预饱和-中空纤维离心超滤-高效液相色谱法测定吡罗昔康凝胶含量

Determine the content of piroxicam gel by presaturated-hollow fiber centrifugal ultrafiltration-HPLC

目的:建立中空纤维离心超滤-HPLC法用于吡罗昔康凝胶剂中吡罗昔康的含量测定。方法:基于中空纤维可截留大分子的特性,采用中空纤维离心超滤法对吡罗昔康凝胶样品进行分离,有效滤除大分子辅料,并采用自身预饱和法解决吸附问题,所得滤液直接进行色谱分析。采用C_(18)色谱柱(250 mm×4.60 mm, 5μm),流动相为甲醇-0.5%冰醋酸溶液(60∶40),流速为1.0 mL·min^(-1),检测波长为338 nm。结果:吡罗昔康在1.03～51.25μg·mL^(-1)范围内线性关系良好(r=0.999 7),回收率在97.0%～102.9%范围内,RSD%≦1.2。结论:该方法简单、快速、准确度高,可用于吡罗昔康凝胶的含量测定。

OBJECTIVE To establish a hollow fiber centrifugal ultrafiltration-HPLC method for the determination of piroxicam in proxicam gel.METHODS Based on the property that hollow fiber can intercept large molecules,the centrifuge ultrafiltration of hollow fiber was used to separate the samples of proxicam gel.It could effectively filtrate large molecular excipients and solved the adsorption problem by using self-presaturation method for the first time.The filtrate was analyzed directly by chromatography.The chromatograhphic colum:C18(250 mm×4.60 mm,5μm);The mobile phase system was methanol-0.5%glacial acetic acid solution(60∶40),flow rate was 1.0 mL·min-1,detection wave length was 338 nm.RESULTS A good linear relation was obtained in the range of 1.03-51.25μg·mL-1(r=0.999 7).The recoveries were in the range of 97.0%-102.9%,with RSD%≦1.2.CONCLUSION The method used in this study is accurate,rapid and simple,and can be used for the determination of piroxicam gel.