核黄素超声结晶工艺优化

doi:10.16085/j.issn.1000-6613.2020-0585

化工进展 ›› 2021, Vol. 40 ›› Issue (2): 1018-1024.DOI: 10.16085/j.issn.1000-6613.2020-0585

核黄素超声结晶工艺优化

陈亮¹(), 田飞豹², 辛秀兰¹, 兰蓉¹, 于然¹, 吴志明¹, 梁浩²^,³()

^1.北京电子科技职业学院生物工程学院，北京 100176
^2.北京化工大学化工资源有效利用国家重点实验室，北京 100029
^3.北京化工大学秦皇岛环渤海生物产业研究院，河北秦皇岛 066000

收稿日期:2020-04-14 修回日期:2020-07-04 出版日期:2021-02-05 发布日期:2021-02-09
通讯作者: 梁浩
作者简介:陈亮（1986—），男，博士研究生，从事天然色素的研究开发。E-mail：chenliang@bpi.edu.cn。
基金资助:
2019年度北京市属高校高水平教师队伍建设支持计划青年拔尖人才培育计划(CIT&TCD 201904047)

Optimization of ultrasonic crystallization process of riboflavin

Liang CHEN¹(), Feibao TIAN², Xiulan XIN¹, Rong LAN¹, Ran YU¹, Zhiming WU¹, Hao LIANG²^,³()

^1.College of Bioengineering, Beijing Polytechnic, Beijing 100176, China
^2.State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China
^3.Qinhuangdao Bohai Biological Research Institute of Beijing University of Chemical Technology, Qinhuangdao 066000, Heibei, China

Received:2020-04-14 Revised:2020-07-04 Online:2021-02-05 Published:2021-02-09
Contact: Hao LIANG

摘要/Abstract

摘要：

核黄素作为药品、色素、营养及动物饲料添加剂被广泛应用，目前生产及销售的核黄素基本上都是针状晶习，其堆密度小、分散性和流动性差，影响压片等加工性能。本文对酸溶法、碱溶法等5种核黄素结晶纯化方法进行了筛选，发现酸溶法收率和纯度的综合效益最佳；在此基础上采用超声辅助结晶，对功率、时间及温度进行优化，通过透射电镜（TEM）及X射线衍射分析法（XRD）等表征方法对结果进行分析。最终确定超声结晶的最佳实验条件为：超声功率为400W，超声时间为40min，超声温度为50℃，核黄素的收率可达到95%，纯度超过96%。核黄素晶习和结晶度有所改善，便于加工应用。

关键词: 核黄素, 超声结晶, 工艺, 优化, 纯化

Abstract:

Riboflavin is widely used as medicine, pigment, nutritional additives, and feed additives. At present, riboflavin in production and sale is mostly needle-like crystals with low bulk density, poor dispersion and fluidity, which affects the processing performance, e.g. tableting. In this paper, five methods of riboflavin crystal purification, such as acid dissolving method and alkali dissolving method, were screened, and the comprehensive benefit of the yield and purity of acid dissolving method was found to be the best; on this basis, ultrasonic assisted crystallization was used to optimize the power, time and temperature, and the results were analyzed by transmission electron microscopy (TEM) and X-ray diffraction (XRD) and other characterization methods. The results show that the optimum parameters for ultrasonic crystallization are: the ultrasonic power is 400W, the ultrasonic time is 40 minutes, and the ultrasonic temperature is 50℃, the yield of riboflavin can reach 95%, and the purity is more than 96%. The crystal habit and crystallinity of riboflavin are improved, which is convenient for its processing and application.

Key words: riboflavin, ultrasonic crystallization, process, optimization, purification

中图分类号:

陈亮, 田飞豹, 辛秀兰, 兰蓉, 于然, 吴志明, 梁浩. 核黄素超声结晶工艺优化[J]. 化工进展, 2021, 40(2): 1018-1024.

Liang CHEN, Feibao TIAN, Xiulan XIN, Rong LAN, Ran YU, Zhiming WU, Hao LIANG. Optimization of ultrasonic crystallization process of riboflavin[J]. Chemical Industry and Engineering Progress, 2021, 40(2): 1018-1024.

图/表 8

图1 核黄素结构式

表1 5种核黄素结晶方法的收率和纯度

序号	收率/%	纯度/%	综合收益/%
溶剂析出法	88.90±2.13	96.56±1.09	85.84±3.03
溶剂析出结合酸溶法	92.7±1.89	94.19±1.25	87.31±2.94
控制结晶法	93.79±1.64	93.03±1.89	87.25±3.30
酸溶法	95.24±1.73	97.15±2.10	92.53±3.68
碱溶法	90.90±2.35	89.08±1.57	80.97±3.52

图2 超声作用时间对结晶纯度和收率的影响

图3 超声功率对结晶纯度和收率的影响

图4 超声温度对结晶纯度和收率的影响

图5 未超声辅助结晶和超声辅助结晶后核黄素的光学显微图（40倍）

图6 未超声辅助结晶和超声辅助结晶后核黄素的电镜透射图

图7 超声功率为400W、不同超声时间下核黄素结晶的XRD谱图

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核黄素超声结晶工艺优化

Optimization of ultrasonic crystallization process of riboflavin

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