尿中2-硫代噻唑烷-4-羧酸的高效液相色谱测定法  

Study on determination of 2-thioxothiazolidine-4-carboxylic Acid in urine by high performance liquid chromatography

作　　者：江金凤 宋为丽 刘亚攀 刘晙玭 王敏 Jiang Jinfeng;Song Weili;Liu Yapan;Liu Junpin;Wang Min(Department of Health Laboratory Technology,Wuhan Prevention and Treatment Center for Occupational Disease,Wuhan 430015,China)

机构地区：[1]武汉市职业病防治院卫生检验科,武汉430015

出　　处：《中华劳动卫生职业病杂志》2022年第5期370-373,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：武汉科技大学职业危害识别与控制湖北省重点实验室开放基金(OHIC2018G07)。

摘　　要：目的:建立尿中2-硫代噻唑烷-4-羧酸(TTCA)的高效液相色谱测定方法。方法:尿样以盐酸酸化,加过量氯化钠作盐析剂,用乙酸乙酯萃取尿中TTCA,经反相C18色谱柱梯度条件洗脱分离,二极管阵列检测器检测,外标法工作曲线定量。结果:尿中TTCA在0.03~10.00 mg/L的浓度范围内线性关系良好,相关系数r为0.9999,方法检出限为0.008 mg/L,最低定量下限为0.027 mg/L。尿中TTCA浓度为0.8、2.0和8.0 mg/L时,方法的批内精密度为0.9%~1.4%,批间精密度为1.3%~3.5%,加标回收率为85.0%~92.7%(n=6)。结论:该梯度洗脱高效液相色谱测定方法操作简单、灵敏度高,适用于二硫化碳接触人群尿中TTCA低浓度含量的测定。Objective To establish a high performance liquid chromatography method for the determination of 2-thioxothiazolidine-4-carboxylic acid(TTCA)in urine.Methods After acidification with hydrochloric acid,TTCA in urine was first extracted by ethyl acetate with excessive sodium chloride,then gradient separated by a symmetry C18 column and then detected by a diode array detector.The quantification was based on a working curve of external standard method.Results The linear relationship of TTCA in urine was good in the range of 0.03-10.00 mg/L,and the correlation coefficient was 0.9999.The detection limit and minimum quantitative concentration of TTCA in urine were 0.008 mg/L and 0.027 mg/L.The intra-assay precision of the method was 0.9%-1.4%,the inter-assay precision was 1.3%-3.5%,and the average recovery was 85.0%-92.7%while the concentrations of TTCA in urine was 0.8,2.0 and 8.0 mg/L,respectively(n=6).Conclusion The gradient elution high performance liquid chromatography method has simple operation and high sensitivity,and it is suitable for the determination of TTCA on a low level in urine for occupational workers exposure to carbon disulfide.

关 键 词：二硫化碳 2-硫代噻唑烷-4-羧酸 尿 色谱法 高效液相 

分 类 号：R446.12[医药卫生—诊断学]