黄柏和酒黄柏中盐酸黄柏碱和盐酸小檗碱含量测定方法研究  

Study on the Determination Method of Phellodendrine Hydrochloride and Berberine Hydrochloride in Phellodendri Chinensis Cortex and Wine Processed Phellodendri Chinensis Cortex

作　　者：阮文辉 叶松华 冯夏珍 吴哲 薛润苗 王晓燕 罗晋萍 Ruan Wenhui;Ye Songhua;Feng Xiazhen;Wu Zhe;Xue Runmiao;Wang Xiaoyan;Luo Jinping(Shanxi Center of Drug Evaluation(Shanxi Institute of Medicine and Life Science),Taiyuan 030006,China;Center of Drug Inspection for Shanxi,Taiyuan 030031,China;Shanxi Institute for Food and Drug Control,Taiyuan 030031,China)

机构地区：[1]山西省药品审评中心(山西省医药与生命科学研究院),太原030006 [2]山西省药品检查中心,太原030031 [3]山西省食品药品检验所,太原030031

出　　处：《山东化工》2023年第1期112-117,共6页Shandong Chemical Industry

基　　金：山西省中药材、中药饮片地方标准研究项目(2019003);山西省重点研发计划项目(201903D321112);山西省中医药科研课题(2020ZYYC098)。

摘　　要：目的:改进黄柏饮片中盐酸黄柏碱(C_(24)H_(32)O_(6)·HCl)和盐酸小檗碱(C_(20)H_(18)NO_(4)·HCl)的高效液相色谱含量测定方法。方法:《中国药典》2020版所载黄柏饮片含测需要两次样本预处理、检测,操作繁琐,系统误差大。本研究采用一次性预处理样本、双波长切换、流动相梯度洗脱等实现一次进样即可同时检测盐酸黄柏碱(C_(24)H_(32)O_(6)·HCl)和盐酸小檗碱(C_(20)H_(18)NO_(4)·HCl)的含量,并进行了方法学验证。结果:线性关系:盐酸小檗碱浓度(1.018~10.179μg,R^(2)=0.9996)和盐酸黄柏碱浓度(224.0~1119.8 ng,R^(2)=0.9991);精密度:盐酸小檗碱(RSD=0.37%),盐酸黄柏碱(RSD=0.49%);重复性:盐酸小檗碱(RSD=0.37%),盐酸黄柏碱(RSD=0.49%);平均回收率:盐酸小檗碱(101.77%,RSD=2.22%),盐酸黄柏碱(98.32%,RSD=2.46%)。结论用改进后的方法测定了15批次不同产地的黄柏饮片和15批次黄柏酒炙品(酒黄柏)中的盐酸黄柏碱和盐酸小檗碱,改进后的方法简单易行,重复性好,稳定性强,可很好的用于黄柏及其酒炙品(酒黄柏)饮片的质量控制。Objective:To improve the HPLC method for the determination of berberine hydrochloride(C_(20)H_(18)NO_(4)·HCl)and berberine hydrochloride(C_(24)H_(32)O_(6)·HCl)in Phellodendri Chinensis Cortex.Methods:The content determination of Phellodendri Chinensis Cortex in Chinese Pharmacopoeia(2020 Edition)required twice sample pretreatment and detection,which was complicated and systematic error.In this paper,the contents of berberine hydrochloride(C_(20)H_(18)NO_(4)·HCl)and berberine hydrochloride(C_(24)H_(32)O_(6)·HCl)can be determined simultaneously by one-time sample pretreatment,dual wavelength switching and gradient elution of mobile phase.Results:The linear relationship was as follows:the concentration of berberine hydrochloride(1.018~10.179μg,R^(2)=0.9996)and the concentration of phellodendrine hydrochloride(224.0~1119.8 ng,R^(2)=0.9991).Precision:berberine hydrochloride(RSD=0.37%),berberine hydrochloride(RSD=0.49%).Repeatability:berberine hydrochloride(RSD=0.37%),berberine hydrochloride(RSD=0.49%).The average recoveries of berberine hydrochloride(101.77%,RSD=2.22%)and phellodendrine hydrochloride(98.32%,RSD=2.46%).Conclusion:The content of phellodendrine hydrochloride and berberine hydrochloride in 15 batches of Phellodendron amurense from different places and 15 batches of Phellodendri Chinensis Cortex processed in wine(wine processed Phellodendri Chinensis Cortex).The improved method is simple,reproducible and stable.It can be used for the quality control of Phellodendron amurense and its processed in wine(Phellodendron amurense).

关 键 词：黄柏 酒黄柏 高效液相色谱 

分 类 号：TQ461[化学工程—制药化工] O657.7[理学—分析化学]