Evaluation of QuEChERS Method for the Analysis of 15 Triazole Pesticides Residues in Fruits by Online Gel Permeation Chromatography Gas Chromatography-Mass Spectrometry
  
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KeyWord:QuEChERS  online gel permeation chromatography/gas chromatography-mass spectrometry(GPC/GC-MS)  triazole pesticides  matrix effects  fruits
  
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LI Hai-fei,NIE Ji-yun*,XU Guo-feng,LI Jing,YAN Zhen,LI Zhi-xia,WU Yong-long,KUANG Li-xue 中国农业科学院果树研究所,农业部果品质量安全风险评估实验室(兴城),农业部果品及苗木质量监督检验测试中心(兴城)
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Abstract:
      A comparison was made among three versions of QuEChERS sample preparation methods for the extraction of 15 triazole pesticides in fruits.The three QuEChERS methods were the original method without buffer,the AOAC Official Method 2007.01 with acetate buffer,and the CEN 15662 Method with citrate buffer.The clean-up effects of primary secondary amine(PSA) sorbent and C18 sorbent on 15 triazole pesticides were studied.The addition method after extraction was used to evaluate the matrix effects of triazole pesticide in matrix of apple,pear,peach,grape,cherry,banana and orange during gel permeation chromatography coupled to gas chromatography-mass spectrometry(GPC/GC-MS) analysis.As a result,the QuEChERS method without buffer gave good recoveries for 15 triazole pesticides. The cleaning up effect of PSA plus C18 is superior to that of C18 or PSA sorbent.The matrix effects were intensive in the 7 kinds of fruits.In this article,15 triazole pesticides were extracted by the QuEChERS method without buffer,and analysed by using matrix-matched standard calibration as the external standard method with gas chromatography-mass spectrometry in selective ion monitoring(SIM) mode.Moreover,a large volume of sample was allowed to be injected using the program of GPC programmed temperature vaporizer of gas chromatography to improve the sensitivity of measurements.The recoveries of 15 residues in 7 matrixes at three spiked levels of 20,50,100μg/kg ranged from 85.7% to 120.1% with relative standard deviations of 0.2%-11.5%.The calibration curves were linear(r>0.998) in the range of 10-400μg/L for all the pesticides.The limits of detection(LOD) for the pesticides in fruits ranged from 0.9μg/kg to 9.5μg/kg.Based on these results,the analytical method was proved to be highly efficient,robust and sensitive,and was suitable for monitoring 15 triazole pesticides residues in fruits.
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