Chwatko Grazyna, Bald Edward
Department of Environmental Chemistry University of Lodz, 163 Pomorska Street, 90-236 Lodz, Poland.
Talanta. 2009 Jul 15;79(2):229-34. doi: 10.1016/j.talanta.2009.03.040. Epub 2009 Mar 27.
Thiosulfate is a sulfate analogue with a thiosulfur substituent and is found in human samples. Its concentration in urine is increased in some diseases and after exposure to hydrogen sulfide gas. We have developed a sensitive, simple and cheap method for thiosulfate determination in urine. The method is based on precolumn derivatization with 2-chloro-1-methylquinolinium tetrafluoroborate followed by reversed-phase liquid chromatography separation and ultraviolet detection of 1-methyl-2-thioquinolone at 375 nm. The calibration curve for thiosulfate was linear in the tested range 0.5-50 micromol L(-1) with correlation coefficient better than 0.999. The analytical recovery and relative standard deviation values for precision within the calibration range were from 90.1% to 104.2% and from 2.39% to 5.59%, respectively. The lower limit of detection and quantitation were 0.3 and 0.5 micromol L(-1), respectively. The mean (range) concentration of thiosulfate normalized against creatinine for apparently healthy seven women and six men was 2.21 (1.45-2.77) and 2.51 (1.36-4.89)mmol mol(-1) creatinine, respectively. We monitored thiosulfate in urine samples from one volunteer for 24 h. The urinary excretion of thiosulfate was 21.4 micromol per 24 h. This method can be used for routine clinical monitoring thiosulfate in urine. Cysteine and cysteinylglycine can be measured concurrently, if needed.
硫代硫酸盐是一种带有硫代硫取代基的硫酸盐类似物,存在于人体样本中。在某些疾病以及接触硫化氢气体后,其尿液中的浓度会升高。我们开发了一种灵敏、简便且廉价的尿液中硫代硫酸盐测定方法。该方法基于用四氟硼酸2-氯-1-甲基喹啉鎓进行柱前衍生化,随后进行反相液相色谱分离,并在375nm处对1-甲基-2-硫代喹诺酮进行紫外检测。硫代硫酸盐的校准曲线在0.5 - 50 μmol L⁻¹的测试范围内呈线性,相关系数优于0.999。在校准范围内,分析回收率和精密度的相对标准偏差值分别为90.1%至104.2%和2.39%至5.59%。检测下限和定量下限分别为0.3和0.5 μmol L⁻¹。七名明显健康的女性和六名男性尿液中经肌酐标准化后的硫代硫酸盐平均(范围)浓度分别为2.21(1.45 - 2.77)和2.51(1.36 - 4.89)mmol mol⁻¹肌酐。我们对一名志愿者的尿液样本进行了24小时硫代硫酸盐监测。硫代硫酸盐的尿排泄量为每24小时21.4 μmol。该方法可用于尿液中硫代硫酸盐的常规临床监测。如有需要,可同时测定半胱氨酸和半胱氨酰甘氨酸。