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机构地区:[1]内蒙古自治区医院药剂处,呼和浩特010017 [2]第二军医大学海医系毒物药物研究室,上海200433
出 处:《药学服务与研究》2011年第3期193-195,共3页Pharmaceutical Care and Research
基 金:国家自然科学基金资助项目(No.20872179);上海市科委中药现代化项目(No.08DZ1971504)
摘 要:目的:优化用超临界CO2从丹参中萃取丹参酮ⅡA的工艺条件,并建立纯化丹参酮ⅡA的柱层析法。方法:以HPLC法测定丹参酮ⅡA的含量。采用正交试验优化超临界CO2萃取丹参酮的条件,考察夹带剂用量、萃取压力、萃取温度和分离温度对提取效果的影响。用100~200目的中性氧化铝柱层析,以苯进行洗脱,收集相关流份,减压回收溶剂后经无水乙醇重结晶得到丹参酮ⅡA晶体。结果:超临界CO2萃取丹参酮ⅡA的最优条件为:夹带剂用量120 ml,萃取压力20 MPa,萃取温度50℃,分离温度35℃。柱层析后重结晶得到纯度为93.49%的丹参酮ⅡA晶体。结论:超临界CO2萃取丹参酮具有操作简便、方法可靠、切实可行、无有机溶剂残留的优点,结合柱层析法可获得高纯度晶体。Objective:To optimize the supercritical CO2 extraction technology of tanshinone ⅡA from Salvia miltiorrhiza Bge.and establish a column chromatography for purification of tanshinone ⅡA crystal.Methods: HPLC method was used to determine the content of tanshinone ⅡA.Technology of supercritical CO2 extract was optimized by orthogonal test.The influential factors of supercritical CO2 extraction,including the amount of entrainer,extraction pressure,extraction temperature and separation temperature were investigated.Crude extract was purified by column chromatography with 100-200 mesh neutral aluminum oxide using benzene as eluent.After recovery of benzene by vacuum distillation,tanshinoneⅡA crystal was obtained by recrystallization with ethanol.Results: The optimal technology of supercritical CO2 extraction was as follows: 120 ml entrainer,extraction pressure at 20 MPa,extraction temperature at 50 ℃ and separation temperature at 35 ℃.The purity of tanshinoneⅡA crystal was up to 93.49%.Conclusion: Supercritical CO2 extraction method is simple,reliable and feasible for extraction of tanshinone ⅡA from Salvia miltiorrhiza Bge.,and there is no residual organic solvent.TanshinoneⅡA of high purity can be obtained by supercritical CO2 extraction combined with column chromatography.
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