Environmental Chemistry

ISSN 0254-6108

CN 11-1844/X

Vol. 38 No. 5
May  2019
Article Contents

Citation:

Determination of 26 pesticides in surface water by solid phase extraction-ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry

  • Received Date: 2018-11-30
    Fund Project:

    Supported by the National Key Research and Development Program of China (2017YFC1601606) and the Science Foundation of the Fujian Province (2016J05045).

  • A rapid method for the screening and determination of 26 pesticides was developed based on solid phase extraction and ultrahigh performance liquid chromatography (UHPLC)-quadrupole time-of-flight mass spectrometry (Q-TOF/MS). Initially, a database containing the accurate mass, retention time and the MS/MS spectra of the 26 pesticides was established. Based on the above database, the qualitative identifications of the 26 pesticides in surface water were accomplished without comparison with the standard substances. The target compounds in real water samples were first enriched by solid phase extraction cartridges and then eluted out of the cartridges using acetonitrile/isopropanol solution (1:1). The resultant samples were then loaded onto a reversed phase C18 column and subjected to separation under gradient elution using 0.1% formic acid in methanol and 0.1% formic acid in water (with 10 mmol·L-1 ammonium acetate) as binary mobile phases, further detected using UHPLC-Q-TOF/MS, and quantificated by external standard method. It was demonstrated that in the studied concentration range, all 26 pesticides exhibited very good linearity with the linear correlation coefficients all higher than 0.994. The recoveries ranged from 67.74% to 112.3% with the relative standard deviations (RSD) between 0.45% and 12.2%.
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Determination of 26 pesticides in surface water by solid phase extraction-ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry

  • 1. Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen, 361026, China;
  • 2. The Inspection Technical Center of Chongqing Entry-Exit Inspection & Quarantine Bureau, Chongqing, 400020, China;
  • 3. Agilent Technologies(China) Co., Ltd, Beijing, 100102, China
Fund Project:  Supported by the National Key Research and Development Program of China (2017YFC1601606) and the Science Foundation of the Fujian Province (2016J05045).

Abstract: A rapid method for the screening and determination of 26 pesticides was developed based on solid phase extraction and ultrahigh performance liquid chromatography (UHPLC)-quadrupole time-of-flight mass spectrometry (Q-TOF/MS). Initially, a database containing the accurate mass, retention time and the MS/MS spectra of the 26 pesticides was established. Based on the above database, the qualitative identifications of the 26 pesticides in surface water were accomplished without comparison with the standard substances. The target compounds in real water samples were first enriched by solid phase extraction cartridges and then eluted out of the cartridges using acetonitrile/isopropanol solution (1:1). The resultant samples were then loaded onto a reversed phase C18 column and subjected to separation under gradient elution using 0.1% formic acid in methanol and 0.1% formic acid in water (with 10 mmol·L-1 ammonium acetate) as binary mobile phases, further detected using UHPLC-Q-TOF/MS, and quantificated by external standard method. It was demonstrated that in the studied concentration range, all 26 pesticides exhibited very good linearity with the linear correlation coefficients all higher than 0.994. The recoveries ranged from 67.74% to 112.3% with the relative standard deviations (RSD) between 0.45% and 12.2%.

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