基于QbD理念的血竭烫伤膏分析方法与其工艺量值传递研究  

Analytical Methods for Draconis Sanguis Scald Ointment Based on QbD Concept and Study on Its Process Quantity Transfer

作　　者：姜慧洁 赵奇江 慎凯峰 刘奇[1] 胡云莉[1] 章越 周丹英[1] JIANG Huijie;Zhao Qijiang;SHEN Kaifeng;LIU Qi;HU Yunli;ZHANG Yue;ZHOU Danying(Zhejiang Traditional Chinese Medicine Research Institute Co.,Ltd.,Hangzhou 310023,China;Department of General Medical,Affiliated Hospital of Shaoxing University,Shaoxing 312000,China)

机构地区：[1]浙江省中药研究所有限公司,杭州310023 [2]绍兴文理学院附属医院全科医疗科,浙江绍兴312000

出　　处：《中国药学杂志》2024年第17期1651-1657,共7页Chinese Pharmaceutical Journal

基　　金：绍兴市科技计划项目资助(2022A14032)。

摘　　要：目的基于质量源于设计(quality by design,QbD)理念研究血竭烫伤膏中血竭素含量测定方法,并对成型工艺进行量值传递研究。方法以血竭素含量为关键质量属性,通过Plackett-Burman设计筛选供试品制备中的关键分析参数;通过Box-Behnken设计评价关键质量属性与关键分析参数间关系。针对烫伤膏药材、中间体、成品的特性,建立不同的血竭素含量测定方法,并进行量值传递研究。血竭烫伤膏含量测定中供试品制备条件:加石油醚除去羊毛脂,以7%磷酸甲醇溶液为提取溶剂,60℃水浴提取30 min。色谱条件:以乙腈-0.05 mol·L^(-1)磷酸二氢钠溶液为流动相,梯度洗脱;流速1.0 mL·min^(-1);检测波长440 nm;柱温40℃。结果通过分析可知血竭烫伤膏制备工艺可行,药材到成品过程中血竭素转移率达90%以上。结论基于QbD理念开发的血竭烫伤膏分析方法能够准确测定血竭素含量,利于产品质量评价与工艺量值传递研究。OBJECTIVE To develop a method for the determination of dracorhodin in Draconis Sanguis scald ointment based on the concept of quality by design(QbD),and to study its preparation process for quantitative transfer.METHODS Using the content of dracorhodin as key quality attribute,the key analytical parameters in preparation of test solution were selected through Plackett-Burman design.The relationship between key quality attribute and key analysis parameters was evaluated through Box-Behnken design.According to characteristics of the medicinal material,intermediate and finished product of scald ointment,the different methods for determining content of dracorhodin were established,and the law of quantity transfer was studied.The preparation conditions of test solution for content determination of Draconis Sanguis scald ointment were as follows:lanolin was removed by petroleum ether,extraction solvent was 7%phosphoric acid methanol solution,and extraction was carried out in a water bath at 60℃for 30 min.The chromatographic conditions were as follows:the mobile phase was consisted of acetonitrile and 0.05 mol·L^(-1)sodium dihydrogen phosphate solution using a gradient elution.Temperature was 40℃and flow rate was 1.0 mL·min^(-1),at a detector wavelength of 440 nm.RESULTS The feasibility of preparation process of Draconis Sanguis scald ointment was proven.The transfer rate of dracorhodin from medicinal material to finished product was over 90%.CONCLUSION The analytical method developed based on concept of QbD could accurately determine content of dracorhodin in Draconis Sanguis scald ointment,which is conducive to product quality evaluation and process value transfer research.

关 键 词：质量源于设计 血竭烫伤膏 血竭素 量值传递 

分 类 号：R917[医药卫生—药物分析学]