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高效液相色谱法测定尿液中2-硫代噻唑烷-4-羧酸的研究

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

作者信息

Jiang J F, Song W L, Liu Y P, Liu J P, Wang M

机构信息

Department of Health Laboratory Technology, Wuhan Prevention and Treatment Center for Occupational Disease, Wuhan 430015, China.

出版信息

Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2022 May 20;40(5):370-373. doi: 10.3760/cma.j.cn121094-20210129-00061.

Abstract

To establish a high performance liquid chromatography method for the determination of 2-thioxothiazolidine-4-carboxylic acid (TTCA) in urine. 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. 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 (=6) . 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.

摘要

建立高效液相色谱法测定尿中2-硫代噻唑烷-4-羧酸(TTCA)的含量。尿样经盐酸酸化后,首先用过量氯化钠的乙酸乙酯萃取尿中的TTCA,然后用Symmetry C18柱进行梯度分离,再用二极管阵列检测器检测。定量采用外标法工作曲线。尿中TTCA在0.03~10.00 mg/L范围内线性关系良好,相关系数为0.9999。尿中TTCA的检测限和最低定量浓度分别为0.008 mg/L和0.027 mg/L。当尿中TTCA浓度分别为0.8、2.0和8.0 mg/L时(n = 6),该方法的批内精密度为0.9%~1.4%,批间精密度为1.3%~3.5%,平均回收率为85.0%~92.7%。梯度洗脱高效液相色谱法操作简便、灵敏度高,适用于职业接触二硫化碳工人尿中低水平TTCA的测定。

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