Laukó A, Horváth P, Trischler F, Görög S
Richter Gedeon Vegyészeti Gyár Rt., Budapest.
Acta Pharm Hung. 1992 May;62(3):82-7.
The following methods are described for the analytical investigation of the intermediates of the synthesis of pipecuronium bromide (Arduan) (for the numbering of the intermediates and their impurities see Figure 1.). 1. Gas chromatographic methods (capillary GC using fused silica capillaries Ultra-2 and Silar 10C WCOT) for the impurity profiling of intermediates I, II, IV and V including the identification and spectroscopic characterization of their impurities; 2. TLC methods for the similar characterisation of the further intermediates (III, VI, VII and VIII); 3. Gas chromatographic assay methods for IV and V using fused silica capillary technique and internal standards; 4. Potentiometric titration methods for the determination of VII and VIII using 0.1 M hydrochloric acid as the titrant.
以下是用于分析溴哌库铵(阿端)合成中间体的方法(中间体及其杂质的编号见图1)。1. 气相色谱法(使用熔融石英毛细管Ultra-2和Silar 10C WCOT的毛细管气相色谱法)用于中间体I、II、IV和V的杂质剖析,包括其杂质的鉴定和光谱表征;2. 薄层色谱法用于其他中间体(III、VI、VII和VIII)的类似表征;3. 使用熔融石英毛细管技术和内标的IV和V的气相色谱测定法;4. 电位滴定法,以0.1 M盐酸为滴定剂测定VII和VIII。