基于二水平析因-星点设计法设计的五灵胶囊水溶性成分指纹图谱的研究  

Study of the chromatogram fingerprints of water-soluble components in Wuling Capsules based on Plackett Burman-central composite design

作　　者：刘妍 郝佳萌 刘妍如 唐志书 宋忠兴 刘红娜 周建平 曹兆军 LIU Yan;HAO Jiameng;LIU Yanru;TANG Zhishu;SONG Zhongxing;LIU Hongna;ZHOU Jianping;CAO Zhaojun(Shaanxi Collaborative and Innovation Center of Chinese Medicinal Resources and Industrialization,Shaanxi University of Chinese Medicine,Xianyang 712083,China;China Academy of Chinese Medical Sciences,Beijing 100700,China;Tsinghua De Ren Xi’an Happiness Pharmaceutical Co.,Ltd,Xi’an 710400,China)

机构地区：[1]陕西中医药大学,陕西省中药资源产业化协同创新中心,咸阳712083 [2]中国中医科学院,北京100700 [3]清华德人西安幸福制药有限公司,西安710400

出　　处：《西北药学杂志》2024年第5期39-47,共9页Northwest Pharmaceutical Journal

基　　金：中药大品种品牌价值提升示范研究项目(编号:202190025);现代农业产业技术体系建设专项资金项目(编号:CARS-21)。

摘　　要：目的 基于二水平析因-星点设计法(plackett burman-central composite design,PB-CCD)实验设计,建立五灵胶囊水溶性成分指纹图谱的测定方法。方法 采用PB设计实验,以两峰分离度、归一化分离因子、色谱信息量和色谱分层响应效能作为评价指标,优化影响指纹图谱液相分析的因素(检测波长、柱温、线性梯度时间、进样体积、流速、乙腈初始比例、甲酸比例和色谱柱类型)。进一步以CCD设计对筛选出的因素进行优化,确定水溶性成分指纹图谱建立的最佳工艺。以建立的测定方法计算10批五灵胶囊水溶性成分指纹图谱的相似度,评价各批样品的质量。结果 基于优化的测定条件,建立了五灵胶囊水溶性成分指纹图谱测定方法,确认了15个共有峰。方法学考察结果显示其专属性、重复性、稳定性、精密度均良好。10批五灵胶囊样品的相似度均大于0.95。结论 基于PB-CCD设计建立的五灵胶囊水溶性成分指纹图谱测定方法模型预测性良好,可用于五灵胶囊的质量控制。Objective To establish the chromatogram fingerprints of water-soluble components in Wuling Capsules based on the Plackett Burman-central composite design(PB-CCD).Methods The factors influencing the chromatogram fingerprint analysis were optimized firstly by utilizing PB experimental design.The sum of chromatographic peak resolutions(∑R s),normalized resolution factors(r),information contents(φ),and hierarchical chromatographic response function(HCRF)were set as response factors.Correspondingly,the detection wavelength,column temperature,duration time,sample inject volume,flow rate,and initial acetonitrile ratio etc.were set as observation factors.Subsequent optimization was conducted by using the CCD design to determine the optimal process for establishing the water-soluble component chromatogram fingerprints.Then,the similarity of the fingerprints of 10 batches Wuling Capsules was calculated by using the established methodology,and the quality of each batch was evaluated.Results Following the optimized parameters,the chromatogram fingerprints of water-soluble components in Wuling Capsules was established,and 15 common peaks were selected.The methodological examination indicates good specificity,repeatability,stability,and precision results.Furthermore,the similarity of the 10 batches of Wuling Capsule samples was calculated greater than 0.95.Conclusion The methodology for the Wuling Capsules water-soluble component chromatogram fingerprints was established by using the PB-CCD design,which exhibited a proper model fitting capabilities,and could be used for the quality control of this formulation in the future.

关 键 词：五灵胶囊 二水平析因-星点设计法(PB-CCD) 超高效液相色谱法 水溶性成分 指纹图谱 

分 类 号：R917[医药卫生—药物分析学]