化学合成香叶醇-β-D吡喃葡萄糖苷的分离纯化
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(1. 广东海洋大学食品科技学院,广东 湛江 524088;2. 青岛科技大学化学与分子工程学院,山东 青岛 266042;3. 青岛科技大学化工学院,山东 青岛 266042;4. 云南中烟工业有限责任公司技术中心,云南 昆明 650231)

作者简介:

程东伟,男,广东海洋大学在读硕士研究生。

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国家自然科学基金资助项目(编号:21275035);云南中烟工业有限责任公司技术中心科技项目(编号:HYHH2013HX03);云南中烟工业有限责任公司科技项目(编号:2013CP02)


Separation and purification geraniol-beta-D-glycosidase by chemical synthesis
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(1. College of Food Science and Technology, Guangdong Ocean University, Zhanjiang, Guangdong 524088, China; 2. College of Chemistry and Molecular Engineering, Qingdao University of Science & Technology, Qingdao, Shandong 266042, China;3. College of Chemical Engineering, Qingdao University of Science & Technology, Qingdao, Shandong 266042, China; 4. Technology Center of China Tobacco Yunnan Industrial Co., Ltd., Kunming, Yunnan 650231, China)

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    摘要:

    为实现化学合成的香叶醇-β-D-吡喃葡萄糖苷的高效、系统分离纯化,采用改进的Koenigs-Knorr法,以硅胶担持碳酸银催化剂提高合成收率,利用硅胶柱层析及高效液相(HPLC)对粗样品进行分离纯化,硅胶柱层析通过薄层层析选择较佳的流动相配比,即乙酸乙酯和乙醇按照501,401,301依次进行梯度洗脱,利用HPLC 技术的高精密性,其流动相乙腈水为5545,分别纯化合成的粗品。结果表明:采用新型的催化剂使产物收率由56.1%提高到75%,收率得以较为显著的提高;且硅胶柱层析得到产物纯度为90.12%,HPLC纯化得到的产物纯度为98.66%,两种层析方法均可得到纯度较佳的香叶醇糖苷;为香叶醇吡喃葡萄糖苷合成及纯化提供一定的借鉴。

    Abstract:

    In order to find an efficient and systematic way of producing and purifying geraniol glycosidase,an improved method of Koenigs-Knorr was gotten, which used the silicone to hold silver carbonate catalyst to improve the productivity and perfects the synthesis process, separating and purifying the crude sample by silica gel column chromatography(SGCC) and high performance liquid chromatography (HPLC) . The method of SGCC applies the thin plate chromatography to get the better flow matches which is the ethyl acetate and ethanol according to 50:1, 40:1, 30:1, but the HPLC selects water and acetonitrile which is to 45:55, each of the two flows with the raw sample. The results showed that the new way of synthsis could improve product yield from 61% to 68% and simplify the synthesis process; The purity of the final product purified by silica gel was 90.12%, and the purity of the final product purified by HPLC was 98.66%, both of them could get the better purity of geraniol glycoside. It provides a reference for the synthesis and purification of geraniol glycosidase.

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程东伟,杨锡洪,解万翠,等.化学合成香叶醇-β-D吡喃葡萄糖苷的分离纯化[J].食品与机械,2016,32(6):171-175.
CHENGDongwei, YANGXihong, XIEWancui, et al. Separation and purification geraniol-beta-D-glycosidase by chemical synthesis[J]. Food & Machinery,2016,32(6):171-175.

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  • 收稿日期:2016-01-05
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  • 在线发布日期: 2023-03-09
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