响应面法优化藏红花素碱水解制备反式藏红花酸工艺  

Optimization of the Preparation of Trans-crocetin from Crocin by Alkaline Hydrolysis via Response Surface Methodology

作　　者：王吉宇 李成文 徐彦靖 于青 刘楠 刘东春[1] WANG Jiyu;LI Chengwen;XU Yanjing;YU Qing;LIU Nan;LIU Dongchun(School of Chinese Materia Medica,Shenyang Pharmaceutical University,Shenyang 110016,China;School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]沈阳药科大学中药学院,辽宁沈阳110016 [2]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《食品工业科技》2021年第23期176-183,共8页Science and Technology of Food Industry

基　　金：2019年辽宁省自然科学基金计划指导计划项目(2019-ZD-0447);2019年教育部“春晖计划”合作科研项目(LN2019016);2019年沈阳药科大学中青年教师事业发展支持(ZQN2019012)。

摘　　要：目的:研究优化藏红花素碱水解制备反式藏红花酸的工艺,进而精制得到高纯度反式藏红花酸。方法:采用单因素实验初步考察水解反应时间、温度、氢氧化钠浓度对反式藏红花酸的产率的影响,进而采用BoxBehnken设计响应面试验进行参数优化。结果:反应时间60.0 min,温度80.0℃,氢氧化钠浓度1.70 mg/mL为最佳水解条件,此条件下得到纯度为86.0%、产率为80.09%的反式藏红花酸粗品,经重结晶后其纯度提高到99.3%,纯化产物经核磁共振碳谱和氢谱分析,确定为全反式藏红花酸。结论:碱水解藏红花素后重结晶的方法可以简便有效的制取高纯度全反式藏红花酸。Objective: To optimize the preparation conditions of trans-crocetin from crocin by alkaline hydrolysis for obtaining trans-crocetin with high purity. Methods: A single factor experiment was used to preliminarily investigate the influence of the hydrolysis reaction time, temperature, and alkali concentration on the yield of trans-crocetin. Then the BoxBehnken design response surface experiment was used to optimize the parameters. Results: The best hydrolysis conditions were determined as follows: the reaction time, temperature and alkali concentration were 60.0 min, 80.0 ℃ and 1.70 mg/mL respectively. Under this condition, crude trans-crocetin with purity of 86.0% was obtained, the yield was 80.09%. After recrystallization, the purity of the crude product was increased to 99.3%. The purified product was determined to be alltrans-crocetin by carbon nuclear magnetic resonance(13 C NMR) and hydrogen spectrum(1 H NMR) analysis. Conclusion: It is an effective method of alkaline hydrolysis from crocin and recrystallization to prepare trans-crocetin with high purity.

关 键 词：藏红花素 藏红花酸 响应面法 结构鉴定 碱水解 

分 类 号：R15[医药卫生—营养与食品卫生学]