分析化学2017，Vol.45Issue(11)：1648-1654,7.DOI:10.11895/j.issn.0253-3820.171027
液相色谱-串联质谱法测定尿液中7种有机磷酸酯代谢物
Determination of Seven Urinary Metabolites of Organophosphate Esters Using Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A simple method was developed for simultaneous determination of seven urinary metabolites of organophosphate esters by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Based on different physical and chemical properties of these OPs metabolites, the solid phase extraction cartridges and the washing and eluting solvents were optimized in details. Furthermore, the mobile phase and mass spectrometric parameters were also investigated. The results showed that Oasis WAX cartridge was the best SPE column in this study, and 2 mL of NH3 ·H2 O (5% ) in methanol and 2 mL of methanol were chosen as the eluting solvents. The recoveries of six analytes were ranged from 60. 5% to 104. 0% , whereas DEP ranged from 17. 8% to 36. 2% . Seven analytes could be baseline separated from each other under the optimized chromatographic conditions. The limits of detection and quantification of seven analytes ranged from 0. 005 to 0. 2 μg / L and 0. 02 to 0. 5 μg / L, respectively. The standard deviations of response repeatability for intra-day and inter-day period were lower than 15. 4% . This method was finally applied to determination of metabolites of OPs from 10 urines from general population in Guangzhou city. The concentrations of total OPs metabolites in urine samples ranged from 0. 5 to 6. 7 μg / L.关键词
液相色谱-串联质谱/有机磷酸酯/尿液/代谢产物Key words
Liquid chromatography-tandem mass spectrometry/Organophosphate esters/Urine/Metabolites引用本文复制引用
李佩,曾祥英,崔君涛,赵灵娟,于志强..液相色谱-串联质谱法测定尿液中7种有机磷酸酯代谢物[J].分析化学,2017,45(11):1648-1654,7.基金项目
本文系国家杰出青年科学基金(No. 41225013)和中国科学院战略性先导科技专项(B 类) (No. XDB14010202)资助 This work was supported by the National Natural Science Foundation of China (No. 41225013). （No. 41225013）
