摘要
目的研究pH区带精制逆流色谱制备钩吻素子的工艺参数。方法在选定的溶剂体系下,采用pH区带精制逆流色谱分离钩吻总生物碱,以钩吻素子的得率、纯度以及分离时间为指标,分别研究主机螺旋管转速、流动相流速、恒温循环器温度对钩吻素子制备的影响,选择适合的工艺参数。结果当溶剂体系为甲基叔丁基醚-乙腈-水(3∶1.5∶4,V/V/V),上相加三乙胺至浓度为20mmol/L作为固定相,下相加盐酸至浓度为10mmol/L作为流动相,此时适合钩吻素子制备的工艺参数为:主机正向洗脱转速为850r/min,流动相流速为2.0mL/min,恒温循环器温度为25℃。结论在上述条件下,可应用pH区带精制逆流色谱自钩吻总碱中分离钩吻素子。
Objective To establish the technical parameters for preparing koumine by pH-zone-refining counter-current chromatography.Methods Under selected solvent system,the circulation water temperature,flow rate of the mobile phase and revolution speed were optimized in the light of the yield and purity of koumine and the separation time.Results Under the selected solvent system（MtBE-CH3CN-water=3∶1.5∶4,V/V/V,TEA was added to the upper organic stationary phase at 20 mmol/L and HCl was added to the lower aqueous phase at 10 mmol/L final concentration）,850 r/min for clockwise revolution speed,2.0 mL/min for flow rate of the mobile phase and 25 ℃ for the circulation water were selected in the pH-zone-refining counter-current chromatography.Conclusion Under the above defined conditions,koumine could be isolated perfectly by pH-zone-refining counter-current chromatography.
出处
《福建医科大学学报》
2011年第4期254-256,260,共4页
Journal of Fujian Medical University
基金
福建省改革与发展委员会产业技术开发项目[闽发改投资(2009)958号]
福建医科大学重大科研项目(ZD009)
福建医科大学苗圃科研基金(2010MP045)
关键词
色谱法
高压液相
钩吻碱
工艺学
制药
chromatography
high pressure liquid
GELSEMINE
technology
pharmaceutical
