气相色谱法测定人血白蛋白辛酸钠含量的方法优化

Optimization of Gas Chromatography for Determination of Sodium Caprylate in Human Albumin

目的:优化气相色谱法测定人血白蛋白辛酸钠含量的方法。方法:在《中华人民共和国药典》2020年版通则“3111辛酸钠含量测定方法”的基础上,删除“将三氯甲烷挥发至干,另加三氯甲烷100μL溶解残渣”,对优化前、后气相色谱法测定人血白蛋白辛酸钠含量的方法效果进行对比研究。结果:优化后的方法实验时间由2 d缩短为1 d;方法优化前、后系统适用性试验辛酸对照品溶液连续进样5针所得辛酸峰与庚酸峰面积之比的RSD值分别为0.1%、3.0%,均符合《中华人民共和国药典》规定(≤5%);测定同一批人血白蛋白质控品辛酸钠含量6次,优化前、后方法重复性RSD值分别为4%、2%,优化前、后方法重复性无显著性差异;测定高、中、低3个浓度回收率溶液各3次,优化前、后方法RSD值为1.70%、1.55%,回收率平均值分别为97.7%、99.7%,优化后方法准确度优于优化前方法。结论:优化后的方法适用于人血白蛋白辛酸钠含量测定。

Objective:The determination method of sodium caprylate in human albumin by gas chromatography is optimized.Methods:On the basis of general rule“3111 the determination of sodium octanoate content”of the Pharmacopoeia of the People’s Republic of China,2020 edition,delete“volatilize chloroform to dry,and add chloroform 100μL dissolved residue”,a comparative study is carried out on the determination of sodium octanoate in human albumin by gas chromatography before and after optimization.Results:The experimental time of the optimized method is shortened from 2 days to 1 day.Methods before and after optimization,the RSD values of the ratio of octanoic acid peak to heptanic acid peak area obtained from continuous injection of octanoic acid reference solution for 5 times are 0.1%and 3.0%respectively,which are in line with the provisions of the Pharmacopoeia of the people’s Republic of China(≤5%).The content of sodium octanoate in the same batch of human albumin quality control is determined for 6 times.The RSD values of the method repeatability before and after optimization are 4%and 2%respectively.There is no significant difference in the repeatability of the method before and after optimization.Determine the high,medium and low concentration recovery solutions for three times respectively.The RSD values of the pre optimization and post optimization methods are 1.70%、1.55%,and the average recoveries are 97.7%and 99.7%respectively.The accuracy of the optimized method is better than that of the pre optimization method.Conclusion:The optimization method is suitable for the determination of sodium caprylate in human albumin.