高效液相色谱-电雾式检测器法测定托吡酯片中主要成分及杂质含量

Determination of Main Component and Impurities in Topiramate Tablets by HPLC-CAD

目的建立测定托吡酯片中主要成分及杂质含量的高效液相色谱-电雾式检测器(HPLC-CAD)法。方法色谱柱为Waters Sun Fire C_(18)柱(150 mm×4.6 mm,5μm),流动相为乙腈-0.2%甲酸水溶液(35∶65,V/V),流速为1.0 m L/min,柱温为35℃,雾化温度为35℃,过滤常数为3.6 s,幂率为1.0,采样频率为10 Hz,进样量为10μL。结果托吡酯质量浓度在0.05~1.0 mg/m L范围内与峰面积线性关系良好(r=0.9956),检测限和定量限分别为1μg/m L和3μg/m L;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为100.19%,RSD为1.19%(n=9)。3批样品中托吡酯含量为97.98%~98.96%,杂质总量为0.25%~0.31%。结论所建立的方法操作简便,结果准确可靠,可用于托吡酯片中主要成分及杂质的含量测定。

Objective To establish a high-performance liquid chromatography-charged aerosol detection(HPLC-CAD)method for the determination of main component and impurities in Topiramate Tablets.Methods The chromatographic column was Waters SunFire C_(18) column(150 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.2% formic acid aqueous solution(35∶65,V/V),the flow rate was 1.0 mL/min,the column temperature was 35℃,the atomization temperature was 35℃,the filtration constant was 3.6 s,the power function value was 1.0,the collection frequency was 10 Hz,and the injection volume was 10μL.Results The linear range of topiramate was 0.05-1.0 mg/mL(r=0.9956).The limit of detection and limit of quantification were 1μg/mL and 3μg/mL,respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rate of topiramate was 100.19% with an RSD of 1.19%(n=9).The contents of topiramate and total impurities in three batches of samples were in the range of 97.98% to 98.96% and 0.25% to 0.31% respectively.Conclusion The established method is simple,accurate and reliable,which can be used for the content determination of main component and impurities in Topiramate Tablets.