| 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 |
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| 引用本文： | 刘妍慧,于常红,刘岩,刘健,张婷.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[J].茶叶科学,2014,34(3):271-278. |
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| 作者姓名： | 刘妍慧 于常红 刘岩 刘健 张婷 |
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| 作者单位： | 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 |
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| 基金项目： | 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） |
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| 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0.1~1.7 μg·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10~400 μg·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1.7~339.4 μg·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。
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| 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 |
| 收稿时间： | 2013-09-02 |
Simultaneous Determination of 11 Kinds of Pesticide Residues in Tea by HPLC-MS-MS |
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| LIU Yanhui,YU Changhong,LIU Yan,LIU Jian,ZHANG Ting.Simultaneous Determination of 11 Kinds of Pesticide Residues in Tea by HPLC-MS-MS[J].Journal of Tea Science,2014,34(3):271-278. |
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| Authors: | LIU Yanhui YU Changhong LIU Yan LIU Jian ZHANG Ting |
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| Institution: | 1. College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China; 2. Key Lab of Ocean Environment and Ecology, Ministry of Education, Ocean University of China, Qingdao 266100, China; 3. Medical School,Qingdao University, Qingdao 266071, China; 4. Shandong Provincial Key Laboratory of Ocean Environment Monitoring Technology, Institute of Oceanographic Instrumentation, Shandong Academy of Sciences, Qingdao 266001, China |
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| Abstract: | 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 0.1-1.7 μg·kg-1. The correlation rate was more than 0.9995. The average recoveries (spiked at the levels of 10-400 μg·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 1.7-339.4 μg·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. |
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| Keywords: | tea matrix solid-phase disperse extraction HPLC-MS-MS pesticide residues |
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