HPLC-MS/MS快速测定远志中远志(口山)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

摘要:

目的: 建立一种远志中远志(口山)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, 3.5 μm),流动相乙腈-0.1%甲酸水 (28:72),流速0.3 mL·min^-1,进样量10 μL,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(口山)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(口山)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(口山)酮Ⅲ和3,6'-二芥子酰基蔗糖的定量分析.

Abstract:

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 C₁₈ column(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.