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Journal of Tea Science ›› 2014, Vol. 34 ›› Issue (3): 271-278.doi: 10.13305/j.cnki.jts.2014.03.009

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

LIU Yanhui1,2, YU Changhong3,*, LIU Yan4, LIU Jian1,2, ZHANG Ting4   

  1. 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
  • Received:2013-09-02 Revised:2013-10-21 Online:2014-06-15 Published:2019-09-03

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.

Key words: tea, matrix solid-phase disperse extraction, HPLC-MS-MS, pesticide residues

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