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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: To establish a HPLC-MS / MS method for the determination of the contents of sevoflurane III and 3,6’-alanyl sucrose in COSCO Polygala. METHODS: The mobile phase consisted of acetonitrile-0.1% formic acid water (28:72), flow rate 0.3 mL · min-1 and injection volume 10 μL on a ZORBAX Eclipse plus C18 column (4.6 mm × 100 mm, 3.5 μm) Temperature 20 ℃. Mass spectrometry conditions: electrospray ionization mode, multi-reaction monitoring mode (MRM), the detection ion pairs were m / z 567.2 ~ 345.1 (Polygalathin Ⅲ), m / z 753.3 ~ 205.1 sucrose). Results: The linear relationship between the two components was good and the analysis took only 6 min. The RSD of intragastric precision and daytime precision of farnesetin Ⅲ were 2.2% and 2.5%, respectively, and the recovery rates were 96.1% ~ 101.7% (RSD 2.4%). The intraday precision of 3,6’-diastereoyl sucrose And RSD of daytime precision were 2.3% and 2.4%, respectively. The recoveries ranged from 95.7% to 101.4% (RSD 2.0%). Conclusion: The method is rapid, sensitive and selective. It is suitable for the quantitative analysis of chlortonone Ⅲ and 3,6’-alanyl sucrose in Polygala.