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
  
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
Author NameAffiliation
FENG Wenhuan1, WU Zhengzhang2, ZHANG Peng2, CHANG Ming1, JIN Qingzhe1, WANG Xingguo1 1.National Functional Food Engineering Technology Research Center, School of Food Science and Technology, Jiangnan University, Wuxi 214122, Jiangsu,China
2.Jiangsu CONAT Biological Products Co., Ltd., Taixing 225400,Jiangsu,China 
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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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