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作 者:朱海鸥[1,2] 单淇[3] 刘顺[3,4] 朱晓薇[1] 侯文彬[3]
机构地区:[1]天津中医药大学,天津300193 [2]天津传染病医院,天津300192 [3]天津药物研究院,天津300193 [4]南京中医药大学附属医院,江苏南京210029
出 处:《中成药》2011年第1期49-53,共5页Chinese Traditional Patent Medicine
基 金:天津市科委重点攻关项目(033187511)
摘 要:目的:优选土贝母总皂苷的提取纯化工艺。方法:以总皂苷中含量较高的土贝母苷甲转移率为考察指标,采用正交设计对提取工艺进行优化;采用HPLC法结合薄层显色法考察6种大孔树脂对土贝母总皂苷的分离富集性能,选出最优树脂,确定最佳纯化工艺条件。结果:正交试验表明,以60%的乙醇20倍体积(8∶6∶6),提取3次,每次1.5 h,提取效率最高,苷甲转移率达89.71%。通过对树脂的考察优选出对土贝母皂苷甲吸附率和解吸率都很高的NKA-9树脂,上样浓度为0.2 g/mL,以水洗脱除杂后,用95%乙醇洗脱得到土贝母总皂苷,上样、洗脱流速为3B V/h。结论:以此提取纯化工艺制得3批样品,平均土贝母总皂苷得率3.34%,含量达90.66%,平均苷甲含量30.67%。AIM:To optimize the extraction and purification of tubeimosides from Bolbostemma paniculatum.METHODS:The transfer rate of tubeimosideⅠ was taken as marker and the orthogonal design was applied.Both HPLC and TLC were used to investigate the separation and enrichment behavior of six kinds of macroporous resin,including HPD-400,DM-301,AB-8,DA-201,HPD100 and NKA-9.RESULTS:The orthogonal design indicated that the maximum extraction efficiency of Bolbostemma paniculatum could be gained under the condition of reflux with 60% ethanol for 3 times(1.5 hour each time) and solution volume 20 times as much as the weight of raw ma-terials(8 ∶ 6 ∶ 6).The transfer rate of tubeimoside Ⅰ was 89.71%.Finally NKA-9 possessed the good absorption and de-absorption property among the 6 selected resins.With the HPLC and TLC analysis,the loading concentra-tion was determined as 0.2 g/mL and eluded with 95% ethanol after water washing.Loading flow rate and elution flow rate were determined at 3 BV/h.CONCLUSION: Three batches of total tubeimosides were prepared based on the methods as above,and the average yield rate of total tubeimosides is 3.34%,with 90.66% of an average content,and 30.67% of average content of tubeimoside Ⅰ.
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