制川乌《中华人民共和国药典》含量测定方法的改进  

Improvement of Determination Method of Aconiti Radix Cocta in Chinese Pharmacopoeia

作　　者：赵振霞 段琼 孔亚萍 朱靖 刘永利 ZHAO Zhen-xia;DUAN Qiong;KONG Ya-ping;ZHU Jing;LIU Yong-li(Hebei Institute for Drug and Medical Device Control,Hebei Key Laboratory of Traditional Chinese Medicine Quality Evaluation and Standard Research,Shijiazhuang 050227,China;Hebei Medical University,Shijiazhuang 050017,China)

机构地区：[1]河北省药品医疗器械检验研究院河北省中药质量评价与标准研究重点实验室,河北石家庄050227 [2]河北医科大学,河北石家庄050017

出　　处：《中国现代中药》2023年第1期165-170,共6页Modern Chinese Medicine

基　　金：河北省市场监督管理局科研计划项目(2021YJ01)。

摘　　要：目的:改进《中华人民共和国药典》(以下简称《中国药典》)2020年版中制川乌含量测定方法,进一步优化固相萃取技术,建立同时测定制川乌中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱、乌头碱的高效液相色谱方法。方法:采用强阳离子吸附树脂MCX固相萃取小柱对制川乌进行纯化,制备供试品溶液;使用COSMOSIL C_(18)色谱柱(250 mm×4.6 mm,5μm),以甲醇、乙腈和0.1%磷酸水溶液为流动相梯度洗脱,流速为1.0 mL·min^(-1),柱温为25℃,检测波长为232 nm。结果:6个成分分别在各自范围内线性关系良好(r=0.9999),平均加样回收率分别为101.8%、100.2%、100.8%、99.0%、99.7%、98.2%,RSD分别为0.9%、1.2%、0.9%、1.3%、1.5%、1.0%。结论:改进了《中国药典》2020年版中制川乌含量测定的方法,解决了样品前处理复杂、使用有毒有害试剂较多的问题。建立了同时测定制川乌6个生物碱成分含量的方法,该方法准确、简便、快速、重复性好,对不同仪器和不同色谱柱的适应性好,可用于制川乌的质量控制。Objective:To improvement the method of determination of Aconiti Radix Cocta in Chinese Pharmacopoeia(2020 edition),and further optimize the technology of solid-phase extraction,thereby establishing a new high-performance liquid chromatography(HPLC)for the simultaneous determination of benzoylmesaconine,benzoylaconine,benzoylhypaconine,mesaconitine,hypaconitine,and aconitine in Aconiti Radix Cocta.Methods:The test solution was purified by solid-phase extraction using a strong cationic adsorption resin MCX column.The analysis was performed on COSMOSIL C_(18) column(250 mm×4.6 mm,5μm),with methanol-acetonitrile-0.1%phosphoric acid solution as the mobile phase in gradient elution,and the flow rate was 1.0 mL·min^(-1).The column temperature was 25℃and the detection wavelength was 232 nm.Results:Six constituents showed good linear relationships in their respective ranges(r=0.9999),and the average recoveries were 101.8%,100.2%,100.8%,99.0%,99.7%,and 98.2%respectively.The relative standard deviation(RSD)were 0.9%,1.2%,0.9%,1.3%,1.5%,and 1.0%,respectively.Conclusion:This experiment has improved the method for determination of Aconiti Radix Cocta in Chinese Pharmacopoeia(2020 edition)and also solved the problems such as the complex pretreatment of samples and excessive use of toxic and harmful reagents.The improved method for simultaneous determination of 6 alkaloids is established in this study,which is simple,rapid,and highly accurate.This method has good reproducibility and good adaptability to different instruments and chromatographic columns,which can be used for the quality control of Aconiti Radix Cocta.

关 键 词：制川乌 乌头碱 次乌头碱 新乌头碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 苯甲酰新乌头原碱 含量测定 

分 类 号：R282[医药卫生—中药学]