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| Citation: |
LI Siyan, ZHONG Yuanqin, CAI Xiaoxuan, ZHOU Changxia, ZHUANG Xiaozhou, MA Zheng, YE Lihe, YANG Peishan, XIONG Jinguang, CHEN Manlian. Determination of 1, 1, 2, 2-tetrachloroethene in human urine by automated headspace-gas chromatography[J]. Occupational Health and Emergency Rescue, 2024, 42(4): 528-532. DOI: 10.16369/j.oher.issn.1007-1326.2024.04.027
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To establish an automated headspace-gas chromatography method for the determination of 1, 1, 2, 2-tetrachloroethene in human urine.
A urine sample of 5.00 mL was placed in a 20 mL headspace vial, and 2.0 g of anhydrous sodium sulfite was added before sealing the vial. The vial was placed in an automated headspace sampler and heated at 80 ℃ for 50.00 min to equilibrate. Under these heating conditions, 1, 1, 2, 2-tetrachloroethene in human urine was completely reacted with anhydrous sodium sulfite to form trichloroethylene. The trichloroethylene vapor above the headspace vial was separated by a DB-624 capillary column and detected with a flame ionization detector. Quantification was achieved by plotting a standard curve with the peak area of trichloroethylene and the mass concentration of 1, 1, 2, 2-tetrachloroethane.
The results showed good linear ranges of 1, 1, 2, 2-tetrachloroethene in urine between 0.008 3 and 32.000 mg/L, and the correlation coefficient was higher than 0.999 4. For this method, the limit of detection was 2.5 μg/L, and the lower limit of quantification was 8.3 μg/L; the intra-batch precision was 4.79% to 5.28%, and the inter-batch precision was 4.61% to 6.44%; the average recovery rate was 87.53% to 101.17%.
The automated headspace gas chromatography method for determining 1, 1, 2, 2-tetrachloroethene in human urine was characterized by high sensitivity, good linearity, minimal interference, high precision, and simple sample preparation. It is suitable for measuring the concentration of 1, 1, 2, 2-tetrachloroethene in human urine.
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