Jiang J F, Song W L, Liu Y P, Liu J P, Wang M
Department of Health Laboratory Technology, Wuhan Prevention and Treatment Center for Occupational Disease, Wuhan 430015, China.
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.
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.
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。