基于UPLC-Triple-TOF-MS技术初步分析雅安产道地中药材川牛膝中生物碱成分  

Preliminary Analysis of Alkaloids from Ya′an Dao-di Herbs Cyathulae Radix by UPLC-Triple-TOF-MS

作　　者：王悦秋[1] 王昌 梁林辉 梁大伟[1] Wang Yueqiu;Wang Chang;Liang Linhui;Liang Dawei(School of Pharmacy&Medical Laboratory Science,Ya′an Polytechnic College,Ya′an 625100,China;Key Laboratory of Structure-based Drug Design&Discovery of Ministry of Education,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]雅安职业技术学院药学与检验学院,四川雅安625100 [2]沈阳药科大学基于靶点的药物设计与研究教育部重点实验室,辽宁沈阳110016

出　　处：《山东化工》2024年第3期155-157,160,共4页Shandong Chemical Industry

基　　金：雅安市应用技术研究与开发项目(21KJJH0080);雅安市科技创新创业苗子工程重点项目(YKZ20211307)。

摘　　要：采用乙醇提取、成盐、二氯甲烷萃取等方法初步富集川牛膝总生物碱,确定最优提取分离工艺;通过超高液相色谱串联三重四级杆飞行时间质谱法,采用Waters XSelect CSH-C_(18)色谱柱(2.1 mm×150 mm,1.7μm),梯度洗脱,流速为0.3 mL/min,测试波长254 nm,柱温为50℃,进样量为3μL,采用电喷雾离子源正离子模式,扫描范围为m/z 100~1500,并采用全扫描模式对样品数据进行收集,根据高分辨质谱结合二级质谱所得信息对川牛膝中生物碱类化学成分进行快速鉴定,通过对比分子离子峰和碎片离子的质荷比、Scifinder和Reaxy数据库及相关文献,推测出两种生物碱成分。研究建立的生物碱类化学成分提取与分析方法,为提高雅安产道地中药材川牛膝的质量控制水平及后续阐明药效物质基础提供了实验依据。The alcohol extraction,salinization,dichlormethane extraction and concentration methods were adopted to extract and separate the total alkaloid from Cyathulae Radix and determine the optimal extraction and separation process.To establish a rapid qualitative analysis method for alkaloids in Cyathulae Radix by ultra-performance liquid chromatography triple quadrupole timeof-flight mass spectrometry(UPLC-Triple-TOF-MS),the Waters XSelect CSH-C_(18)column(2.1 mm×150 mm,1.7μm)was used,the mobile phase was 0.1%aqueous formic acid solution(A)-acetonitrile(B)with gradient elution,the flow rate was 0.3 mL/min,the UV detection wavelength was 254 nm,the column temperature was 50℃,and the injection quantity was 3μL.Electrospray ion source positive ion mode was adopted,and the scanning range was m/z 100~1500.The sample data were collected by full scanning mode,and the alkaloid composition of Cyathulae Radix was quickly identified according to the information obtained by high-resolution mass spectrometry combined with secondary mass spectrometry.Two kinds of alkaloids in Cyathulae Radix were detected through the mass-to-charge ratio of molecular ion peaks and fragment ions,the Scifinder and Reaxy databases,and the literatures.The method of qualitative analysis of the alkaloids established in this study provides experimental basis for improving the quality control level and further elucidating the pharmacodynamic substance basis of Ya′an Dao-di herbs Cyathulae Radix.

关 键 词：川牛膝 生物碱 提取方法 超高液相色谱串联三重四级杆飞行时间质谱法 定性分析 

分 类 号：O657.63[理学—分析化学]