Schroeder A C, DiGiovanni J H, Von Bredow J, Heiffer M H
Department of Pharmacology, Walter Reed Army Institute of Research, Washington, DC 20307-5100.
J Pharm Sci. 1989 Feb;78(2):132-6. doi: 10.1002/jps.2600780212.
A high-performance liquid chromatographic (HPLC) method is described for quantitation of pralidoxime chloride and its decomposition products 2-carboxy-, 2-formyl-, and 2-(aminocarbonyl)-1-methylpyridinium chloride. These decomposition products and 2-cyano- and 2-(hydroxymethyl)-1-methylpyridinium chloride and 1-methyl-2(1H)-pyridinone were separated from pralidoxime chloride on a silica gel column using a mobile phase of acetonitrile:water (86:14) in which the aqueous component was 8.36 mM in tetraethylammonium chloride and 52.5 mM in acetic acid. This method allows quantitation of the relatively low levels of 2-formyl-1-methylpyridinium chloride formed in acidic solution at room temperature. Sensitivity was shown to be at least 5 ng of the pralidoxime chloride and 15 ng of the 2-carboxy-, 2-formyl-, and 2-(aminocarbonyl)-1-methylpyridinium chloride injected on column. The coefficient of variation was 4% or less for all components measured. Autoinjectors containing 300 mg/mL of pralidoxime chloride in water were stored at room temperature for 8-10 years, followed by analysis for hydrogen cyanide using an ion-selective electrode. Less than 15 micrograms of cyanide per autoinjector was detected. The HPLC analysis of the solutions after being stored an additional 3-4 years at approximately 5 degrees C demonstrated that greater than 90% of the total of all measured components consisted of pralidoxime chloride. The remaining percentage was made up of 2-carboxy-, 2-formyl-, and 2-(aminocarbonyl)-1-methylpyridinium chloride.
描述了一种高效液相色谱（HPLC）方法，用于定量测定氯解磷定及其分解产物2-羧基-、2-甲酰基-和2-（氨基羰基）-1-甲基吡啶鎓氯化物。这些分解产物以及2-氰基-和2-（羟甲基）-1-甲基吡啶鎓氯化物和1-甲基-2（1H）-吡啶酮在硅胶柱上与氯解磷定分离，流动相为乙腈：水（86:14），其中水相成分中氯化铵为8.36 mM，乙酸为52.5 mM。该方法可定量测定室温下在酸性溶液中形成的相对低水平的2-甲酰基-1-甲基吡啶鎓氯化物。结果表明，对注入柱中的氯解磷定，灵敏度至少为5 ng；对2-羧基-、2-甲酰基-和2-（氨基羰基）-1-甲基吡啶鎓氯化物，灵敏度至少为15 ng。所测所有组分的变异系数均为4%或更低。将含300 mg/mL氯解磷定水溶液的自动进样器在室温下储存8至10年，然后用离子选择性电极分析氰化氢。每个自动进样器检测到的氰化物含量低于15微克。在约5℃下再储存3至4年后，对溶液进行HPLC分析表明，所有测定组分总量中超过90%为氯解磷定。其余百分比由2-羧基-、2-甲酰基-和2-（氨基羰基）-1-甲基吡啶鎓氯化物组成。
