防风色原酮类对照提取物制备工艺研究

Preparation technology of the control extract of chromone from Saposhnikovia divaricata

目的:建立防风色原酮类对照提取物制备工艺。方法:采用正交设计实验以及单因素考察法对防风色原酮类成分的提取、富集以及纯化等工艺进行研究,建立防风色原酮类对照提取物的最佳制备工艺,并进行工艺验证。结果:防风色原酮类成分的最佳提取工艺为:10倍量70%乙醇提取3次,每次2 h,合并3次提取液,回收溶剂;防风70%乙醇提取物加水分散,使上样液浓度为3.84 mg/mL(以总色原酮量计),通过AB-8型大孔吸附树脂法柱,吸附流速1.0 mL/min,树脂柱径高比为1∶8,上样量为7.68 mg/mL(以总色原酮量计),以10%乙醇洗脱2 BV进行除杂,流速为1.0 mL/min,再用5 BV 70%乙醇洗脱,流速为2.0 mL/min,收集70%乙醇洗脱液,即为防风色原酮部位;防风色原酮部位加甲醇溶解,与200~300目硅胶按1∶1.3的比例拌样,将硅胶按径高比为1∶15干法装柱,再以环己烷-醋酸乙酯-甲醇(1∶9∶1.5)1.6 BV洗脱,合并含有目标成分的硅胶部分,加甲醇洗脱,回收溶剂、减压干燥得防风色原酮类对照提取物。结论:该研究建立的制备工艺准确性高、重复性好,可用于防风色原酮类对照提取物的制备,为后续防风色原酮类对照提取物的标定定值及相关应用研究等提供了基础。

Objective:TO establish the optimal preparation process of the control extract of chromone from Saposhnikovia divaricata.Methods:We used the rthogonal design and single factor experiment to study the extraction,enrichment and purification of chromone from Saposhnikovia divaricata.The optimal preparation process of chromone from Saposhnikovia divaricata reference extract was established and verified.Results:We used denary of 70%ethanol to extract the Saposhnikovia divaricata 2 h for three times,then combined 3 extracts.The sample concentration of 70%ethanol extract of Saposhnikovia divaricata was adjusted to 3.84 mg/mL(based on total chromones),the adsorption flow rate was 1.0 mL/min,the ratio of diameter to height of resin column was 1∶8,the sample volume was 7.68 mg/mL(based on total chromones),2 BV was eluted with 10%ethanol,the flow rate was 1.0 mL/min,and then 5 BV 70%ethanol was eluted,the flow rate was 2.0 mL/min to prepare Saposhnikovia divaricata.The sample was dissolved and mixed with 200~300 mesh silica gel in the ratio of 1∶1.3.The silica gel was packed in the ratio of diameter to height of 1∶15 by dry method,and then eluted 1.6 BV with cyclohexane-ethyl-acetate methanol(1∶9∶1.5).The silica gel containing the target component was combined,eluted with methanol,and dried under reduced pressure to obtain the control extract of Saposhnikovia chromone.Conclusion:The preparation process established in this study has high accuracy and good repeat-ability.This can be used for the preparation of the control extract of Saposhnikovia providing a basis for the related research and calibration of the control extract of Saposhnikovia.