摘要
以质量源于设计(QbD)理念为指导优选煅磁石的煅淬工艺,建立煅磁石XRD特征图谱,为煅磁石质量标准制定提供科学依据。根据《中国药典》中磁石的炮制方法和质量要求,以煅制温度、煅制时间、粒径大小、铺置厚度、醋淬次数为关键工艺参数(CPPs),以Fe元素质量分数、Fe^(2+)溶出、表面颜色为关键质量属性(CQAs),采用层次分析(AHP)和基于指标相关性的权重(CRITIC)相结合的方法确定权重系数,正交优选煅制工艺;以表面颜色为CQAs,并基于色度值原理客观量化煅磁石表面颜色,优选醋淬工艺,确定最佳炮制工艺;采用X射线衍射(XRD)技术建立煅磁石特征图谱,结合相似度评价、聚类分析及正交偏最小二乘判别分析(OPLS-DA)等方法对特征图谱进行质量评价。最终优选的煅磁石炮制工艺为煅制温度750℃、煅制时间1 h、铺置厚度4 cm、粒径0.4~0.8 cm、醋淬1次(磁石-醋10∶3),工艺验证稳定、可行;建立了以9个共有峰为特征指纹信息的煅磁石XRD特征图谱分析方法,平均数相关系数在0.839 5~0.988 1,平均数夹角余弦在0.914 4~0.995 6,相似性良好;聚类分析结果表明磁石、煅磁石可聚为一类,两者成分整体相似;OPLS-DA筛选3个关键特征峰,其中Fe_(2)O_(3)是区分两者的差异性成分。最终优选出的炮制工艺稳定、可行,并初步建立煅磁石XRD特征图谱,为后续煅磁石的质量控制及质量标准的制定提供参考。
Guided by the concept of quality by design(QbD),this study optimizes the calcination and quenching process of calcined Magnetitum and establishes the XRD characteristic spectra of calcined Magnetitum,providing a scientific basis for the formulation of quality standards.Based on the processing methods and quality requirements of Magnetitum in the Chinese Pharmacopoeia,the critical process parameters(CPPs)identified were calcination temperature,calcination time,particle size,laying thickness,and the number of vinegar quenching cycles.The critical quality attributes(CQAs)included Fe mass fraction,Fe^(2+) dissolution,and surface color.The weight coefficients were determined by combining Analytic Hierarchy Process(AHP)and the criteria importance though intercrieria correlation(CRITIC)method,and the calcination process was optimized using orthogonal experimentation.Surface color was selected as a CQA,and based on the principle of color value,the surface color of calcined Magnetitum was objectively quantified.The vinegar quenching process was then optimized to determine the best processing conditions.X-ray diffraction(XRD)was used to establish the characteristic spectra of calcined Magnetitum,and methods such as similarity evaluation,cluster analysis,and orthogonal partial least squares-discriminant analysis(OPLS-DA)were used to evaluate the quality of the spectra.The optimized calcined Magnetitum preparation process was found to be calcination at 750℃for 1 h,with a laying thickness of 4 cm,a particle size of 0.4-0.8 cm,and one vinegar quenching cycle(Magnetitum-vinegar ratio 10∶3),which was stable and feasible.The XRD characteristic spectra analysis method,featuring 9 common peaks as fingerprint information,was established.The average correlation coefficient ranged from 0.8395-0.9881,and the average angle cosine ranged from 0.9144 to 0.9956,indicating good similarity.Cluster analysis results showed that Magnetitum and calcined Magnetitum could be grouped together,with similar compositions.OPLS-DA discriminant analysis identified three key characteristic peaks,with Fe_(2)O_(3) being the distinguishing component between the two.The final optimized processing method is stable and feasible,and the XRD characteristic spectra of calcined Magnetitum was initially established,providing a reference for subsequent quality control and the formulation of quality standards for calcined Magnetitum.
作者
曾德雯
周靖惟
何天行
陈玉梅
徐欢欢
冯健
杨玥
陈欣
邹佳良
陈林
陈鸿平
陈士林
胡媛
刘友平
ZENG De-wen;ZHOU Jing-wei;HE Tian-xing;CHEN Yu-mei;XU Huan-huan;FENG Jian;YANG Yue;CHEN Xin;ZOU Jia-liang;CHEN Lin;CHEN Hong-ping;CHEN Shi-lin;HU Yuan;LIU You-ping(State Key Laboratory of Southwestern Chinese Medicine Resources,School of Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Sichuan New Green Pharmaceutical Technology Development Co.,Ltd.,Pengzhou 611930,China)
出处
《中国中药杂志》
北大核心
2025年第9期2391-2403,共13页
China Journal of Chinese Materia Medica
基金
第四次全国中药资源普查项目(GZY-KJS-2018-004,GZY-KJS-2019-001)。
作者简介
通信作者:胡媛,副教授,主要从事中药药效物质与质量评价研究,E-mail:huyuan@cdutcm.edu.cn;通信作者:刘友平,研究员,博士生导师,主要从事中药药效物质与质量评价研究,E-mail:youpingliu@cdutcm.edu.cn;曾德雯,硕士研究生,主要从事中药物质基础及质量标准研究,E-mail:2770587942@qq.com。
