Rutherford B S, Bishara R H
J Pharm Sci. 1976 Sep;65(9):1322-5. doi: 10.1002/jps.2600650915.
A GLC method of analysis of a new antiarrhythmic agent, aprindine, is described. The raw material of the new drug substance, supplied as the hydrochloride salt, is dissolved in deionized water, and the base is liberated by a 10% aqueous solution of sodium carbonate. aprindine is extracted with chloroform and mixed with the internal standard, 5alpha-cholestane. GLC is perfomed on a glass column packed with 3.8% W-98 on Chromosorb W-HP. Quantitation is achieved by computer calculation of the peak area ratios. GLC-mass spectral analysis indicates that the observed peak is that of aprindine, with a molecular ion at m/e 322. The retention times of aprindine and the internal standard are 2.0 and 5.8 min, respectively. All synthetic precursors show a shorter retention time than aprindine. This GLC method is applied to the quantitative determination of aprindine as raw material and in capsule and ampul formulations. The method is also used to measure the stability of aprindine to acid, base, dry, heat, refluxing, and UV light and to pH variations.
本文描述了一种用于分析新型抗心律失常药物安搏律定的气相色谱法。作为盐酸盐提供的新药原料溶解于去离子水中，并用10%的碳酸钠水溶液释放出其碱基。安搏律定用氯仿萃取，并与内标物5α-胆甾烷混合。气相色谱分析在填充有3.8% W-98（Chromosorb W-HP）的玻璃柱上进行。通过计算机计算峰面积比实现定量分析。气相色谱-质谱分析表明，观察到的峰是安搏律定的峰，其分子离子峰为m/e 322。安搏律定和内标物的保留时间分别为2.0分钟和5.8分钟。所有合成前体的保留时间均短于安搏律定。该气相色谱法用于定量测定作为原料以及胶囊和安瓿制剂中的安搏律定。该方法还用于测定安搏律定对酸、碱、干燥、加热、回流和紫外线以及pH变化的稳定性。
