培植牛黄中7种胆汁酸类成分含量测定方法的建立及验证  

Development and Validation of Simultaneous Determination of 7 Kinds of Bile Acids in Cultured Bezoar

作　　者：和晶 吕宝俊 汪国鹏 HE Jing;LYU Baojun;WANG Guopeng(Hospital of Renmin University of China,Beijing 100872,China;Shang Pharmacy(Ningxia)Pharmaceutical Co.,Ltd.,Yinchuan 750004,China;Zhongcai Health(Beijing)Biological Technology Development Co.,Ltd.,Beijing 101503,China)

机构地区：[1]中国人民大学医院,北京100872 [2]尚药局制药有限公司,宁夏银川750004 [3]中财瀚熙生物科技发展有限公司,北京101503

出　　处：《中医药学报》2023年第3期41-47,共7页Acta Chinese Medicine and Pharmacology

摘　　要：目的:基于分析方法质量源于设计理念,建立与优化同时测定培植牛黄中7种胆汁酸含量分析方法。方法:应用Plackett-Burman和全析因设计筛选和优化色谱参数;应用设计空间确定关键色谱参数的最优值和控制范围。最后,对所建立的分析方法进行方法学验证。结果:设计空间确定关键色谱参数范围和最优值:柱温可接受范围:30~40℃,最优值35℃;乙腈初始浓度范围可接受范围:38.8%~41.6%,最优值40%;乙腈终点浓度可接受范围:61.3%~64.60%,最优值63%。方法学验证各项指标均合要求。鹅去氧胆酸、去氧胆酸、牛黄脱氧胆酸钠、甘氨胆酸钠、甘氨脱氧胆酸钠的相对校正因子分别为1.15、1.19、1.29、1.54、1.49。结论:所建立的胆汁酸含量测定分析方法准确稳定,可用于同时测定培植牛黄中7种胆汁酸的含量。Objective:To develop and optimize the determination method of 7 kinds of bile acids in cultured bezoar based on analytical quality by design concept(AQbD).Methods:Plackett-Burman and full factorial design were used to screen and optimize the critical chromatographic parameters affecting chromatographic separation.The design space was used to determine the optimum and acceptable range of three critical chromatographic parameters.Finally,the developed analytical method was validated.Results:The design space was utilized to determine the optimum and control range of three key parameters,i.e.,column temperature acceptable range was 30-40℃,with the optimum value of 35℃;pH acceptable range for starting concentration of acetonitrile was 38.8%-41.6%,with the optimum value of 40%;acceptable range for final concentration of acetonitrile was 61.3%-64.60%,with the optimum value of 63%.The analytical method validation met the standard.The relative correlation factors of chenodeoxycholic acid,deoxycholic acid,tauroursodeoxycholic acid,glycocholic acid and glydeoxycholic acid were calculated to be 1.15,1.19,1.29,1.54 and 1.49,respectively.Conclusion:The developed analytical method is accurate and stable and can be used to determine the contents of 7 kinds of bile acids in cultured bezoar simultaneously.

关 键 词：方法质量源于设计 培植牛黄 胆汁酸 设计空间 相对较正因子 

分 类 号：R284[医药卫生—中药学]