Determination of 1,1,2,2-tetrachloroethene in human urine by automated headspace-gas chromatography
Objective To establish an automated headspace-gas chromatography method for the determination of 1,1,2,2-tetrachloroethene in human urine.Methods 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.Results 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 2.5μg/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％.Conclusions 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.
NETL
NSTL
万方数据
