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目的本文建立了一高效液相色谱法用于测定复方水杨酸搽剂中水杨酸的含量,并同时鉴别水杨酸、间苯二酚、苯酚及水杨酸甲酯。方法色谱柱为C18柱(150×4.6mm;5μm),流动相为磷酸三乙胺溶液(含0.4%的磷酸和0.4%的三乙胺,pH2.5)-乙腈(71:29),检测波长为220nm。结果在0.3～0.9mg/ml浓度范围内水杨酸溶液浓度与峰面积呈良好的线性关系,回归方程为C=47.6A+198.6,r=1.000;平均回收率为99.7%(n=6);精密度试验RSD=0.36%、重现性试验RSD=0.11%,水杨酸、间苯二酚、苯酚及水杨酸甲酯各相邻峰之间的分离度均大于3.0。结论本法具有简单、准确,专属性强的特点,既可准确测定水杨酸的含量,又可同时鉴别水杨酸、间苯二酚、苯酚及水杨酸甲酯。
OBJECTIVE To establish a HPLC method for the determination of salicylic acid in compound salicylic acid liniment and to simultaneously identify salicylic acid, resorcinol, phenol and methyl salicylate. Methods The column was C18 column (150 × 4.6 mm; 5 μm). The mobile phase was triethylamine phosphate (containing 0.4% phosphoric acid and 0.4% triethylamine, pH2.5) -acetonitrile (71:29) The wavelength is 220 nm. Results The concentration of salicylic acid showed a good linear relationship with the peak area in the range of 0.3 ~ 0.9mg / ml. The regression equation was C = 47.6A + 198.6, r = 1.000; the average recovery was 99.7% (n = 6) ; RSD of precision test was 0.36%, RSD of reproducibility test was 0.11%. The separation of salicylic acid, resorcinol, phenol and methyl salicylate between adjacent peaks was more than 3.0. Conclusion This method has the characteristics of simple, accurate and specific. It can not only accurately determine the content of salicylic acid, but also simultaneously identify salicylic acid, resorcinol, phenol and methyl salicylate.