首批异替勃龙国家对照品的标定研究

Standardization of the First Batch National Standard of Isobolone

目的制备并标定首批异替勃龙国家对照品,以有效控制替勃龙及其制剂产品质量。方法应用红外光谱、质谱、核磁共振谱对异替勃龙进行结构确证,采用反相高效液相色谱(HPLC)法测定待标品纯度,采用质量平衡法对待标品进行赋值,并对待标品的均一性和稳定性进行考察。结果异替勃龙待标品经标定,以C_(21)H_(28)O_(2)计,含量为99.6%;均一性考察符合要求,25℃±2℃、RH 75%±5%条件,40℃±2℃、RH 75%±5%条件,光照4500 lx±500 lx条件下放置10 d,纯度略有下降。结论本批待标品确认为异替勃龙,可作为第一批异替勃龙国家对照品,以供异替勃龙HPLC法鉴别和含量测定用,以C_(21)H_(28)O_(2)计,本批待标品含量为99.6%。

Objective To prepare and calibrate thefirst batch national standard(NS)of isobolone in order to assure the quality of tibolone and its preparation.Methods The structure of isobolone was confirmed by infrared spectroscopy,mass spectrometry,and nuclear magnetic resonance spectroscopy.RP-HPLC method was used to determine the purity,the mass balance method was used to assign a value to the candidate preparation.Thermal stability and uniformity test for the candidate preparation were carried out.Results The content of the NS candidate of isobolone is 99.6%as C_(21)H_(28)O_(2).The uniformity inspection meets the requirements.The purity decreased slightly placed under 25℃±2℃,RH 75%±5%conditions,40℃±2℃,RH 75%±5%conditions,light 4500 lx±500 lx conditions for 10 days.Conclusions The candidate preparation was confirmed to be the isobolone to serve as thefirst batch NS isobolone which can be used for HPLC identification,content determination.The content of the NS candidate of isobolone is 99.6%as C_(21)H_(28)O_(2).