HPLC法同时测定克霉唑片中多种有关物质

Simultaneous Determination of a Variety of Related Substances in Clotrimazole Tablets by HPLC

目的:建立HPLC法同时检测克霉唑片中多种有关物质。方法:采用Inert SustainC18色谱柱(4.6 mm×150 mm,5μm),以磷酸二氢钾-四丁基硫酸氢铵溶液为流动相A、乙腈为流动相B,按梯度进行洗脱,流速为1.0 m L·min^(-1),检测波长为210 nm。结果:克霉唑与有关物质A、B、E、F在该色谱条件下均完全分离,在0.08~3.03μg·m L^(-1)浓度范围内克霉唑与峰面积线性关系良好(r=0.9998);有关物质A在0.04~3.42μg·m L^(-1)范围内与峰面积线性关系良好(r=0.9999),平均回收率为99.43%,RSD=1.72%(n=9);有关物质E在0.42~3.58μg·m L^(-1)范围内与峰面积线性关系良好(r=0.9997),平均回收率为100.10%,RSD=1.17%(n=9)。结论:HPLC方法准确、简便、快速,适用于同时测定克霉唑片中多种有关物质。

Objective： To develop an HPLC method for simultaneous determining a variety of relatedsubstances in clotrimazole tablets. Methods： The separation was carried out on an InertSustain- Ctg （4.6mm × 150 mm, 5 μm ） column with a mobile phase of potassium dihydrogen phosphate -tetrabutylammoniumhydrogen sulfate solvent （A） and acetonitrile （B） in gradient, at a flow rate of 1.0 m L-min-1. The detectionwave was set at 210 nm. Results： Clotrimazole was well separated with related substances A , B , E and Funder the above chromatographic conditions. The calibration curve was linear （r=0.9998） within the range of0.08-3.03μg·mL-1 for clotrimazole. The calibration curve was linear （r=0.9999） within the range of 0.043.42μg·mL-1 for related substance A , the average recovery rate was 99.43% with RSD at 1.72% （n =9）.The calibration curve was linear （r=0.9997） within the range of 0.42-3.58μg·mL-1 for related substance E ,the average recovery rate was 100.10% with RSD at 1.17% （n=9）. Conclusion： This method can be usedto simultaneously separate and determine clotrimazole and a variety of related substances in clotrimazoletablets. It is accurate, simple and fast.