柱前衍生化法测定复方氨基酸注射液(18AA-Ⅱ)中氨基酸的含量
Determination of amino acids in compound amino acid injection(18AA-Ⅱ)by pre-column derivatization method
尧爱珉 1葛晓莹 1申兰慧1
作者信息
- 1. 无锡市药品安全检验检测中心,无锡 214028
- 折叠
摘要
目的 建立复方氨基酸注射液(18AA-Ⅱ)的柱前衍生化含量分析方法.方法 以邻苯二甲醛联合 9-芴甲基氯甲酸酯(OPA-FMOC)进行在线衍生,采用Zorbax Eclipse-AAA柱,以 40 mmol/L NaH2PO4 溶液(pH7.8)为流动相A,乙腈-甲醇-水(45:45:10)为流动相B,梯度洗脱,检测波长 338、262 nm,柱温 40℃.结果 各氨基酸之间分离度良好,线性相关系数均不小于 0.9994,平均回收率 99%～103%,重复性RSD均小于 2%.结论 该法稳定、准确、高效,可为复方氨基酸注射液的含量测定和质量评估提供参考,并首次报道了OPA-FMOC衍生分析法中赖氨酸峰面积重复性不佳的优化方法.
Abstract
Objective To develop an assay method of amino acids in compound amino acid injection(18AA-Ⅱ).Methods The online pre-column OPA-FMOC derivatization method was applied.A Zorbax Eclipse-AAA column was used in the gradient elution with 40 mmol/L NaH2PO4 solution(pH7.8)as mobile phase A and acetonitrile-methanol-water(45:45:10)as mobile phase B,the detection wavelength was 360 nm and 262 nm,and the column temperature was 40℃.Results The separation degree of amino acids was good.All the linear correlation coefficients were no less than 0.9994.The average recoveries were between 99%and 103%,the RSDs of repeatability were less than 2%.Conclusion This method could provide references for the quantitation and evaluation of amino acids in compound amino acid injection with good repeatability,accuracy and efficiency,and a solution to the weak repeatability of lysine peak area in OPA-FMOC derivatization method was reported for the first time.
关键词
氨基酸/含量测定/柱前衍生/邻苯二甲醛/9-芴甲基氯甲酸酯/复方氨基酸注射液(18AA-Ⅱ)Key words
amino acids/assay/pre-column derivatization/phthalendehyde/9-fluorenylmethylchloroformate/compound amino acid injection(18AA-Ⅱ)引用本文复制引用
基金项目
江苏省市场监督管理局科技计划项目(KJ2022029)
出版年
2024
NETL
NSTL
万方数据