尿中氯乙烯代谢产物亚硫基二乙酸测定的固相萃取-离子色谱法  被引量:2

Determination of thiodiglycolic acid in urine by ion chromatography with solid-phase extraction

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作  者:刘晓东[1] 赵玮[1] 潘兴富[1] 闫慧芳[1] 

机构地区:[1]中国疾病预防控制中心职业卫生与中毒控制所,北京100050

出  处:《中华劳动卫生职业病杂志》2016年第4期297-299,共3页Chinese Journal of Industrial Hygiene and Occupational Diseases

基  金:科技部科技支撑计划项目(2014BAll2802);卫生部行业公益项目(201402021)

摘  要:目的 建立周相萃取-离子色谱法测定氯乙烯职业接触者尿液中氯乙烯代谢产物亚硫基二乙酸(TDGA).方法 取10 ml尿液样品以3 000 r/min离心10 min、C18固相萃取小柱净化后,AS19阴离子交换色谱柱分离,电导检测器检测,以保留时间定性,峰面积与外标法定量.结果 该方法的线性范围为0.05~50.00 μg/ml,r=0.999 9,方法检出限为0.1 μg/ml,方法定量下限为0.3 μg/ml,批内精密度为1.26%~5.03%,批间精密度为0.50%~8.78%,加标回收率为80.10%~ 104.20%;样品在-20 ℃条件下可放置14d;样品中共存和可能共存的氯乙酸、二氯乙酸、三氯乙酸及其他内源性离子化合物均不干扰TDGA的测定.结论 该方法前处理简单,灵敏度和特异性较高,适用于氯乙烯职业接触人群尿液中TDGA的定性定量分析.Objective To establish a SPE-IC method to determine the thiodiglycolic acid in the urine of workers who were exposed to vinyl chloride monomer.Methods The samples were prepared by the process of being centrifuged and purified by C18 SPE column before separated by AS19 anion exchange column and detected by conductivity detector.The thiodiglycolic acid were characterized by the retention time and quantified by peak area and external standard method.Results The range of linearity was 0.05~50.00 μg/ml,and the correlation coefficient was 0.999 9.The method detection limit was 0.1 μg/ml and the method quantitative limit was 0.3 μg/ ml.The within-run precision was 1.26%~5.03% and the between-run precision was 0.50%~8.78%.The spiked recoveries were 80.10%~104.20%.Samples could bestored at-20 ℃ for at least 2 weeks.The determination of thiodiglycolic acid could not be interfered by chloroacetic acid,dichloroacetic acid,trichloroacetic acid and other endogenous ionic compounds.Conclusion This method is feasible for determination of thiodiglycolic acid in the urine of workers who were exposed to vinyl chloride monomer.

关 键 词:亚硫基二乙酸 尿 同相萃取 色谱法 

分 类 号:R131[医药卫生—劳动卫生] R446.12[医药卫生—公共卫生与预防医学]

 

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