Simultaneous Determination of 24 Pesticide Residues in Environmental Water Using Solid-phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:solid-phase extraction(SPE)  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  pesticides  water detection
  
AuthorInstitution
HE Xin,MA Yang-fan,ZHAO Hong-xia,NIE Xiao-jing 大连理工大学环境学院,工业生态与环境工程教育部重点实验室
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Abstract:
      A method of solid-phase extraction(SPE) and high performance liquid chromatography-tandem mass spectrometry(SPE/HPLC-MS/MS) was developed for the simultaneous determination of 24 pesticides in water.The samples were extracted with acetonitrile,then enriched and purified with solid-phase extraction cartridges.Acetonitrile and 0.1%(by volume) formic acid aqueous solution were used as mobile phases.Target pesticides were analyzed by HPLC-MS/MS in positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode.Results showed that 24 pesticides were separated in 25 min with excellent linear relationships(r2≥0.998).The recoveries at spiked levels of 5,20,100 μg/L in water samples ranged from 65.9%-127.8% with relative standard deviations(RSDs) of 0.7%-14.2%.The limits of detection were in the range of 0.05-0.71 ng/L.This method was applied in the detection of the water samples from 10 estuaries and 2 reservoirs in Dalian,and 10 pesticides were detected in the concentration range of 0.2-558.3 ng/L.The proposed SPE/HPLC-MS/MS method is efficient and sensitive,and is suitable for the determination of various pesticides in actual water samples.
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