烯丙孕素对照品的研制及标定

Development and Calibration of Altrenogest

研制了烯丙孕素对照品并对其进行标定。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,高效液相色谱法进行纯度检查,质量平衡法进行定量分析,并用核磁共振波谱法对赋值结果进行验证。结果显示,烯丙孕素对照品原料纯度为99.96%;质量平衡法赋值结果为99.92%,定量核磁共振法验证结果为99.60%。烯丙孕素工作对照品定量赋值结果准确、可靠,能够用于烯丙孕素原料及制剂的鉴别和含量测定。

To develop and calibrate chemical reference substance of Altrenogest,the structure of the material was characterized by ultraviolet-visible(UV),infrared(IR),nuclear magnetic resonance(NMR),mass spectrum and X-ray single crystal diffraction.Its chromatographic purity was determined by HPLC.The result of qualitative identification of Altrenogest was 99.96%.The assigned value by mass balance method was 99.92%,in accordance with that obtained by the method of quantitative NMR(99.60%).The structure and purity of the Altrenogest material met the requirements of CRS for assay.The accuracy of the assigned value obtained by mass balance method was accurate and reliable.Thus the altrenogest material can be used for quality control.