Citation: LIN Xingtao, WANG Xiaoyi, ZHAO Jingqiang. Determination of phthalate monoesters and diesters in urine by solid-phase extraction and gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(5): 528-532. doi: 10.3724/SP.J.1123.2016.01024 shu

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

1.
College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124, China

Corresponding author: WANG Xiaoyi,
Received Date: 18 January 2016

Fund Project: 国家自然科学基金项目(21177004). (21177004)

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.
- gas chromatography-mass spectrometry (GC-MS),
- solid-phase extraction (SPE),
- chemical derivatization,
- phthalate monoesters,
- phthalate diesters,
- urine
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沈阳化工大学材料科学与工程学院沈阳 110142