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r2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 difference in structure and chemical properties of amino acids, it is difficult to determine amino acids with different properties by GC-MS. A method was established for the simultaneous determination of 20 amino acids by using ethyl chloroformate (ECF) as the derivatization reagent and adjusting pH 9-10 in the second derivatization in this study. The results showed that 20 amino acids were well separated and the compounds in the 2-20 μg·mL-1 concentrations were detected with a good linear response correlation coefficient r2 greater than 0.99. The results of precision and system adaptability show that RSD 〈 10%, the average recovery of samples in the 78.3%-109.9%. The results showed that the method was simple and easy to use, and the derivatization method could be.carried out in aqueous solution. The derivatization product was stable with wide linear range, thus this method could be used for the determination of a variety of biological samples such as Astragalus mongolicus, mouse urine sample and mouse serum sample.