银菊解毒口服液大孔树脂纯化工艺研究

目的在指纹图谱的基础上,联用AHP-CRITIC混合加权法、Plackett-Burman设计(PBD)与Box-Behnken设计(BBD),多目标筛选银菊解毒口服液(YJOL)的纯化工艺。方法采用HPLC法建立YJOL HPLC图谱,以6种指标成分绿原酸、蒙花苷、R,S-告依春、哈巴俄苷、补骨脂素、异补骨脂素的回收率和HPLC图谱相似度为指标,筛选10种大孔树脂中最佳型号。AHP-CRITIC混合加权法赋予6种指标成分的回收率和相似度权重,计算综合指标作为评价标准,运用PBD筛选显著性影响因素,结合BBD优选大孔树脂纯化YJOL的最佳工艺参数。结果 HPD-400型大孔树脂对复方中6个指标成分的富集选择性最高。最佳工艺参数为径高比1∶7,上样pH值3.5,上样质量浓度0.18 g/m L,上样量(药材:树脂)0.96g/g,8 BV的77%乙醇洗脱。纯化后6个指标成分的回收率为78%~98%,HPLC指纹图谱相似度大于0.99,成分均衡回收。模型综合评价预测值为94.28%,实验所得综合评价为93.69%,相对偏差0.59%。结论在HPLC图谱的基础上,联用AHP-CRITIC混合加权法、PBD与BBD筛选YJOL纯化工艺是科学可行的,不仅能提高有效成分的纯度,还能保持化学成分的一致性。

Purification technology of Yinju Jiedu Oral Liquid

Objective To multi-objectively optimize the purification process parameters of Yinju Jiedu Oral Liquid (YJOL), mixed weight of AHP-CRITIC, Plackett-Burman design (PBD), and Box-Behnken design (BBD) were adopted on the basis of HPLC fingerprints. Methods HPLC was used to establish HPLC fingerprint of YJOL. Recovery rate of fingerprints of six components (chlorogenic acid, linarin, harpagoside, R,S-epigoitrin, psoralen, and isobalin) and HPLC fingerprint similarity was taken as the index to optimize the type of macroporous resin among 10 types. Weights of the recovery rates of six components and similarity were determined by mixed weight of AHP-CRITIC, in order to obtain the comprehensive index as the evaluation criterion. The significantly influencing factors were firstly evaluated by PBD, and purification conditions were optimized by BBD. Results HPD-400 type resin showed a high selectivity for six components. The optimized purification technology was as follows:the ratio of dia-height was 1:7, pH value was 3.5, sample concentration was 0.18 g/mL, ratio of sample to resin was 0.96 g/g, and 77% ethanol''s dosage was 8 BV. Under the conditions, the recovery rates of six components were 78%-98%, and the similarity of fingerprint was higher than 0.99. These components could get balanced recovery. Moreover, the theoretical and actual comprehensive indexes were 94.28% and 93.69%, respectively, with a relative error of 0.59%. Conclusion Based on HPLC fingerprints, mixed weight of AHP-CRITIC, combined with PBD and BBD-RSM used to optimize the purification process for the YJOL in this study is scientific and feasible, this way can improve the purity of the active components and keep the uniformity of main components in the YJOL as well.