论文部分内容阅读
[目的]对井冈霉素原药进行提纯,并测定其含量,以用于井冈霉素生产中的质量控制。[方法]选用混合溶剂对62%井冈霉素原药进行重结晶;利用苯酚“硫酸比色法对其含量进行测定,并研究了不同测定条件对含量测定结果的影响。[结果]经过重结晶后的样品,其纯度提高至97.7%。苯酚”硫酸比色法测定井冈霉素含量的最佳条件为:对照品为无水葡萄糖;苯酚用量5%;苯酚溶液1.0ml,浓硫酸用量5.0ml,反应后静置20min,检测波长490nm;葡萄糖标准曲线的相关系数(R2)为0.9939;平均加标回收率为99.72%,RSD为0.3628%。[结论]重结晶法可以很好的完成井冈霉素的精制;硫酸“苯酚比色法用于测定井冈霉素的含量,操作简单,准确度高,可靠性强,可以在工业化生产中推广应用。
[Objective] The Jinggangmycin original drug was purified and its content was determined for the quality control of Jinggangmycin production. [Method] The 62% validamycin was recrystallized by using mixed solvent. The content of phenol was determined by phenol / sulfuric acid colorimetric method and the influence of different measuring conditions on the determination of content was studied. [Result] After crystallization, the purity of the sample increased to 97.7%. The optimum conditions for the determination of validamycin by phenol- ”sulfuric acid colorimetry were as follows: the reference substance was anhydrous glucose; the amount of phenol was 5%; the amount of phenol solution was 1.0ml; 5.0ml, the reaction was allowed to stand for 20min, the detection wavelength was 490nm; the correlation coefficient (R2) of glucose standard curve was 0.9939; the average recovery was 99.72% with RSD 0.3628%. [Conclusion] The recrystallization method can be well Jing Jingmycin refined; sulfuric acid "phenol colorimetric method for the determination of the content of validamycin, simple operation, high accuracy, high reliability, can be promoted in industrial production application.