高效液相色谱法测定盐酸达泊西汀中9种杂质

Determination of nine impurities in dapoxetine hydrochloride by high performance liquid chromatography

建立了高效液相色谱法测定盐酸达泊西汀中9种工艺杂质和降解杂质的含量。采用飞诺美Gemini C_(18)色谱柱,以0.04%(体积分数)二乙胺-10 mmol/L碳酸氢钠水溶液作为流动相A,乙腈作为流动相B,进行梯度洗脱,柱温为40℃,检测波长为210 nm和293 nm,流量为1.0 mL/min,进样体积为20μL。结果表明,9种杂质的质量浓度在0.013~2.107μg/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.9990,定量限为0.013~0.079 mg/kg。按加校正因子的自身对照法计算,样品的平均加标回收率为95.0%~103.0%,测定结果的相对标准偏差为0.5%~2.2%(n=9),各杂质分离度良好。该方法专属性强、精密度好、准确度高,可作为盐酸达泊西汀中工艺杂质和降解杂质的控制和质量评价方法。

An high performance liquid chromatography method for the detection of nine impurities contents in dapoxetine hydrochloride was established.The chromatographic column was Phenomenex Gemini C_(18),mobile phase A was a 0.04%(volume fraction)diethylamine with 10 mmol/L sodium bicarbonate in water,and mobile phase B was acetonitrile;the column temperature was 40℃;the detection wavelength was 210 nm and 293 nm;the flow rate was 1.0 mL/min;the injection volume was 20μL.The results showed that the mass concentration of 9 impurities had a good linear relationship with the chromatographic peak area in the range of 0.013-2.107μg/mL,the correlation coefficients were all greater than 0.9990,and the limits of quantitation were 0.013-0.079 mg/kg.According to the self-control method with correction factor,the average recoveries of the sample were 95.0%-103.0%,the relative standard deviations of the determination results were 0.5%-2.2%(n=9),and the impurities were well separated.The method has strong specificity,good repeatability,accurate and reliable results,which can be used for impurity control and quality assessment of dapoxetine hydrochloride.