[关键词]
[摘要]
目的:建立超高效液相色谱-质谱/质谱联用法(UPLC-MS/MS)测定泰山白首乌药材中γ-氨基丁酸(GABA)的含量。方法:泰山白首乌药材粉末分别用20 倍量和15 倍的水超声提取2 次,每次20 min,定容,备用。以GABA 为标准品,采用ACQUITY UPLCTM BEH C18 柱(100 mm×2.1 mm, 1.7 μm)分离,流动相为乙腈∶0.1%甲酸水溶液(v/v)=20∶80,流速为0.20 mL/min,通过电喷雾离子化,采用多反应监测(MRM)方式进行正离子检测。结果:线性范围为11.5~2300.0 ng/mL,平均回收率为94.0%,相对标准偏差RSD 不高于5%。泰山白首乌药材中γ-氨基丁酸含量为0.202%。结论:该方法灵敏度高,分析速度快,操作简便,适用于含GABA 成分的药物和功能食品的含量测定分析。
[Key word]
[Abstract]
A quantitative method to determine the content of γ-GABA in roots of Cynanchum Bungei Decne was established using Ultra-performance Liquid Chromatography-tandem Mass Spectrometry (UPLC-MS-MS). Powder of roots of Cynanchum Bungei Decne was extracted with 15 times and 20 times water, each 20 min respectively. Set volume to the mark, and the solution was ready for determination. The γ-GABA was measured with GABA as standard, and separated through column of ACQUITY UPLCTM BEH C18 (100 mm×2.1 mm, 1.7 μm), mobile phase of 20% acetonitrile-80% water (containing 0.1% formic acid). The flow rate was at 0.2 mL/min. ESI source and MRM mode were applied. Linear calibration curve range was 11.5~2300.0 ng/mL. The mean extraction recovery of γ-GABA was 94.0%. And the RSD was less than 5%. The results showed that the content of γ-GABA in roots of Cynanchum Bungei Decne was 0.202%. It was concluded that this is a rapid and sensitive method, which is suitable for the analysis of drug and functional food containing γ-GABA.
[中图分类号]
[基金项目]
山东省教育厅项目(J08LHIO):山东著名中药泰山白首乌抗衰老有效部位谱效关系及作用机制研究,负责人:徐凌川。