摘要
目的优选“红黄白”凝胶的提取工艺并建立该制剂的含量测定方法。方法采用高效液相色谱(HPLC)梯度洗脱法测定红景天苷、盐酸小檗碱和1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯的含量;采用蒽酮-硫酸法测定总多糖的含量;采用层次分析法-基于指标客观性的权重赋权法(AHP-CRITIC)复合加权法计算4个指标的权重系数,以综合得分为评价指标,结合L_(9)(3^(4))正交试验设计,考察料液比、提取时间和提取次数对“红黄白”凝胶提取工艺的影响,优选最佳提取工艺并进行工艺验证;建立该制剂中4种指标成分的含量测定方法并进行方法学考察。结果“红黄白”凝胶的最佳提取工艺为料液比1∶45、提取时间2 h、提取2次;4种指标成分在各自线性范围内线性关系良好,均R^(2)>0.9990;平均加样回收率为98.67%~102.09%,RSD为0.77%~3.17%;精密度、重复性和稳定性良好,RSD≤2.28%。结论AHP-CRITIC复合加权法结合正交试验优选的“红黄白”凝胶最佳提取工艺稳定且经济合理;该凝胶的含量测定方法操作可行,结果可靠,为该制剂质量标准的建立提供了实验依据。
Objective To optimized the extraction process of the"Honghuangbai"gel and to establish the content determination method of the gel.Methods The contents of salidroside,berberine hydrochloride and 1,4-bis[4-(glucose-oxy)benzyl]-2-isobutyl malate in"honghuangbai"extract were determined by HPLC with gradient elution;the content of total polysaccharide was determined by anthrone-sulfuric acid method.AHP-CRITIC composite weighting method was used to calculate the weight coefficient of 4 indicators,and the comprehensive score was taken as the evaluation index.Combined with L_(9)(3^(4))orthogonal experiment design,the effects of solid-liquid ratio,extraction time and times on the extraction process of"honghuangbai"gel were investigated,and the optimal extraction process was selected and verified.The method for the determination of 4 index components in the gel was established and the methodology was investigated.Results The optimal solid-liquid ratio was 1∶45,the optimal extraction time was 2 h and the optimal extraction times was twice.The linear relationships of the four indexes were good in their respective linear ranges,with R^(2)>0.9990.The average recoveries were 98.67%~102.09%,and RSD was 0.77%~3.17%.Good precision,repeatability and stability,RSD≤2.28%.Conclusion The optimal extraction process of"honghuangbai"gel optimized by AHP-CRITIC combined with orthogonal test is stable and economical.The method of the gel content determination is feasible and the result is reliable,which provides experimental basis for the establishment of the quality standard of the gel.
作者
高艳果
朱海涛
黄良永
叶方
王启斌
郑涛
陈黎
GAO Yanguo;ZHU Haitao;HUANG Liangyong;YE Fang;WANG Qibin;ZHENG Tao;CHEN Li(Department of Pharmacy,Taihe Hospital,Hubei University of Medicine,Shiyan 442000,China;Institute of Wudang Traditional Chinese Medicine,Taihe Hospital,Hubei University of Medicine,Shiyan 442000,China;School of Pharmaceutical Sciences,Hubei University of Medicine,Shiyan 442000,China)
出处
《医药导报》
北大核心
2025年第8期1322-1329,共8页
Herald of Medicine
基金
国家自然科学基金青年基金项目(81703582)
湖北省卫生健康科研基金(WJ2021ZH0017,WJ2019M057)
“十四五”湖北省高等学校优势特色学科群(生物与医药)项目(2024BMXKQT3,2023BMXKQT3,2022BMXKQT3)。
