Yang Min, Dong Zhonghua, Jiang Xiaoyan, Zhao Zhongxi, Zhang Jianqiang, Cao Xinke, Zhang Daizhou
School of Pharmaceutical Sciences, Shandong University, 44 West Wenhua Road, Jinan, Shandong 250012, P.R. China.
Shandong Engineering & Technology Research Center for Jujube Food and Drug, 44 West Wenhua Road, Jinan, Shandong 250012, P.R. China.
J Chromatogr Sci. 2018 May 1;56(5):396-402. doi: 10.1093/chromsci/bmy001.
In this work, a rapid, simple, sensitive and specific LC-MS/MS method was developed and validated for the quantification of S-Allylmercaptocysteine (SAMC) in plasma. After a simple sample procedure by one step protein precipitation with acetontrile, the samples were separated on Gemini-NX C18 column (2.1 mm i.d. 150 mm, 3 μm, Phenomenex). The mobile phase was composed of water-acetonitrile (20:80, v/v) at an isocratic flow rate of 0.3 mL/min. The developed method was validated based on the International Conference on Harmonization (ICH) guidelines. The results show that the method had satisfactory specificity, precision and accuracy in a linear range of 50-3,000 ng/mL for SAMC. The precision conformed to the acceptance criteria, and the lower limit of quantification was 50 ng/mL for the analyte. The plasma samples stored for 10 days or after two freeze-thaw cycles (-80°C) were stable. This method was successfully applied to a pharmacokinetics study of SAMC in rats. It was found that SAMC metabolized very quickly in rats and its plasma half-life was less than 5 min.
在本研究中，开发并验证了一种快速、简便、灵敏且特异的液相色谱-串联质谱（LC-MS/MS）方法，用于定量测定血浆中的S-烯丙基半胱氨酸（SAMC）。通过用乙腈一步沉淀蛋白进行简单的样品处理后，样品在Gemini-NX C18柱（内径2.1 mm，150 mm，3 μm，菲罗门公司）上进行分离。流动相由水-乙腈（20:80，v/v）组成，等度流速为0.3 mL/min。所开发的方法依据国际协调会议（ICH）指南进行验证。结果表明，该方法在50 - 3000 ng/mL的SAMC线性范围内具有令人满意的特异性、精密度和准确度。精密度符合验收标准，分析物的定量下限为50 ng/mL。储存10天或经过两次冻融循环（-80°C）的血浆样品是稳定的。该方法成功应用于SAMC在大鼠体内的药代动力学研究。结果发现，SAMC在大鼠体内代谢非常迅速，其血浆半衰期小于5分钟。
