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目的对刺五加80%体积分数乙醇提取物采用水解原位萃取的方法将结合态异秦皮啶转化成游离态异秦皮啶。方法确定的工艺条件为每克80%体积分数乙醇浸膏按固液比1∶100加入0.6 mol.L-1盐酸,加入同体积的1,2-二氯乙烷,搅拌下85℃回流水解2.5 h。结果在此条件下,刺五加根皮、茎皮和根茎混合异秦皮啶分别由原来的0.042 4、0.011 2和0.005 3 mg.mL-1增加到1.264 1、0.441 2和0.260 0 mg.mL-1,分别增加28.81、38.39和48.06倍;根木质部和茎木质部由水解前检测不到异秦皮啶增加到0.023 3和0.009 7 mg.mL-1。结论将水解原位萃取法分离异秦皮啶工艺与目前常用的传统酸水解-有机溶剂萃取工艺进行了对比,水解温度由原来的100℃降低到85℃,处理时间由原来的14.5 h降低到2.5 h,溶剂使用量仅为原来的3/4。
OBJECTIVE To convert 80% ethanolic extract of Acanthopanax senticosus into free isofenzil by the method of in situ extraction by hydrolysis. The process conditions were as follows: 80% ethanol extract per gram was added with 0.6 mol·L-1 hydrochloric acid at a solid-to-liquid ratio of 1: 100 and the same volume of 1,2-dichloroethane was added, 2.5 h. Results Under this condition, the isofenzuron mixture of root, bark and rhizome increased from 0.042 4, 0.011 2 and 0.005 3 mg.mL-1 to 1.264, 0.441 2 and 0.260 0 mg.mL -1, increased by 28.81, 38.39 and 48.06 times respectively; the xylem and xylem in roots did not detect isofuranton up to 0.023 3 and 0.009 7 mg.mL-1 by hydrolysis. Conclusion The separation of isoflavipine by in situ extraction was compared with the conventional acid hydrolysis-organic solvent extraction. The hydrolysis temperature was reduced from 100 ℃ to 85 ℃ and the treatment time was reduced from 14.5 h to 2.5 h, solvent usage is only 3/4 of the original.