溶剂萃取/HPLC-MS/MS法快速测定1,1,2,2-四氯乙烷职业接触人群尿中二氯乙酸与三氯乙酸OA

A rapid detection method using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established for determining dichloroacetic acid(DCA)and trichlo-roacetic acid(TCA)in urine of occupationally exposed individuals to 1,1,2,2-tetrachloroethane.The urine samples were acidified by adding hydrochloric acid solution,followed with sodium chloride being added and shaking.Subsequently DCA and TCA were extracted with ethyl acetate.The upper extract was concentrated to near dryness using nitrogen blowing,and then redissolved with 15%ace-tonitrile solution.After being filtered through a microporous membrane,they were injected into the instrument.Chromatographic separation was achieved using a Waters HSS T3(2.1 mm×100 mm,1.8 µm)column,with acetonitrile-0.1%acetic acid aqueous solution as the mobile phase for gradi-ent elution.Electrospray ionization(ESI)source and multiple reaction monitoring(MRM)mode were employed.Quantification was performed using the matrix-matched curve external standard method.Both DCA and TCA exhibited linear relationships within the mass concentration range of 2.0-100 µg/L,with linear correlation coefficients(r)higher than 0.999.The limits of detection(LODs)and the limits of quantitation(LOQs)were calculated to be 0.2 µg/L and 1.0 µg/L,respectively.The re-coveries at low,medium and high spiked concentration levels ranged from 75.3%to 104%.The aver-age recoveries of DCA and TCA were 91.1%and 86.1%,respectively,with relative standard devia-tions(RSDs)ranging from 2.1%to 9.5%.The established analytical procedure was employed for urine DCA and TCA level investigating of the general population,routine occupational population,and occupational poisoning patients.The method is simple,rapid and highly sensitive,providing a technical reference for biological monitoring and clinical testing of occupational poisoning in occupa-tionally exposed individuals to 1,1,2,2-tetrachloroethane.