高效液相色谱法测定盐酸黄酮哌酯原料和制剂中有关物质  

Determination of Related Substance in Active Pharmaceutical Ingredient and Preparations of Flavoxate Hydrochloride by HPLC

作　　者：沈丹丹 曾杰 梁涵雁 姜学美 蒋晨 Shen Dandan;Zeng Jie;Liang Hanyan;Jiang Xuemei;Jiang Chen(Chongqing Institute for Food and Drug Control,Chongqing,China401121;Chongqing Research Center for Drug Process and Quality Control Engineering,Chongqing,China401121;Fuan Pharmaceutical

机构地区：[1]重庆市食品药品检验检测研究院,重庆401121 [2]重庆市药物过程与质量控制工程技术研究中心,重庆401121 [3]福安药业<集团>股份有限公司,重庆401121

出　　处：《中国药业》2018年第5期16-21,共6页China Pharmaceuticals

摘　　要：目的建立测定盐酸黄酮哌酯原料及制剂中有关物质的高效液相色谱(HPLC)法,考察6个厂家产品的真实杂质水平。方法色谱柱采用Phenomenex Luna C_18柱(150 mm×4.6 mm,5μm),流动相为缓冲液(取1 g己烷磺酸钠,加水适量使溶解,加三乙胺1 mL和磷酸1 mL,加水稀释至650 mL,摇匀)-乙腈(65∶35),梯度洗脱,流速为1.0 mL/min,检测波长为293 nm,柱温为30℃。结果盐酸黄酮哌酯、杂质A、杂质B、杂质C、杂质D依次出峰,各峰间分离度均大于1.5;杂质A,B,C,D及盐酸黄酮哌酯质量浓度分别在0.292 2~5.844 0,0.306 3~6.126 0,0.308 7~6.173 8,0.321 2~6.423 2,0.108 1~2.162 0μg/m L范围内与峰面积线性关系良好;杂质A,B,C,D平均回收率分别为98.92%,99.11%,100.04%,99.48%,RSD分别为0.62%,1.34%,1.02%,1.43%(n=6),校正因子分别为1.5,1.4,1.3,1.2。结论该方法灵敏度高,分离效果好,能同时测定盐酸黄酮哌酯中几种工艺杂质和降解杂质。To establish an HPLC method for determination of the related substances in active pharmaceutical ingredient(iVPI)and preparations of flavoxate hydrochloride,and to investigate the real impurity levels of the products in 6 manufacturers.Methods The Phenomenex Luna C1 column(150 mm x 4.6 mm,5μm)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 0.292 2-5.844 0,0.306 3-6.126 0,0.308 7-6.173 8,0.321 2-6.423 2,0.108 1-2.162 0μg/mL.The average recoveries of impurities A,B,C and D were 98.9 2%,99.1 1%,100.0 4%,99.4 8%,RSDs were 0.6 2%,1.3 4%,1.0 2%,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 

分 类 号：R917[医药卫生—药物分析学] R927.1[医药卫生—药学]