花椒生物碱富集纯化工艺优化及其成分分析  

Optimization of purification process and component analysis of alkaloids from Zanthoxylum bungeanum Maxim

作　　者：杨贺英 罗彩萍 彭婷 梁文仪 沈颂章 苏娟 YANG Heying;LUO Caiping;PENG Ting;LIANG Wenyi;SHEN Songzhang;SU Juan(School of Medicine,Shanghai University,Shanghai 200444,China;National Demonstration Center for Experimental Military Pharmacy Education,Naval Medical University,Shanghai 200433,China)

机构地区：[1]上海大学医学院,上海200444 [2]海军军医大学军事药学国家级实验教学示范中心,上海200433

出　　处：《药学实践与服务》2025年第2期75-81,共7页Journal of Pharmaceutical Practice and Service

基　　金：国家自然科学基金(82304813);大学生创新能力培养项目(FH2023095)。

摘　　要：目的优化大孔树脂富集纯化花椒生物碱的工艺条件,并进行成分分析。方法单因素实验与正交试验相结合,以羟基-α-山椒素(HAS)、羟基-β-山椒素(HBS)含量为指标,确定最佳工艺参数。利用超高效液相色谱-四级杆-飞行时间质谱(UPLC-Q-TOF-MS^(E))技术定性分析生物碱类化学成分。结果最佳条件为选用三菱HP-20型大孔树脂,上样液浓度为0.2 g生药/ml,生药量与树脂体积比为1 g∶2.5 ml,树脂柱径高比为1∶7,以每小时4倍柱体积(BV)的速率动态吸附,静置1 h;20%乙醇2 BV除杂;80%乙醇5 BV洗脱。HAS、HBS的含量分别为4.71%、1.02%,共鉴定出20种生物碱。结论该方法稳定可行,得到高纯度多种类的花椒生物碱,可用于花椒生物碱的富集纯化。Objective To optimize the process conditions and analyze the components of alkaloids from Zanthoxylum bungeanum Maxim(Z.bungeanum)using macroporous resin.Methods Combining single factor tests and orthogonal tests,the content of hydroxy-α-sanshool(HAS)and hydroxy-β-sanshool(HBS)were considered as indexes to determine the best process parameters.Ultra-performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry(UPLC-Q-TOF-MS^(E))was used to identify the structures of alkaloids.Results The optimal conditions were Mitsubishi HP-20 macroporous resin,the loading solution concentration was 0.2 g crude drug/ml,the ratio of crude drug to resin volume was 1 g∶2.5 ml,the diameter/height ratio of resin column was 1∶7,the dynamic adsorption flow rate was 4 times of bed volume(BV)per hour,and the adsorption time was 1 h.Impurities were removed by using 2 BV of 20%ethanol,5 BV of 80%ethanol was used to elution,and the content of HAS and HBS was 4.71%and 1.02%,respectively.A total of 20 alkaloids were identified from Z.bungeanum.Conclusion This method was stable and feasible,obtaining high purity and various kinds of alkaloids,which could be used for the enrichment and purification of alkaloids from Z.bungeanum.

关 键 词：花椒 生物碱 大孔树脂 正交设计 超高效液相色谱-四级杆-飞行时间质谱 

分 类 号：R28[医药卫生—中药学]