| 冯文欢1，吴正章2，张 鹏2，常 明1，金青哲1，王兴国1.超声辅助分步结晶法制备高纯度豆甾醇的工艺研究[J].中国油脂,2019,44(10):129~135.[FENG Wenhuan1, WU Zhengzhang2, ZHANG Peng2, CHANG Ming1,
JIN Qingzhe1, WANG Xingguo1.Preparation of high purity stigmasterol with ultrasound-assisted fractional crystallization[J].China Oils and Fats,2019,44(10):129~135.] |
| 超声辅助分步结晶法制备高纯度豆甾醇的工艺研究 |
| Preparation of high purity stigmasterol with ultrasound-assisted fractional crystallization |
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| DOI： |
| 中文关键词: 植物甾醇 豆甾醇 超声辅助 富集 精制 |
| 英文关键词:phytosterol stigmasterol ultrasound-assist enrichment purification |
| 基金项目:植物甾醇和植物甾醇酯的行业标准研究（18DZ2200300）；上海市2018年度“科技创新行动计划”技术标准项目 |
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| 中文摘要: |
| 通过富集和精制两步法分离纯化豆甾醇，采用非极性溶剂结晶法富集植物甾醇中的豆甾醇，在此基础上利用超声辅助在极性溶剂中对豆甾醇进一步重结晶精制。采用单因素实验对豆甾醇富集和精制工艺条件进行优化。结果表明：优化的富集工艺条件为以环己酮为溶剂、料液比1∶ 3.5、养晶温度25 ℃、养晶时间16 h，在此条件下重复结晶5次，豆甾醇纯度提高到94.69%；优化的精制工艺条件为以丙酮为溶剂、超声时间3 min、超声功率90 W、料液比1∶ 70、养晶温度25 ℃、养晶时间3 h，在此条件下重结晶2次，最终将豆甾醇的纯度提高至99.36%；经质谱、红外光谱和核磁等结构鉴定确认样品为豆甾醇。 |
| 英文摘要: |
| Stigmasterol was separated and purified from phytosterol by two-step method of enrichment and purification. Stigmasterol was firstly enriched by crystallization with non-polar solvent，then purified by ultrasound-assisted recrystallization with polar solvent. The conditions of enrichment and purification processes of stigmasterol were optimized by single factor experiment. The results showed that the purity of stigmasterol reached 94.69% by five times crystallization under the optimal enrichment conditions of with cyclohexanone as solvent,ratio of material to liquid 1∶ 3.5，crystal growth temperature 25 ℃ and crystal growth time 16 h. And the purity of stigmasterol increased to 99.36% by twice recrystallization under the optimal purification conditions of with acetone as solvent,ultrasonic time 3 min,ultrasonic power 90 W,ratio of material to liquid 1∶ 70，crystal growth temperature 25 ℃ and crystal growth time 3 h. The samples were identified as stigmasterol by MS，FT-IR and NMR. |
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