The advent of the triple quadrupole technology to the inductively coupled plasma mass spectrometry (ICPMS) technique has allowed a strong improvement in the accuracy and detection limits of ICPMS for non-metal elements such as sulfur by removing major polyatomic interferences. Up to now, there has been no report utilizing this development for sulfur speciation in complex human biological matrices. In the present report, we show the success of HPLC-ICPQQQMS for the simultaneous determination of two major sulfur metabolites, taurine and sulfate, in human urine and serum, by direct injection without the need for sample clean-up. The optimized chromatographic method was validated, tested for robustness, and applied for investigating the intra-individual variability in taurine urinary excretion in eight healthy volunteers over a period of 8 weeks. The limit of detection and limit of quantification for taurine determination was found to be 0.2 and 0.7 pmol, respectively. The concentrations found in the analyzed group of urine samples (n = 64) had a range, mean, and SD of 0.6–99, 20.4, and 23.2 μg mL⁻¹ for taurine, and 115–1373, 616, and 259 μg mL⁻¹ for sulfate. Taurine was found to exhibit a much higher intra-individual variability than sulfate. The developed method can be applied in large-scale epidemiological studies and clinical studies in order to establish the potential cardioprotective effects of taurine.

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电感耦合等离子体质谱 (ICPMS) 技术中三重四极杆技术的出现，消除了主要的多原子干扰，大大提高了 ICPMS 对硫等非金属元素的准确度和检测限。到目前为止，还没有报道利用这一进展来研究复杂的人类生物基质中的硫形态。在本报告中，我们展示了 HPLC-ICPMS/MS 成功地通过直接进样同时测定人尿液和血清中的两种主要硫代谢物（牛磺酸和硫酸盐），无需样品净化。优化的色谱方法经过验证、稳健性测试，并用于研究 8 名健康志愿者在 8 周内牛磺酸尿排泄的个体差异。牛磺酸测定的检测限和定量限分别为 0.2 和 0.7 pmol。分析组尿液样本 ( n  = 64) 中牛磺酸的浓度范围、平均值和 SD 分别为 0.6–99、20.4 和 23.2 μg mL ^-1，以及 115–1373、616 和 259 μg mL -1 ^-1为硫酸盐。研究发现牛磺酸表现出比硫酸盐更高的个体内变异性。所开发的方法可应用于大规模流行病学研究和临床研究，以确定牛磺酸的潜在心脏保护作用。

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