HPLC法测定曲安奈德益康唑乳膏中的有关物质

目的:建立测定曲安奈德益康唑乳膏中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Venusil ASB C18,流动相A、B分别为甲醇-0.077%醋酸铵溶液(20∶80,V/V,磷酸调节pH至4.5)和甲醇-乙腈(40∶60,V/V),梯度洗脱,流速为1.0 ml/min,检测波长为225 nm,柱温为35Ⅴ,进样量为10μl。结果:曲安西龙、硝酸咪康唑以及3个单个未知杂质均能与曲安奈德益康唑乳膏中的主成分完全分离;曲安西龙、硝酸咪康唑的检测质量浓度分别在1.071⁸.568、1.0398.568、1.039⁸.312μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.999 8、0.999 6),检测限分别为5.15、7.31 ng,定量限分别为15.69、21.97 ng。结论:该方法灵敏、准确、专属性强、重复性好,可用于曲安奈德益康唑乳膏的质量控制。

Determination of Related Substance in Triamcinolone Acetonide and Econazole Nitrate Cream by HPLC

OBJECTIVE： To establish a method for the content determination of related substances in Triamcinolone acetonide and econazole nitrate cream. METHODS： HPLC method was adopted. The determination was performed on Venusil ASB C18 column with mobile phase A composed of methanol-0.077% ammonium acetate （20： 80, VIV, pH value adjusted to 4.5 using phosphoric acid） and methanol-acetonitrile （40： 60, V/V） as mobile phase B （gradient elution） at the flow rate of 1.0 ml/min, The detection wavelength was 225 nm, and the column temperature was 35 ℃. The sample size was 1 0 μl. RESULTS： Fluoxyprednisolone and miconazole nitrate and unknown impurity were completely separated from main components of Triamcinolone acetonide and econazole nitrate cream. The linear range of 2 kinds of known impurities were 1.071-8.568 μg/ml（r=0.999 8） and 1.039-8.312 μg/ml （r=0.999 6）. The detection limits were 5.15 ng and 7.31 ng , and quantitative limits were 15.69 ng and 21.97 ng. CONCLUSIONS： The method is sensitive, accurate specific and reproducible, which can be used for the quality control of related substance in Triamcinolone acetonide and econazole nitrate cream.