口腔速溶膜剂中他达拉非的反相高效液相色谱测定.docVIP

口腔速溶膜剂中他达拉非的反相高效液相色谱测定 　　[摘要]目的 建立反相高效液相色谱（RP-HPLC）分析方法测定口腔速溶膜剂中他达拉非（TDF）的含量。方法 用溶剂浇铸法制备每2 cm×3 cm理论含药量为20 mg的他达拉非口腔速溶膜剂。采用色谱柱：Cosmosil 5 C18-MS-Ⅱ（4.6×250 mm，5 μm），以乙腈-0.1%三氟乙酸水溶液（44：56）为流动相，检测波长：285 nm，流速：1.0 ml/min，柱温40℃，进样量20 μl，测定他达拉非口腔速溶膜剂中的药物含量。结果 他达拉非在0.8～40 μg/ml的浓度范围内线性关系良好（R2=0.9998）；日内精密度相对标准偏差RSD为0.002%～0.963%，日间精密度RSD为1.22%～1.83%，平均加样回收率为99.22%，定量限为0.902 ng，检测限为0.271 ng。他达拉非口腔速溶膜剂中的药物含量为96.43%。结论 建立的他达拉非RP-HPLC分析方法专属性强，精密度、回收率高，稳定性良好，适用于他达拉非口腔速溶膜剂中药物的含量测定。 　　[关键词]反相高效液相色谱；他达拉非；口腔速溶膜剂；聚乙烯醇；含量测定 　　[中图分类号] R698.1 [文献标识码] A [文章编号] 1674-4721（2017）12（a）-0008-04 　　[Abstract]Objective To establish ananalytical method of reverse phase high performance liquid chromatography （RP-HPLC） to analyze the Tadalafil （TDF） content in Orodispersible Films （ODFs）.Methods TDF-loaded ODFs with a loading capacity up to 20 mg TDF in an area of 2 cm×3 cm were prepared using a solvent casting method.The chromatographic column was Cosmosil 5 C18-MS-Ⅱ （4.6×250 mm，5 μm） and mobile phase of acetonitrile-0.1% Trifluoroacetic Acid （44：56） were used，the detection wavelength was set at 285 nm，the flow rate was 1.0 ml/min，the column temperature was maintained at 40℃ and the injection volume was 20 μl.The drug content in TDF-loaded ODFs was analyzed.Results The TDF concentration range with good linear relationship was 0.8-40 μg/ml，R2=0.9998.The RSD of intra-day was in the range of 0.002%-0.968%，RSD of inter-day was in the range of 1.22%-1.83%.Mean result of recovery rate was 99.22%.The limit of quantitation （LOQ） was 0.902 ng and the limit of detection （LOD） was 0.271 ng.The drug content of TDF-loaded ODFs was 96.43%.Conclusion The RP-HPLC method of TDF showed high specific，good precision，recovery rate and stability.This method is suitable for thedetermination of drug content of TDF-loaded ODFs. 　　[Key words]RP-HPLC；Tadalafil；Orodispersible films；Polyvinyl alcohol；Content determination 　　口腔速溶膜剂（Orodispersible Films，ODFs）是一种口服速释膜剂，供口含、舌下给药和口腔内局部贴敷，经唾液润湿并黏附在给药部位，膜溶解或分散同时释放药物的一种膜制剂[1-2