加米霉素对照品标定方法的建立

Establishment of Chemical Reference Substance of Gamithromycin

关键词:  加米霉素  对照品标定  结构确证  质量平衡法  定量核磁共振

Key words:  Gamithromycin  substance calibration  structural characterization  standard material analysis  mass balance method

摘要:

建立加米霉素对照品的标定方法。采用紫外光谱、红外光谱、核磁共振波谱、质谱和X射线单晶衍射进行结构确认；采用高效液相色谱法进行纯度检查,采用质量平衡法进行定量分析,并采用定量核磁技术对赋值结果进行验证。结果加米霉素对照品原料纯度为99.9%；质量平衡法赋值结果为98.8%,定量核磁共振法验证结果为98.3%。加米霉素对照品原料定量赋值结果准确、可靠,能够用于加米霉素原料及制剂的鉴别和含量测定。

Abstract:

To establish Chemical Reference Substance of Gamithromycin.The structure of the candidate material was characterized by ultraviolet-visible(UV), infrared(IR), nuclear magneticresonance(NMR), mass spectrum and x-ray single crystal diffraction. Its chromatographic purity was determined by HPLC. The results of qualitative identification of Gamithromycin was 99.9%. The assigned value by mass balance method was98.8%, in accordance with that obtained by quantitative NMR(98.3%. The structure and purity of the Gamithromycin material met the requirements of CRS for assay. The accuracy of the assigned value obtained by mass