色谱Issue(6)：622-627,6.DOI:10.3724/SP.J.1123.2015.01037
高效液相色谱-串联质谱法同时测定人尿液中7种邻苯二甲酸酯代谢物
Determination of seven phthalate metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method has been developed for the analysis of seven metabolites of phthalates in human urine by high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). The urine samples were hydrolyzed with glucuronidase followed by purification with solid-phase extraction( SPE)cartridges. Both 0. 1% formic acid in water( v/v)and 0. 1% for-mic acid in acetonitrile were used as the mobile phases in a gradient mode. The chromatograph-ic separation was achieved on a phenyl column. Mass detection was then conducted by electros-pray ionization in negative ion mode and multiple reaction monitoring mode. The components were quantified by stable isotope-labelled( 13 C-)phthalate monoester internal standards. The calibration curves of the seven phthalates metabolites showed good linear relationships in the range of 0. 2-200. 0 μg/L( r﹥0. 999 76 ). The recoveries at three levels were from 88. 8% to 108. 9% with relative standard deviations no more than 17. 05%. The limits of detection of the method were 13. 43-80. 2 ng/L. The limits of quantification were 44. 77-267. 37 ng/L. This method was successfully applied to the determination of metabolism of phthalates in human urine with efficiency,increased accuracy and high sensitivity.关键词
固相萃取/同位素内标法/高效液相色谱-串联质谱/邻苯二甲酸酯代谢物/尿Key words
solid-phase extraction(SPE)/isotope internal standard method/high perform-ance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/phthalate metabo-lites/urine分类
化学化工引用本文复制引用
高慧,许媛媛,孙丽,金忠秀,胡海婷,盛杰,任玲玲,陶芳标..高效液相色谱-串联质谱法同时测定人尿液中7种邻苯二甲酸酯代谢物[J].色谱,2015,(6):622-627,6.基金项目
国家自然科学基金重点项目（81330068）；国家自然科学基金青年基金项目（81302449）． （）
