垂体后叶素药效成分纯化工艺过程控制研究

Research on the process control method of active pharmaceuticalingredient in pituitrin

目的 建立符合药品生产企业检测标准要求,操作简捷易行、具有较高的可靠性、适合相关生产企业对该原料药质量过程控制的原料药垂体后叶素中药效成分含量的分析检测方法。方法 采用反相高效液相色谱法：色谱柱：Zorbax Eclipse XDB-C18（250mm×4.6mm,5μm）;色谱柱Column（P/N 993967-902/5063-6600）填料色谱柱;柱温：25℃;检测器：紫外可见检测器,检测波长：220 nm;流速：1.2 m L/min;色谱分析流动相：流动相A：0.13 mol/L的磷酸二氢钠水溶液,流动相B：50%乙腈水溶液;进样量：20μL;洗脱方式为梯度洗脱。结果 垂体后叶素中药效成分催产素、升压素含量采用本方法分析检测,操作简捷易行,可靠性好,精密度高。采用不同生物提取工艺方法A和B进行垂体后叶素注射液生产,所得产品中药效成分：催产素和升压素的含量略有差别,但浓度高低不同,其中工艺B所得浓度较高。结论 本研究建立了医药生产企业分析检测中心快速有效测定垂体后叶素原料药中催产素和升压素含量的有效方法,并能为原料药垂体后叶素分离纯化进行过程控制。本研究为原料药垂体后叶素的生产及研发提供相关技术信息。

Objective A novel Active Pharmaceutical Ingredient （API） pituitrin efficacy component content analysis method was explored, and the method is conformed to the requirements of the pharmaceutical production enterprise testing standard. Methods The reverse phase high performance liquid chromatography （RP-HPLC） was performed on a Zorbax Eclipse XDB-C18（250nunx4.6mm, 5 （jm） （P/N 993967-902/ 5063-6600） Column, the column temperature was 25^, the wavelength of detector was set at 220 mn, flow rate was 1.2 mL/min, 50% Acetonitrile- 0.13mol/L sodium dihydrogen phosphate aqueous solution was used as mobile phase for gradient elution. 20 {iL sample solution was injected in each perform. Results The content of oxytocin and vasopressin as pituitrin efficacy components were analyzed by this method with advantage of simple and easy operation, good reliability and high precision. Different biological extraction technology process A and B was used on pituitrin injection production, the content of medicinal ingredients in the product： oxytocin and vasopressin is slightly different, but concentration level is different, which process B concentration is higher than that of A. Conclusion In this study, an effective determination the levels o f oxytocin and vasopressin in pituitrin API method was established for a pharmaceutical production enterprise, can provide API ？如打 nn purification process control. Relevant technical information can be provided in the above, which worked on the biological API pituitrin research and development.