UPLC-MS/MS法同时测定阿胶中18种核苷、游离氨基酸的含量  

Simultaneous content determination of eighteen nucleosides and free amino acids in Colla corii asini by UPLC⁃MS/MS

作　　者：杨帅 郑林[1] 迟明艳[1,2] 巩仔鹏 李月婷[1] 魏茂陈[3] 黄勇 YANG Shuai;ZHENG Lin;CHI Ming-yan;GONG Zi-peng;LI Yue-ting;WEI Mao-chen;HUANG Yong(Guizhou Provincial Key Laboratory for Pharmaceutics/State Key Laboratory for Functions and Applications of Medicinal Plants,Guizhou Medical University,Guiyang 550004,China;College of Pharmacy,Guizhou Medical University,Guiyang 550004,China;Guiyang Xintian Pharmaceutical Co.,Ltd.,Guiyang 550018,China)

机构地区：[1]贵州医科大学,贵州省药物制剂重点实验室/药用植物功效与利用国家重点实验室,贵州贵阳550004 [2]贵州医科大学药学院,贵州贵阳550004 [3]贵阳新天药业股份有限公司,贵州贵阳550018

出　　处：《中成药》2024年第7期2140-2146,共7页Chinese Traditional Patent Medicine

基　　金：贵州省科技计划项目(黔科合支撑[2021]419号,黔科合平台人才-GCC[2022]031-1号,黔科合平台人才-CXTD[2023]019号)。

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WatersBEHC18色谱柱(2.1mm×50mm,1.7μm);流动相乙腈(含0.1%甲酸)-水;体积流量0.35mL/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≥0.9990),平均加样回收率98.0%~104.9%,RSD1.6%~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。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 C18 column(2.1 mm×50 mm,1.7μm),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≥0.9990),whose average recoveries were 98.0%-104.9%with the RSDs of 1.6%-4.9%.Seventeenbatches 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.

关 键 词：阿胶 核苷 游离氨基酸 含量测定 UPLC-MS/MS 化学模式识别 

分 类 号：R284.1[医药卫生—中药学]