摘要
目的建立测定马来酸曲美布汀缓释片中杂质3,4,5-三甲氧基苯甲酸含量的高效液相色谱法。方法用十八烷基硅烷键合硅胶为填充剂,以高氯酸缓冲液(取高氯酸0.85 mL,加水至1 000 mL,用0.1%醋酸胺溶液约1 000 mL调pH至3.75±0.05,取此溶液1 000 mL,加戊烷磺酸钠1.54 g,振摇使溶解)-乙腈(65∶35)为流动相,检测波长为267 nm,进样量10μL。结果 3批样品中3,4,5-三甲氧基苯甲酸杂质的含量均未超过0.1%,其质量浓度在0.099～19.8μg/mL范围内与峰面积线性关系良好,平均回收率为99.73%,RSD为0.23%。结论高效液相色谱法测定马来酸曲美布汀缓释片中杂质3,4,5-三甲氧基苯甲酸的灵敏度高,线性范围宽,回收率高。
Objective To establish a scientific and rational HPLC method for the quantitative determination of impurity 3,4,5-trimethoxy benzoic acid in trimebutine maleate sustained release tablets.Methods The high performance liquid chromatography（HPLC） was used with octadecyl silane bonded silica as the filler.Perchlorate buffer（taking perchloric acid 0.85 mL,adding water to 1 000 mL,adjusting to pH 3.75±0.05 with 0.1%ammonium acetate solution 1 000 mL,taking the solution 1 000 mL,adding pentanesulfonic acid sodium 1.54 g and shaking the solution）-acetonitrile（65 ∶35）was the mobile phase.The detection wavelength was 267 nm.The injection volume：10 μL.Results The content of impurity 3,4,5-trimethoxy benzoic acid in three batches of sample of trimebutine maleate sustained release tablets produced by our corporation,sustained-release tablets sample produced by korea and trimebutine maleate tablets produced by Japan did not exceed 0.1%.The good linearity relation with the peak area was in the concentration range of 0.099-19.8 μg/mL.The average recovery rate was 99.73%,RSD 0.23%.Conclusion The HPLC determination of impurity 3,4,5-trimethoxy benzoic acid in trimebutine maleate sustained release tablets has high sensitivity,wide linear range and high recovery rate.
出处
《中国药业》
CAS
2011年第12期37-38,共2页
China Pharmaceuticals
