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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RSD<10%,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。
Due to the different structure and chemical nature of amino acids, GC-MS method has some difficulties in determination of amino acids with many different properties. In this paper, a GC-MS method for simultaneous determination of 20 amino acids was established by using ethyl chloroformate (ECF) as a derivatization reagent and adjusting p H to be 9 to 10 at the second derivatisation. The results showed that 20 kinds of amino acids were well separated, and the concentration was linear with the response value in the range of 2 ~ 20μg · m L -1 with the correlation coefficients r ~ 2 greater than 0.99. The experimental results of precision and system adaptability showed that the RSD was less than 10% and the average sample recovery was between 78.3% and 109.9%. The biological samples such as Astragalus membranaceus, urine samples of mice and blood samples were determined. The experimental results show that the method is simple and easy to operate. The derivatization method can be carried out in aqueous solution with stable product and wide linear range and can be used in many biological samples Determination.