食品科学 ›› 2013, Vol. 34 ›› Issue (7): 56-61.doi: 10.7506/spkx1002-6630-201307013

• 基础研究 • 上一篇    下一篇

辅酶Q10微细颗粒的反溶剂重结晶法制备与表征

桑 梅,隋小宇,宋 瑱,赵修华,祖元刚*   

  1. 东北林业大学 森林植物生态学教育部重点实验室,黑龙江 哈尔滨 150040
  • 收稿日期:2012-01-13 修回日期:2013-03-01 出版日期:2013-04-15 发布日期:2013-03-20
  • 通讯作者: 祖元刚 E-mail:zygorl@yahoo.com.cn
  • 基金资助:
    国家公益性行业(林业)科研专项(201204601)

Preparation by Antisolvent Recrystallization Method and Characterization of Coenzyme Q10 Microparticles

SANG Mei,SUI Xiao-yu,SONG Zhen,ZHAO Xiu-hua,ZU Yuan-gang*   

  1. Key Laboratory of Forest Plant Ecology, Ministry of Education, Northeast Forestry University, Harbin 150040, China
  • Received:2012-01-13 Revised:2013-03-01 Online:2013-04-15 Published:2013-03-20
  • Contact: ZU Yuan-gang E-mail:zygorl@yahoo.com.cn

摘要: 为了提高辅酶Q10的亲水性,采用反溶剂重结晶法制备辅酶Q10微粒。考察药物质量浓度、体系温度、搅拌速率及搅拌时间等因素对辅酶Q10微粒平均粒径的影响,优化辅酶Q10微粒制备的工艺条件。实验利用扫描电镜、X射线衍射、红外光谱分析和差示扫描量热分析等方法对辅酶Q10原药及辅酶Q10微粒的性质进行表征。结果表明:通过调整工艺条件,可以控制微粒的粒径尺寸。优化获得的工艺条件为:药物质量浓度50mg/mL、溶剂与反溶剂体积比1:6、体系温度4℃、搅拌速率4000r/min、搅拌时间10min。按此工艺,可以制备得到平均粒径为1.84μm的微细颗粒。表征结果显示,辅酶Q10微粒的化学结构与原药相比未发生变化,但熔点及分解温度均降低,晶体衍射峰强度减弱。

关键词: 辅酶Q10, 反溶剂, 重结晶, 微粒

Abstract: Coenzyme Q10 microparticles with improved hydrophilicity were prepared by antisolvent crystallization method. We investigated the effects of Coenzyme Q10 concentration, system temperature, stirring speed and stirring time on average micro-particle size. In addition, the preparation conditions were optimized. Properties of coenzyme Q10 and micro-particles were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), infrared spectroscopy (FT-IR) and differential scanning calorimetry (DSC) analysis. The results showed that powder particle size could be adjusted by changing the process conditions. The optimal preparation conditions were 50 mg/mL, 1:6, 4 ℃, 4000 r/min and 10 min for substrate concentration, solvent/anti-solvent volume ratio, system temperature, stirring speed and stirring time, respectively. Under these conditions, the average diameter of micro-particles was 1.84 μm. The chemical structure of coenzyme Q10 microparticles did not reveal an obvious change when compared with coenzyme Q10, but the melting point and decomposition temperature revealed a decrease, and the intensity of crystal diffraction peak became weaker.

Key words: coenzyme Q10, antisolvent, recrystallization, micro-particles

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