Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (5): 528-532.DOI: 10.3724/SP.J.1123.2016.01024

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Determination of phthalate monoesters and diesters in urine by solid-phase extraction and gas chromatography-mass spectrometry

LIN Xingtao, WANG Xiaoyi, ZHAO Jingqiang   

  1. College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124, China
  • Received:2016-01-18 Online:2016-05-08 Published:2012-12-18
  • Supported by:

    National Natural Science Foundation of China (No. 21177004).

Abstract:

A method for the determination of phthalate monoesters and diesters in urine by solid-phase extraction and gas chromatography-mass spectrometry (SPE-GC-MS) was developed. After urine enzymatic hydrolysis by β-glucuronidase, the sample was pretreated by SPE. Phthalate monoesters and diesters were eluted by acetonitrile, ethyl acetate and ethyl ester-n-hexane (1: 19, v/v), separately. The mixture of the elution was dried by N2 and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide before GC-MS analysis. Good linear relationships were obtained in the range of 5-1000 μ g/L. The limits of detection were between 0.3 and 1.1 μ g/L. The recoveries of phthalate monoesters and diesters were in the range of 77.9%-97.7% and the relative standard deviations (RSDs) were 3.7%-10.9%. The method was applied to analyze 50 urine samples. Seven compounds, such as di-2-ethylhexyl phthalate (DEHP), were detected. The mean concentrations were between 6.0 and 142.7 μ g/L. The method is highly accurate, reliable and sensitive for monitoring phthalate monoesters and diesters in urine.

Key words: chemical derivatization, gas chromatography-mass spectrometry (GC-MS), phthalate diesters, phthalate monoesters, solid-phase extraction (SPE), urine

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