Citation: GAO Hui, XU Yuanyuan, SUN Li, JIN Zhongxiu, HU Haiting, SHENG Jie, REN Lingling, TAO Fangbiao. Determination of seven phthalate metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(6): 622-627. doi: 10.3724/SP.J.1123.2015.01037 shu

Determination of seven phthalate metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry

GAO Hui ¹ ,
XU Yuanyuan ^1,2 ,
SUN Li ¹ ,
JIN Zhongxiu ² ,
HU Haiting ¹ ,
SHENG Jie ² ,
REN Lingling ² ,
TAO Fangbiao ^1,2,,

1.
1. Department of Maternal, Child and Adolescent Health, School of Public Health, Anhui Medical University, Hefei 230032, China;

Corresponding author: TAO Fangbiao,
Received Date: 27 January 2015

Fund Project: 国家自然科学基金重点项目(81330068) (81330068)国家自然科学基金青年基金项目(81302449). (81302449)

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% formic acid in acetonitrile were used as the mobile phases in a gradient mode. The chromatographic separation was achieved on a phenyl column. Mass detection was then conducted by electrospray ionization in negative ion mode and multiple reaction monitoring mode. The components were quantified by stable isotope-labelled (¹³C-) 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>0.99976). 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.
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