基于氯甲酸乙酯二次衍生化的GC-MS法同时测定生物样本中20种氨基酸

发布时间：2018-06-18 06:50

本文选题：氯甲酸乙酯衍生化 + 氨基酸　；参考：《药学学报》2017年04期

【摘要】：由于氨基酸结构和化学性质不同,GC-MS方法测定多种不同属性的氨基酸存在一定的困难。本文通过以氯甲酸乙酯(ECF)作为衍生化试剂,并在第2次衍生化时调节p H为9~10,建立了同时测定20种氨基酸的GC-MS分析方法。结果表明,20种氨基酸得到较好分离,且在2~20μg·m L~(-1)内其浓度与响应值具有良好的线性关系,相关系数r~2均大于0.99。精密度和系统适应性实验结果表明RSD10%,样品平均加样回收率在78.3%~109.9%之间。通过对黄芪花、小鼠尿样、血样等生物样本进行测定,实验结果表明该方法简便易操作,而且该衍生化方法可在水溶液中进行且产物稳定、线性范围宽,可用于多种生物样本测定。
[Abstract]:It is difficult to determine amino acids with different properties by GC-MS because of the different structure and chemical properties of amino acids. A GC-MS method for simultaneous determination of 20 amino acids was established by using ethyl chloroformate (ECF) as derivatization reagent and adjusting pH to 9 ~ 10 during the second derivatization. The results showed that 20 kinds of amino acids were well separated, and their concentration had a good linear relationship with the response value in the range of 20 渭 g / L ~ (-1), and the correlation coefficient (r ~ (2) was all greater than 0.99m 路L ~ (-1). The experimental results of precision and system adaptability showed that the average recovery of samples was between 78.3% and 109.9%. Through the determination of Astragalus membranaceus, mouse urine and blood samples, the experimental results show that the method is simple and easy to operate, and the derivative method can be used in aqueous solution with stable product and wide linear range. It can be used for a variety of biological samples.
【作者单位】：山西大学中医药现代研究中心;山西大学化学化工学院;山西大学化学生物学与分子工程教育部重点实验室;中国医学科学院北京协和医学院药物研究所;美国路易斯维尔大学;
【基金】：国家自然科学基金资助项目(31300278) 教育部博士点新教师类基金项目(20131401120006) 山西省科技攻关项目(20150313004-5) 山西省优秀人才项目(201605D211030) 山西省中药产业重点科技攻关项目(201603D311101) 国家中药标准化项目(ZYBZH-Y-JIN-34) 山西省药材行业标准-恒山黄芪药材与精品饮片商品等级标准研究(2014ZD0401)
【分类号】：R917

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