HPLC测定复方水杨酸制剂中醋酸曲安奈德和水杨酸的含量

目的:建立用高效液相色谱法(high-performance liquid chromatography,HPLC)同时测定复方水杨酸制剂中水杨酸和醋 酸曲安奈德含量的方法,并分别以峰高和峰面积计算其含量,比较两者的差异,选择最优的计算方法.方法:采用HPLC,以炔诺酮为内标,选用Hipersil C8色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇-乙腈0.075 mol/L磷酸二氢钾溶液-1.0 mol/L枸橼酸溶液(15∶15∶26∶4),流速1.0 mL/min.检测波长254 nm,柱温30℃.进样复方制剂10 μL,分别记录水杨酸和醋酸曲安奈德的峰高与峰面积.结果:水杨酸和醋酸曲安奈德的峰高线性范围分别为:60～400 μg/mL(r峰高=0.9996)和15.00～35.00 μg/mL(r峰高=0.9999),日内精密度RSD为2.1869％和2.9389％,重复性RSD分别为0.9093％和0.4202％,稳定性RSD为1.6307％和0.5460％,平均回收率(n=9)RSD分别为1.12％和0.51％.用峰高计算回归方程曲线的相关系数较用面积计算高.结论:本试验确定了用峰高计算目标物的含量,方法简便快捷,且结果准确,可用于复方水杨酸制剂中水杨酸和醋酸曲安奈德的含量测定.

Simultaneous determination of salicylic acid and triamcinolone acetonide acetate in compound salicylic acid preparations by HPLC

Objective：To establish a PHLC method to simultaneously determine salicylic acid and triamcinolone acetonide acetate in compound salicylic acid preparations and to calculate the content by peaks height and peak areas for comparing the difference between them and selecting optimal calculation method.Methods：The HPLC method was adopted with norethindrone as the internal standard.The chromatographic column was the Hipersil C8 column（4.6 mm×250 mm,5 μm） with the mobile phase composed of methanol-acetonitrile-0.075 mol/L potassium dihydrogen phosphate-1.0 mol/L citric acid（15：15：26：4）.The detection wave length was 254 nm,the flow rate was 1.0 mL/min and the column temperature was 30 ℃.The sample injection was 10 μl.The peak heights and peak areas of salicylic acid and triamcinolone acetonide acetate were recorded respectively.Results：The linear ranges of peak height were 60~400 μg/mL（rpeak=0.999 6） for salicylic acid and 15.00~35.00 μg/mL（rpeak=0.999 9） for triamcinolone acetonide acetate,respectively.The within-day precision of salicylic acid and triamcinolone acetonide acetate were 2.186 9% and 2.938 9%,respectively.The average recovery rates（n=9） of salicylic acid and triamcinolone acetonide acetate were 1.12% and 0.51% respectively.Their stabilities were 1.630 7% and 0.5460 % and the repeatabilities were 0.909 3% and 0.4202%,respectively.The related coefficient of regression equation calculated by peak height was higher than that by peak area.Conclusion：This experiment confirms that the method using peak height to calculate the target′s content is simple and fast with accurate results,which can be used to determine the content of salicylic acid and triamcinolone acetonide acetate in the preparations with salicylic acid and triamcinolone acetonide acetate as the main active constituents.