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| Determination of dichloroacetic acid and trichloroacetic acid in urine using headspace gas chromatography |
| YANG Qinghua1, SHI Yilan1, GU Jun1, CHEN Feng1, WEI Jiamei2
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1. Department of Physics and Chemistry, Nantong Center for Disease Prevention and Control, Nantong, Jiangsu 226002, China;
2. Pukou Center for Disease Prevention and Control, Nanjing, Jiangsu 210000, China |
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Abstract Objective To develop a headspace gas chromatography ( HS-GC ) assay for simultaneous determination of dichloroacetic acid ( DCA ) and trichloroacetic acid ( TCA ) in urine. Methods Urine samples (5 mL) were transferred to a 22 mL headspace bottle, added with 0.5 mL 10% sodium acetate solution , immediately sealed, and shaken evenly. The bottle was placed in the HS-GC system, and equilibrated at 90 ℃ for 60 minutes. The mixture was separated with the HP-INNOWAX chromatographic column, and the DCA and TCA concentrations were detected with the hydrogen flame detector. Results Under the optimal experimental conditions, the correlation coefficient of DCA and TAC was both > 0.999 0 within the range of 10-500.0 μg/L, and the lowest detection limits of DCA and TAC were 2.0 and 3.5 μg/L, with the spike recovery rate of 87.40% to 101.44%, and relative standard deviations of 1.89% to 3.25%. Of the 35 urine samples sampled from occupational populations, DCA and TCA were not detected. Conclusions The establishment of the HS-GAS assay through addition of sodium acetate and optimization of the headspace conditions, has high recovery and precision, which is effective to meet the requirements for daily determination of DCA and TCA in urine samples.
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Received: 09 August 2021
Revised: 28 October 2021
Published: 14 February 2022
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