马来酸氟吡汀含量测定方法的研究

Study on the determination methods for Flupirtine maleate

目的研究马来酸氟吡汀的含量测定方法。方法建立了非水溶液滴定法和HPLC法测定马来酸氟吡汀的含量。非水溶液滴定法以冰醋酸-醋酐(1∶1)作为溶剂,用0.1 mol.L-1高氯酸滴定液滴定,结晶紫为指示剂;HPLC法采用Gemini C18色谱柱(150 mm×4.6 mm,5μm),流动相为乙腈-水-冰醋酸(34∶66∶1),内含0.05%的庚烷磺酸钠,检测波长245 nm。结果非水溶液滴定法∶马来酸氟吡汀0.2～0.4 g与消耗滴定液体积的线性关系良好(r=0.9999),RSD=0.1%(n=6);HPLC法∶马来酸氟吡汀1.0～5.0μg与峰面积呈良好的线性关系(r=0.9995),RSD=0.2%(n=6);样品测定的结果与非水滴定法比较无显著性差异。结论所建的两种测定方法准确、简便、可靠,可用于马来酸氟吡汀的质量控制。

OBJECTIVE To establish two methods for the determination of Flupirtine maleate.METHODS A non-aqueous titration method and a HPLC method were established.In the nonaqueous titration method,glacial acetic acid-acetic anhydride（1：1）was used as solvent,and 0.5% viola crystalline was used as indicator.Flupirtine maleate was titrated by 0.1 mol·L-1 perch-loric acid solution.The ion-pair RP-HPLC was performed on a Gemini C18 column（150 mm×4.6 mm,5 μm）,and the mobile phase was CH3CN-H2O-CH3COOH（34：66：1） containing 0.05% sodium heptanesulfonate.The detection wavelength was set at 245 nm.RESULTS Non-aqueous titration：the linear range was within 0.2-0.4 g（r=0.9999）,RSD was 0.2%（n=6）.The ion-pair RP-HPLC method：good linearity was obtained in the range of 1.0-5.0 μg（r=0.9995）,repeatability（RSD）was 0.2%（n=6）.There was no significant difference in accuracy between the results of HPLC method and the nonaqueous titration method.CONCLUSION The results indicated that the two methods were simple,accurate and reproducible.