毒性中药天仙子有效成分的液相色谱-质谱法定性定量分析

目的: 总结中药天仙子毒性毒理,针对现有质量标准检定方法建立一个专属性较强的毒性药效成分定性与定量分析方法。 方法: 采用Restek Allure PFP Propyl (2.1 mm×100 mm,5 μm)色谱柱,流动相为乙腈-醋酸铵缓冲液(20∶80),流速200 μL·min^-1,分流比率9∶1,进样量10 μL;正离子多反应监测模式监测,扫描范围为m/z 200~350的高效液相色谱-质谱联用方法,对天仙子中毒性药效成分进行定性鉴别和含量测定。 结果: 利用东莨菪碱及阿托品的液相色谱分离及其特征质谱-质谱图,对3批不同产地药材进行定性定量分析,总莨菪碱(以阿托品计)含量范围为0.02%~0.05%之内。 结论: 本文建立的液相色谱-质谱联用技术具有专属性强等优点,可为质量标准修订提供参考。

Objective: To review the toxicity and pharmacology actions of a commonly used potent Chinese medicinal material,Hyoscyami Semen.To establish a highly selective analytical method for the qualitative and quantitative analysis of the toxic and active compounds of Hyoscyami Semen with reference to existing quality control methods. Methods: LC-MS/MS technique which was performed on Restek Allure PFP Propyl(2.1 mm×100 mm,5 μm) column with acetonitrile-ammonium acetate buffer solution (20∶80) as the mobile phase at flow rate of 200 μL·min^-1 with split ratio 9∶1,and positive ion multiple reaction monitoring(MRM) mode,scanning the range of m/z 200-350 was employed for qualitative identification and quantitative determination of the toxic and active compounds for Hyoscyami Semen. Results: With the use of liquid chromatography separation and MS/MS spectrum characteristics,scopolamine,atropine and other related alkaloids present in Hyoscyami Semen could be identified and quantified,respectively.The method was applied to the analysis of 3 batches of herbs collected from different sources and the total scopolamine and atropine content was found in the range of 0.02%-0.05%(calculated as at atropine). Conclusion: A highly selective LC-MS/MS method is developed which can serve as a reference method for quality control purposes.