曲安奈德益康唑乳膏含量和有关物质检测方法的建立

Determination of content and related substances in triamcinolone acetonide and econazole nitrate cream

目的:建立反相高效液相色谱法测定曲安奈德益康唑乳膏的有关物质和含量。方法:采用Agilent Infinity C_(18)柱(4.6 mm×150 mm,4μm);以乙酸盐缓冲液(取0.585 g乙酸铵,加500 mL水溶解,再加入1%乙酸溶液9 mL,加水至1000 mL)-乙腈(95∶5)为流动相A,以异丙醇为流动相B,以乙腈为流动相C,梯度洗脱;流速为0.42 mL·min^(-1);柱温为35℃;检测波长为225 nm(硝酸益康唑)和240 nm(曲安奈德),进样量:10μL。结果:有关物质曲安奈德的检测限为0.12μg·mL^(-1),硝酸益康唑的检测限为0.40μg·mL^(-1);含量测定线性范围曲安奈德为4.78~95.6μg·mL^(-1),r=1.0000硝酸益康唑为51.8~1036μg·mL^(-1),r=0.9995;精密度、稳定性、重复性试验的RSD≤0.8%;曲安奈德的平均回收率为101.5%,RSD为1.3%(n=9),硝酸益康唑的平均回收率为99.6%,RSD为1.4%(n=9)。曲安奈德含量分布于90.8%~109.6%之间,不呈正态分布(P<0.05),硝酸益康唑含量分布于95.0%~107.2%之间,呈正态分布(P>0.05)。结论:本法更加简便、准确,专属性好,可用于测定曲安奈德益康唑乳膏的含量和有关物质。

Objective:To establish a RP-HPLC method for the determination of related substances and content in triamcinolone acetonide and econazole nitrate cream.Methods:The assay was performed on an Agilent Infinity C_(18) column(4.6 mm×150 mm,4μm)with gradient elution of acetate buffer(0.585 g of ammonium acetate was dissolved in 500 mL of water,then 9 mL of 1% acetic acid solution was added,and the total volume was diluted to 1000 mL using water)-acetonitrile(95∶5)as mobile phase A,isopropanol as mobile phase B,and acetonitrile as mobile phase C.delivered at a flow rate of 0.42 mL·min^(-1).Triamcinolone acetonide and econazole nitrate were detected at wavelengths of 225 nm and 224 nm,respectively.The column temperature was 35℃,and the injection volume was 10μL.Results:The limit of detection for triamcinolone acetonide was 0.12μg·mL^(-1),and the limit of detection for econazole nitrate was 0.40μg·mL^(-1.)The linear range of triamcinolone acetonide was from 4.78 to 95.6μg·mL^(-1)(r=1.0000),and the linear range of econazole nitrate was from 51.8 to 1036μg·mL^(-1)(r=0.9995).The assay precision,stability and repeatability of triamcinolone acetonide and econazole nitrate were≤0.8%.The average recovery of triamcinolone acetonide was 101.5%,and the RSD was 1.3%(n=9).The average recovery of econazole nitrate was 99.6%,and the RSD was 1.4%(n=9).The content of triamcinolone acetonide in cream was from 90.8% to 109.6%,which did not present normal distribution(P<0.05),and the content of econazole nitrate was from 95.0% to 107.2%,which presented normal distribution(P>0.05).Conclusion:The method is simple,accurate and specific,and can be used to determine the content and related substances in triamcinolone acetonide and econazole nitrate cream.