Box-Behnken响应面法优化盆炎灵颗粒的醇沉工艺研究  

Study on the optimization of the ethanol precipitation process of Penyanling Granules by using Box-Behnken response surface methodology

作　　者：蔡霈[1,2] 郑艺 王哲明[2] 文晓柯 CAI Pei;ZHENG Yi;WANG Zheming;WEN Xiaoke(Department of Pharmaceutical Research,Hu′nan Provincial Maternal and Child Health Care Hospital,Hu′nan Province,Changsha410008,China;Hu′nan Engineering Research Center for Optimization of Drug Formulation and Early Clinical Evaluation,Hu′nan Province,Changsha410008,China)

机构地区：[1]湖南省妇幼保健院药学研究部,湖南长沙410008 [2]湖南省药物制剂优化与早期临床评价工程技术研究中心,湖南长沙410008

出　　处：《中国医药导报》2020年第22期32-37,共6页China Medical Herald

基　　金：湖南省自然科学基金项目(2017JJ2142);湖南省中医药管理局重点项目(201708)。

摘　　要：目的优化盆炎灵颗粒的醇沉工艺。方法在单因素试验的基础上,以醇沉前液相对密度、乙醇终浓度与静置时间为考察因素,以绿原酸、芍药苷、阿魏酸、丹酚酸B、去甲异波尔定、甘草苷、延胡索乙素、落新妇苷的转移率与固体去除率的综合评分值为考察指标,采用基于Box-Behnken设计的响应面法优化盆炎灵颗粒的醇沉工艺。色谱条件:色谱柱为Agilent TC-C18(250 mm×4.6 mm,5μm),流速1.0 mL/min,流动相A为乙腈,流动相B为0.2%磷酸水溶液,梯度洗脱(0~10 min,2%A;10~40 min,2%~12%A;40~80 min,12%~18%A;80~110 min,18%~25%A;110~120 min,25%~50%A),柱温30℃,检测波长200~400 nm。结果最佳醇沉工艺条件为醇沉前液相对密度1.13,乙醇终浓度60%,静置时间21 h。验证试验结果显示,综合评分的预测值与实测值相对偏差为0.7%。结论优化的醇沉工艺方法简单、操作简便且结果准确稳定,可为盆炎灵颗粒的制剂生产提供可靠的理论依据。Objective To optimize the ethanol precipitation process for Penyanling Granules.Methods Based on the single factor test,the relative density of the liquid before ethanol precipitation,the final ethanol concentration and the ethanol precipitation time were used as factors.The transfer rates of chlorogenic acid,paeoniflorin,ferulic acid,salvianolic acid B,norisoboldine,liquiritin,tetrahydropalmatine,astilbin and the composite score of solid removal rate were selected as evaluation indexes.The ethanol precipitation process of Penyanling Granules was optimized by Box-Behnken response surface method.Chromatographic conditions:the column was Agilent TC-C18(250 mm×4.6 mm,5μm),the flow rate was 1.0 mL/min.The mobile phase A was acetonitrile and the mobile phase B was 0.2%phosphoric acid solution with gradient elution(0-10 min,2%A;10-40 min,2%-12%A;40-80 min,12%-18%A;80-110 min,18%-25%A;110-120 min,25%-50%A).The column temperature was 30℃and the detection wavelength was 200-400 nm.Results The optimal ethanol precipitation process was as followed:the relative density of the extract was 1.13,and ethanol was added to allow the content of ethanol to reach 60%,and then been placed for 21 h.The test results indicated that the relative difference of comprehensive scoring value between predicated value and measured value was 0.7%.Conclusion The optimal ethanol precipitation process is simple,easy to operate and the results are accurate and stable,which can provide a reliable theoretical basis for the preparation production of Penyanling Granules.

关 键 词：Box-Behnken 响应面法 醇沉工艺 转移率 固体去除率 

分 类 号：R284.2[医药卫生—中药学]