HPLC法测定马来酸曲美布汀的有关物质

Determination of related substances to trimebutine maleate by HPLC

目的:建立HPLC法测定马来酸曲美布汀的有关物质。方法:采用资生堂CAPCELL PAK C18色谱柱(250 mm×4.6 mm,5μm),以缓冲液[取高氯酸0.43 ml,加水950 ml,混匀后用醋酸铵试液调节pH值至(3.75±0.05),用水稀释至1000 ml,加戊烷磺酸钠1.54 g振摇使溶解]-乙腈(65∶35)为流动相,流速为1.0 ml/min,柱温为40℃,检测波长为268 nm。结果:马来酸曲美布汀在0.5～20.0μg/ml的浓度范围内与其峰面积呈良好线性关系(r=0.9999),3,4,5-三甲氧基苯甲酸在0.5～20.0μg/ml的浓度范围内与其峰面积呈良好线性关系(r=0.9999)。马来酸曲美布汀及3,4,5-三甲氧基苯甲酸的最低检出限均为1 ng。已知杂质的平均回收率为98.6%,RSD为1.2%(n=6)。结论:该方法简便准确,重复性好,可用于有关物质的测定。

Objective： To establish an RP - HPLC method for determination of the related substances to trimebutine maleate. Method： The chromatographic separation was achieved on a CAPCELL PAK C18 （250 mm × 4.6 ram,5μm） column with the mobile phase of methanol buffer solution -acetonitrile （65： 35 ）. The flow rate was 1.0 ml/min with column temperature at 40 ℃. The detection wavelength was 268 nm. Results ： A satisfying linear relationship existed between the concentrations of trimebutine, or the known impurity, and the peak areas when the concentration varied from 0.5 μg/ml to 20 μg/ml （ r = 0.9999 ）. The average recoveries were 98.6% and RSD was 1.2% （ n = 6 ） for the known impurity. Conclusion ： The method is simple, accurate and reproducible for determination of the related substances to trimebutine maleate. KEY WORDS trimebutine maleate, HPLC, related substances