HPLC法测定盐酸替罗非班原料药的含量及有关物质

发布时间：2018-06-28 10:09

本文选题：盐酸替罗非班 + 高效液相色谱法　；参考：《中国药房》2015年03期

【摘要】：目的:建立测定盐酸替罗非班原料药含量及有关物质的方法。方法:采用高效液相色谱法。色谱柱为CAPCELL PAK C18,流动相A为0.1%醋酸铵溶液(p H 2.30)-乙腈-甲醇(90∶5∶5,V/V/V)、流动相B为0.1%醋酸铵溶液(p H 2.30)-乙腈-甲醇(10∶85∶5,V/V/V)(梯度洗脱),检测波长为227 nm,柱温为35℃,流速为1.0 ml/min,进样量为10μl。结果:盐酸替罗非班与其中间体及其他杂质分离度良好。盐酸替罗非班的质量浓度在20~140μg/ml范围内与其峰面积积分值呈良好的线性关系(r=0.999 9);精密度、稳定性、重复性试验的RSD≤0.35%;平均回收率为100.09%,RSD=0.81%(n=3);其中间体的检测限、定量限分别为0.5、2.0ng。盐酸替罗非班原料药中的单个杂质含量低于0.05%,总杂质含量低于0.2%。结论:该方法简便、准确、专属性强、灵敏度高,适用于盐酸替罗非班原料药的含量及有关物质测定。
[Abstract]:Objective: to establish a method for determining the content and related substances of tirofiban hydrochloride. Method: HPLC column is CAPCELL PAK C18, A is 0.1% ammonium acetate solution (P H 2.30) - acetonitrile - methanol (90: 5: 5, V/V/V), 0.1% ammonium acetate solution (P H 2.30) - acetonitrile - methanol (10: 85: 5, V/V/V) (10: 85: 5, V/V/V) (gradient) Elution), the detection wavelength was 227 nm, the column temperature was 35 C, the flow rate was 1 ml/min, and the sample volume was 10 L.. The separation degree of tironon HCl was good. The mass concentration of tironon class hydrochloride in the range of 20~140 mu g/ml has a good linear relationship with its peak area integral value (r=0.999 9); precision, stability, repetition. The RSD of the sex test was less than 0.35%, the average recovery rate was 100.09%, and RSD=0.81% (n=3). The limit of the detection limit of the inter body, the limit of the quantitative limit of the single impurity in tirohydrochloric acid, was less than 0.05%, and the total impurity content was lower than that of 0.2%.. The method was simple, accurate, strong and sensitive. It was suitable for tirofiban hydrochloride. Determination of the content and related substances.
【作者单位】：解放军空军总医院;
【分类号】：R927.2;O657.72

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