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| Determination of Five Organophosphate Ester Metabolites in Surface Water Samples by LC-MS/MS |
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| DOI： |
| KeyWord:organophosphate ester metabolites liquid chromatography-tandem mass spectrometry（LC-MS/MS） river water solid phase extraction |
| Author | Institution |
| LI Chuang-xiu,ZHAO Xiao-li,GAO Li-hong,SHI Ya-li,TAN Wei-qiang*,CAI Ya-qi* |
1.青岛理工大学环境与市政工程学院;2.中国环境科学研究院环境基准与风险评估国家重点实验室;3.中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室 |
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| Abstract: |
| A liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the determination of five organophosphate ester metabolites in river water samples.The filtered water samples were enriched and purified by solid phase extraction（SPE） using a HLB cartridges,and then eluted with 6 mL methanol.The eluent was concentrated to a volume of 0.5mL under gentle nitrogen stream and then diluted to 1mL by initial mobile phase（50% methanol）.Instrumental analysis was accomplished by HPLC-MS/MS under negative electrospray ion and multiple reaction monitoring（MRM） mode.Separation of the analytes was performed on a Luna Phenyl-Hexyl column,and a mixture of methanol and 50mmol?L-1 ammonium acetate solution was selected as mobile phase for gradient elution.The recoveries of five organophosphate ester metabolites in river samples were in the range of 57.8%-102% at a spiked concentration of 50ng?L-1 with relative standard deviations（RSD） of 2.8%-15.7%.At a spiked concentration of 10ng?L-1,the recoveries were in the range of 54.1%-83.6% with RSDs of 5.3%-19.5%.The instrumental detection limits（IDL） ranged from 0.002μg?L-1 to 1.15μg?L-1 and the method detection limits（MDL） ranged from 0.15ng?L-1 to 4.48ng?L-1.The matrix effect of river samples was also investigated in this study.The proposed method was successfully applied in the determination of organophosphate ester metabolites in lake water samples collected from Wuhan,Hubei.Except for DEHP,the other four OPEs metabolites were all detectable in lake water.The method showed good precision and accuracy,and was suitable for the analysis of five organophosphate ester metabolites in surface water samples. |
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