Lawrence R C, Lovering E G, Poirier M A, Watson J R
J Pharm Sci. 1980 Dec;69(12):1444-5. doi: 10.1002/jps.2600691227.
One lot of meprobamate raw material and 28 lots of tablets were examined for impurities by TLC. All lots contained di-(2-methyl-2-propyl-3-carbamoyloxypropyl) carbonate (V) at levels that ranged between 0.1 and 1.0% of the total drug content. Nine lots also contained low levels of a second impurity (approximately 0.1%), and one of these lots contained a third impurity (approximately 0.1%), neither of which was identified. Estimates of the unidentified impurities were based on the assumption of a TLC response with furfural-hydrochloric acid spray equivalent to that of meprobamate. Compound V was identified by mass spectrometry and PMR and IR spectroscopy and by comparison of the TLC Rf value to that of a synthesized sample of V.
采用薄层色谱法对一批甲丙氨酯原料药和28批片剂进行杂质检查。所有批次中均含有二-(2-甲基-2-丙基-3-氨甲酰氧基丙基)碳酸酯（V），其含量占药物总含量的0.1%至1.0%。9个批次还含有低水平的第二种杂质（约0.1%），其中一个批次含有第三种杂质（约0.1%），均未鉴定出具体成分。未鉴定杂质的含量估计是基于糠醛-盐酸喷雾薄层色谱响应与甲丙氨酯相当的假设。化合物V通过质谱、核磁共振氢谱和红外光谱以及将薄层色谱比移值与V的合成样品进行比较来鉴定。
