·kg-1. The correlation rate was more than 0.9995. The average recoveries （spiked at the levels of 10-400μg·kg-1） ranged from 62.4% to 114.8% with relative standard deviation between 3.28% and 19.34%. After extraction and purification, 11 pesticide residues in 5 samples of different kinds of tea with significant variation in content were analyzed. And the residue content of 11 pesticides in green tea sample was 1.7-339.4μg·kg-1. Recoveries in this sample were ranged from 86.1%to 104.1%with relative standard deviations less than 20%. This method is accurate, sensitive, simple, rapid, safe and suitable for identification and quantification of multiple pesticide residues in tea.

关 键 词：茶叶 基质固相分散萃取 高效液相色谱串联质谱 农药残留 

分 类 号：O657.63[理学—分析化学] TS272[理学—化学]