摘要
目的 建立UPLC-MS/MS法同时测定阿胶中Asp、Guad、Adeno、Arg、Ade、Cyti、Phe、Leu、Ile、Glu、Ser、Gln、Gly、Ala、Hyp、Thr、Pro、Lys的含量.方法 分析采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7 μm);流动相乙腈(含 0.1%甲酸)-水;体积流量 0.35 mL/min;柱温 45℃;电喷雾离子源;正离子扫描;多反应监测模式.再采用层次聚类分析、主成分分析和正交偏最小二乘判别分析进行化学模式识别.结果 18 种核苷、游离氨基酸在各自范围内线性关系良好(r≥0.999 0),平均加样回收率 98.0%～104.9%,RSD 1.6%～4.9%.17 批样品聚为 2 类,2 种主成分累积方差贡献率为 60.75%,Leu、Phe、Ade和Guad是潜在指标成分.结论 该方法稳定可靠,可用于阿胶的质量控制.
Abstract
AIM To establish a UPLC-MS/MS method for the simultaneous content determination of Asp,Guad,Adeno,Arg,Ade,Cyti,Phe,Leu,Ile,Glu,Ser,Gln,Gly,Ala,Hyp,Thr,Pro and Lys in Asini Corii Colla.METHODS The analysis was performed on a 45℃ thermostatic Waters BEH C18column(2.1 mm×50 mm,1.7 μm),with the mobile phase comprising of acetonitrile(containing 0.1% formic acid)-water flowing at 0.35 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive ion scanning with multiple reaction monitoring mode.Subsequently,chemical pattern recognition was performed by hierarchical clustering analysis,principal component analysis and orthogonal partial least squares-discriminant analysis.RESULTS Eighteen nucleosides and free amino acids showed good linear relationships within their own ranges(r≥0.999 0),whose average recoveries were 98.0%-104.9% with the RSDs of 1.6%-4.9% .Seventeen batches of samples were clustered into two categories,two principal components demonstrated the accumulative variance contribution rate of 60.75%,Leu,Phe,Ade and Guad were potential index constituents.CONCLUSION This stable and reliable method can be used for the quality control of Asini Corii Colla.
基金项目
贵州省科技计划项目(黔科合支撑[2021]419号)
贵州省科技计划项目(黔科合平台人才-GCC[2022]031-1号)
贵州省科技计划项目(黔科合平台人才-CXTD[2023]019号)
国家科技期刊平台
NSTL
万方数据