高效液相色谱法直接测定复方倍氯米松橡胶膏中微量丙酸倍氯米松的含量

Determination of beclometasone dipropionate in compound beclometasone adhesive plaster by directly HPLC microanalysis

目的 建立了复方倍氯米松橡胶膏剂中丙酸倍氯米松的含量测定方法。方法 RP HPLC外标法 ,Shim packCLC ODSC18柱 ,6 .0mm× 15 0mm ,5 μ ;流动相为 0 .0 5mol·L-1磷酸二氢钠溶液 (用 80 %磷酸溶液调节 pH值至 2 .5 ) 甲醇 ( 2 0∶80 ) ;柱温4 0℃ ;检测波长 2 4 0nm。结果 当进样体积为 5 0 μL时 ,在 0 .10 9～ 4 .34μg·mL-1的浓度范围内 ,线性关系良好 ;其他相似物质峰对丙酸倍氯米松的测定没有任何干扰 ;方法的重复性、回收率、溶液的稳定性均令人满意。结论 本法灵敏、方便、准确 ,可作为复方倍氯米松橡胶膏剂中丙酸倍氯米松的含量测定的首选方法。

OBJECTIVE To develop a reversed phase HPLC method to determine the content of beclometasone dipropionate in compound beclometasone adhesive plaster. METHOD The analysis was carried out on a column named Shim pack CLC ODS (6.0mm×150mm, 5μm) with a mobile phase of 0.05mol·L -1 phosphate monobasic sodium solution (adjusted the pH value to 2.5 by 80% phosphate solution) methanol (20∶80), The detection wavelength was 240nm and the column temperature was set at 40℃.RESULTS The linear range was 0.109 ～ 4.34μg·mL -1 ( r =0.999994, n =10) when the injection volume was 50μL; the average recovery of beclometasone dipropionate was 101.6% ( RSD =3.7%, n =9); The reproducibilities of the method ( RSD ) was 1.2% ( n =6). The specificity of the method was very well. CONCLUSION This method is a rapid, simple and accurate procedure, which is suitable for assay of beclometasone dipropionate in compound beclometasone adhesive plaster.