HPLC-MS/MS快速测定远志中远志■酮Ⅲ和3,6'-二芥子酰基蔗糖的含量  

Determination of Polygalaxanthone Ⅲ and 3,6'-Disinapoyl Sucrose in Polygala tenuifolia by HPLC-MS / MS

作　　者：杨改红[1] 程昊[2] 黄群[1] 严志宏[1] 杨武亮[1] 陈海芳[1] 袁金斌[1] 

机构地区：[1]江西中医药大学现代中药制剂教育部重点实验室，南昌 330004 [2]江西中医药大学基础医学院，南昌 330004

出　　处：《中国实验方剂学杂志》2014年第24期39-42,共4页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金项目(81260605)

摘　　要：目的：建立一种远志中远志酮Ⅲ和3,6＇-二芥子酰基蔗糖含量的HPLC-MS/MS分析方法。方法：采用ZORBAX Eclipse plus C18色谱柱,（4.6 mm×100 mm,3.5μm）,流动相乙腈-0.1%甲酸水（28∶72）,流速0.3 m L·min^-1,进样量10μL,柱温20℃。质谱条件：电喷雾负离子化模式,多反应监测模式（MRM）,检测离子对分别为m/z 567.2~345.1（远志酮Ⅲ）,m/z 753.3~205.1（3,6＇-二芥子酰基蔗糖）。结果：两种成分的线性关系良好,分析过程只需6 min。远志酮Ⅲ的日内精密度和日间精密度的RSD分别为2.2%,2.5%,回收率为96.1%~101.7%（RSD 2.4%）;3,6＇-二芥子酰基蔗糖的日内精密度和日间精密度的RSD分别为2.3%,2.4%,回收率为95.7%~101.4%（RSD 2.0%）。结论：该方法快速、灵敏、选择性好,适合远志中远志酮Ⅲ和3,6＇-二芥子酰基蔗糖的定量分析。Objective： The purpose of this study was to develop a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method for the determination of the contents of polygalaxanthone Ⅲ and 3, 6＇-disinapoyl sucrose. Method： Separation was performed on ZORBAX Eclipse plus C18column （4.6 mm × 100 mm, 3.5 μm） with the following settings： mobile phase cetonitrile-0. 1% formic acid （28：72）; flow rate 0.3 mL ·min^-1; the injection volume 10 μL; column temperature 20 ℃. MS condition, electrospray ionization （ESI） and multiple reaction monitoring （MRM） were adopted. The most abundant precursor/production pairs were m/z 567.2-345. 1 for polygalaxanthone Ⅲ , and m/z 753.3-205.1 for 3, 6＇- disinapoyl sucrose. Result： The two components showed good linearity and the analyzing process was just within 6 min. The intra-day precision and inter-day precision for polygalaxanthone Ⅲ were 2.2% and 2.5% respectively;the recoveries were between 96.1% and 101.7% with RSD 2.4% . While the intra-day precision and inter-day precision for 3, 6＇-disinapoyl sucrose were 2.3% and 2.4% ; the average recoveries were in the range of 95.7% - 101.4% with RSD 2.0%. Conclusion： The method is rapid, sensitive, selective and suitable for the quantitative analysis of polygalaxanthone Ⅲ and 3, 6＇-disinapoyl sucrose in polygala tenuifolia.

关 键 词：远志■酮Ⅲ 3 6'-二芥子酰基蔗糖 远志 高效液相色谱-质谱联用 

分 类 号：R284.1[医药卫生—中药学]