目的 研究大孔树脂富集骆驼蓬中总生物碱提取后废液中骆驼蓬碱和去氢骆驼蓬碱的最佳工艺条件。方法 用HPLC测定生物碱含量，以骆驼蓬碱和去氢骆驼蓬碱的吸附量和解吸率为考察指标，对6种不同类型的树脂（LSA-8b、LSA-5b、XDA-1、LSA-21、LSA-10、D101）进行评价。考察药液pH值、吸附流速、吸附温度、洗脱流速等参数对骆驼蓬碱和去氢骆驼蓬碱的吸附和洗脱效果的影响。结果 LSA-5b对骆驼蓬碱和去氢骆驼蓬碱具有较好的富集能力，最佳富集工艺条件：吸附pH值为9，吸附温度为30 ℃，上样流速为3.5 BV（倍柱体积）·h-1，骆驼蓬碱饱和吸附量为32.34 mg·g-1；最佳的洗脱溶剂为体积分数为70%乙醇，最佳洗脱流速为1.5 BV·h-1，洗脱用量为16.7 BV，骆驼蓬总生物碱洗脱率达86.3%。结论 在确定的工艺条件下，体积分数70%的乙醇洗脱液中骆驼蓬总生物碱的含量提高了10倍。
Abstract
OBJECTIVE To optimize enrichment parameters of alkaloids including harmaline (HAL) and harmine (HAR) from the remainder extracts of Peganum harmala by macroporous resins. METHODS The enrichment of HAL and HAR were studied on six types of macroporous resins with special structures. HAL and HAR were determined by HPLC. The performance of HAL and HAR on macroporous resins including LSA-8b，LSA-5b，XDA-1，LSA-21，LSA-10 and D101 was compared according to their adsorption and desorption properties. The conditions of the processing volume, concentrations of HAL and HAR in solution, the pH value of solution, flow rate, and temperature were optimized. RESULTS According to the adsorption, desorption capacities and the adsorption isotherms, LSA-5b was demonstrated with a remarkable capability for enrichment of HAL and HAR from the remainder extracts of P. harmala. The optimal conditions were： the solution pH of 9, flow rate of 3.5 BV·h-1, and temperature of 30 ℃. The gradient elution program was as follows： water for 4 BV then 70% ethanol for 16.7 BV. CONCLUSION The performance achieved good enrichment and higher recovery of HAL and HAR (for 10 folds higher) from remainder extracts of P. harmala by using LSA-5b resin. It is a fast and effective method for the enrichment of HAL and HAR.
关键词
骆驼蓬 /
骆驼蓬碱 /
去氢骆驼蓬碱 /
大孔吸附树脂
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Key words
Peganum harmala L. /
harmaline /
harmine /
macroporous resins
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参考文献
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