Citation: ZHAN Xue-Wang, LI Peng-Hui, XU Lin. Determination of 8 Kinds of Benzenes and 17 Kinds of Volatile Halogenated Hydrocarbons in Urine by Headspace-Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2023, 51(6): 1033-1041. doi: 10.19756/j.issn.0253-3820.221372 shu

Determination of 8 Kinds of Benzenes and 17 Kinds of Volatile Halogenated Hydrocarbons in Urine by Headspace-Solid Phase Microextraction/Gas Chromatography-Mass Spectrometry

ZHAN Xue-Wang ^1,2 ,
LI Peng-Hui ^1,, ,
XU Lin ^2,,

1.
School of Environmental Science and Safety Engineering, Tianjin University of Technology, Tianjin 300382, China;
2.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China

Corresponding author: LI Peng-Hui, XU Lin,
Received Date: 24 July 2022
Revised Date: 7 February 2023

Fund Project: Supported by the National Natural Science Foundation of China (Nos. 22036007, 21876189) and the Youth Innovation Promotion Association, CAS (No. 2018059).

A headspace solid-phase microextraction coupled with gas chromatography-mass spectrometric (GCMS) method was developed for analysis of 8 kinds of benzenes (BTEX) and 17 kinds of volatile halogenated hydrocarbons (VHC) in urine samples. The effects of extraction fiber, extraction temperature, extraction time, urine pH, stirring speed and salt effect on the experimental results were investigated by single-factor experiments, followed by the interaction analysis between factors based on the Box-Behnken experimental design principle with the total peak areas of the chromatograms of 25 kinds of target compounds as the response values. The optimized conditions were as follows: 2 mL of urine sample adjusted to pH=4, 40 μL of internal standard (fluorobenzene and chlorobenzene-d5, 500 μg/L) and 0.55 g NaCl were added to a 40-mL headspace vial; 75 μm Carboxen/ polydimethylsiloxane (Carboxen/PDMS) fiber was selected for headspace extraction at 51℃ with stirring speed of 400 r/min for 35 min. The calibration curves showed good linearity (R² > 0.990) in the range of 0.05-50 μg/L for the 25 kinds of targets, with the detection limits of 0.008-5.780 ng/L and the lower limits of quantification of 0.027-19.268 ng/L. The recoveries of the 25 kinds of stargets ranged from 78.9% to 115.2% and the relative standard deviations were 0.7%-16.2%. The method was applied to determination of urine samples from the healthy population in Lai Yang, Shandong Province. The results showed that 20 kinds of target compounds were detected in 15 human urine samples, with total concentrations ranging from 3.13 to 43.17 μg/L and a median content of 5.78 μg/L. 1,2,4-Trimethylbenzene (1,2,4-TMB) was the compound with the highest median content of BTEX and 1,3-dichlorobenzene (1,3-DCB) was the compound with the highest median content of VHC. The method was sensitive and reproducible for simultaneous determination of BTEX and VHC in urine samples and might provide an important methodological basis for human exposure studies of these two compounds.
- Headspace solid-phase microextraction,
- Gas chromatography-mass spectrometry,
- Urine,
- Benzene,
- Volatile halogenated hydrocarbons
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