反相HPLC法测定阿奇霉素软胶囊含量.docVIP

反相HPLC法测定阿奇霉素软胶囊含量 　【摘要】 目的 采用反相高效液相色谱法测定阿奇霉素软胶囊中阿奇霉素的含量。方法 用耐碱性的十八烷基硅烷键合硅胶柱为固定相，以水∶0.01mol/L磷酸氢二钠溶液(用氢氧化钠试液调节pH值至10.3)∶乙腈(16.7∶23.3∶60)为流动相，流速1.5ml/min，柱温40℃，检测波长210nm。结果 阿奇霉素主成分峰与相邻杂质峰分离状况良好；空白辅料植物油不干扰阿奇霉素主成分的分离检测。阿奇霉素在0.2052～1.9207μg/ml的浓度范围内质量与峰面积呈良好的线性关系；在添加了空白油辅料的体系中在0.1995～2.0147μg/ml的浓度范围内质量与峰面积呈良好的线性关系。在添加了空白油辅料的体系中阿奇霉素的最低检测浓度为1.0483～2.0966μg/ml，最低定量浓度为4.1932～10.483μg/ml。准确性试验的平均回收率为101.4%，RSD为0.2%(n=9)；重复性试验的平均含量为98.0%，RSD为1.0%(n=9)。结论 方法专属性强，精密、准确、耐用，可替代抗生素微生物检定法作为阿奇霉素软胶囊的含量测定方法。 【关键词】 高效液相色谱法； 阿奇霉素； 软胶囊； 含量测定 ABSTRACT Objective To established a high performance liquid chromatography method for determination of azithromycin soft capsules. Methods A high pH stability column (Agilent Zorbax Extend-C18, 4.6mm×150mm, 5μm) was used; the mobile phase consisted of water∶0.01mol/L dibasic sodium phosphate buffer solution (the pH value was adjusted to 10.3 by sodium hydroxide T.S.)∶acetonitrile (16.7 ∶23.3∶60); the flow rate was 1.5ml/min; and the UV detection wavelength was at 210nm. Results The good resolution between peaks of azithromycin and of the adjacent purity was obtained. The blank excipient soybean oil did not interfere with the detection of azithromycin. The linear range for azithromycin was 0.2052～1.9207 μg/ml, and the actual linear range for azithromycin in simulated samples spiked with soybean oil excipient was 0.1995～2.0147 μg/ml. The LOD of azithromycin in simulated samples spiked with soybean oil excipient was 1.0483～2.0966 μg/ml, and the LOQ was 4.1932～10.483 μg/ml. The average recovery 101.4% was obtained with a RSD of 0.2%; and the average content 98.0% was obtained from the precision test; and the RSD was 1.0% (n=9). Conclusion The method is specific, precise, accurate and robust. It′s suitable for the content determination of azithromycin soft capsules. KEY WORDS HPLC; Azithromycin; Soft capsules; Content determination 阿奇霉素是一种15元环含氮大环内酯类抗生素，其抗菌谱广，临床疗效显著。阿奇霉素软胶囊是目前国内较为流行的新颖药物剂型，与其他口服制剂相比，具有吸收快、生物利用度高、密封性和防潮性更好，服用方便等优点。对阿奇霉素及制剂的质量分析，日抗基和中国