FOOD SCIENCE ›› 2010, Vol. 31 ›› Issue (24): 277-280.doi: 10.7506/spkx1002-6630-201024059

• Analysis & Detection • Previous Articles     Next Articles

Determination of 3, 5, 6-Trichloro-2-pyridinol in Vegetables by Gas Chromatography-Mass Spectrometry

XIE Juan1,2，WANG Yan-hong1,*，WANG Shi-cheng1，ZHANG Hong1，WANG Ying1，WANG Shan-shan1   

  1. 1. Institute of Applied Ecology, Chinese Academy of Sciences, Shenyang 110016, China ；
    2. Graduate University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2010-02-03 Revised:2010-10-26 Online:2010-12-25 Published:2010-12-29
  • Contact: WANG Yan-hong E-mail:wangyh@iae.ac.cn

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Abstract:

A gas chromatography-mass spectrometry (GC-MS) method was established for the determination of 3,5,6- trichloro-2-pyridinol (TCP), a kind of metabolite of chlorpyrifos in vegetables. The sample was extracted by acetone, and the extract was purified using hexane and DCM. The water was removed with anhydrous sodium sulfate. After condensation, the extract was dissolved into 1 mL of ethyl acetate and then derivatized with N-(tert-butyldimethylsilyl)-methyltrifluoroacetamide (MTBSTFA), and finally the volume was adjusted to 1 mL using hexane. The analyte was detected by GC-MS, and an external standard method was used for quantifying TCP. The limit of detection was 8.3μg/kg, and the recovery rates of spiked sample were in the range of 70.4% － 107.6% with relative standard deviation of 4.3% － 8.7%. An excellent linear relationship was achieved in the range of 5－500μg/L with correlation coefficients over 0.99. This method is characteristics of accuracy, easy operation and can be applied for determining TCP in vegetables.

Key words: gas chromatography-mass spectrometry(GC-MS), 3,5,6-trichloro-2-pyridinol, vegetables

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