摘要
Abstract
Objective To establish an HPLC method for determination of the related substances in active pharmaceutical ingredient ( API ) and preparations of flavoxate hydrochloride, and to investigate the real impurity levels of the products in 6 manufacturers. Methods The Phenomenex Luna C18 column ( 150 mm × 4. 6 mm, 5 μm ) was adopted, the mobile phase was buffer solution ( taken 1 g sodium hexane sulfonate and added water to make it dissolve, added 1 mL three ethylamine and 1 mL phosphoric acid, and then added water to 650 mL, shaken well ) -acetonitrile ( 65:35 ) , gradient elution, the flow rate was 1. 0 mL/min, the detection wavelength was 293 nm, and the column temperature was 30 ℃. Results The peak occurrence sequence was as follows:flavoxate hydrochloride, impurity A, impurity B, impurity C and impurity D, the separation degree of each peak was more than 1. 5. The linear ranges of impurity A, impurity B, impurity C, impurity D and flavoxate hydrochloride were 0. 2922-5. 8440, 0. 3063-6. 1260, 0. 3087-6. 1738, 0. 3212-6. 4232, 0. 1081-2. 1620 μg/mL. The average recoveries of impurities A, B, C and D were 98. 92％, 99. 11％, 100. 04％, 99. 48％, RSDs were 0. 62％, 1. 34％, 1. 02％, 1. 43％ ( n=6 ) , respectively, and the correction factors were 1. 5, 1. 4, 1. 3 and 1. 2, respectively. Conclusion The method has high sensitivity and good separation effect, it can simultaneously determine several process impurities and degradation impurities in flavoxate hydrochloride.关键词
盐酸黄酮哌酯/有关物质/3-甲基黄酮-8-羧酸/3-甲基黄酮-8-羧酸乙酯/校正因子/高效液相色谱法Key words
flavoxate hydrochloride/related substances/3-Methylflavone-8-carboxylic acid/3-Methylflavone-8-carboxylic acid ethyl ester/correction factor/HPLC分类
医药卫生
