高效液相色谱法测定盐酸异丙嗪咖啡因片的含量及溶出度  

Determination and dissolution of promethazine hydrochloride and caffeine tablets by HPLC

作　　者：刘圆圆[1] 孙建绪[1] 李迎[1] 张慧[1] 郭飞[1] 郑爱萍[1] 

机构地区：[1]抗毒药物与毒理学国家重点实验室,军事医学科学院毒物药物研究所,北京00850

出　　处：《国际药学研究杂志》2016年第2期392-397,共6页Journal of International Pharmaceutical Research

摘　　要：目的建立测定盐酸异丙嗪咖啡因片的含量及溶出度的高效液相色谱法。方法色谱柱：Agilent TC C18柱（250 mm×4.6 mm,5μm）;流动相：甲醇-三乙胺水溶液（浓度为3‰,磷酸调至p H2.3）=（50∶50）;流速：1.0 ml/min;检测波长分别为250和272 nm;柱温：30℃;进样量20μl（溶出度测定时进样量为10μl）。溶出条件采用桨法,温度为37℃,分别以900 ml p H1.2盐酸、p H 4.5醋酸缓冲液、p H 6.8磷酸缓冲液及水为溶出介质,以50、75 r/min作为转速进行溶出条件的筛选。结果该HPLC检测方法专属性良好;盐酸异丙嗪、咖啡因分别在0.5~100μg/ml和4.0~400μg/ml范围内线性关系良好,线性回归方程分别为Y=96.21X-7.303（r=1）、Y=51.33X＋68.88（r=0.9999）;盐酸异丙嗪检测限为15 ng/ml,定量限为40 ng/ml;咖啡因检测限为2 ng/ml,定量限为10 ng/ml。平均回收率分别为盐酸异丙嗪（100.04±1.39）%（n=9）,咖啡因（99.42±1.07）%（n=9）;供试溶液在12 h保持稳定。确立了以900 ml p H 1.2盐酸为溶出介质,桨法转速为50 r/min的溶出方法,溶出时间30 min。制剂在4种溶出介质中溶出度均在15 min内达85%以上,其溶出不受体液p H影响。结论所选溶出条件适用于盐酸异丙嗪咖啡因片的溶出测定。所建含量及溶出度检测方法简便、快速、灵敏,精密度高,重现性好,结果准确,适合同时对盐酸异丙嗪及咖啡因进行含量及溶出度分析。Objective To develop a high performance liquid chromatography（HPLC）method for determining the content and dissolution of promethazine hydrochloride and caffeine tablets. Methods Agilent TC C18column（250 mm×4.6 mm,5 μm）was used. The mobile phase was methanol-3‰ triethylamine solution（adjusted to p H2.3 with phosphoric acid）（50∶50,v/v）with a flow rate1.0 ml/min,and the detection wavelengths were set at 250 nm and 272 nm,respectively. The column temperature was 30℃ and the injection volume was 20 μl（injection volume of 10 μl for dissolution）. Dissolution of tablets was determined by paddle method and the temperature was 37℃,900 ml p H 1.2 hydrochloric acid solution,acetic acid buffer（p H 4.5）,phosphoric acid buffer（p H 6.8）and water were used as dissolution medie at the rotation speed of 50,75 r/min for selecting dissolution condition. Results The calibration curves were linear within the range of 0.5-100 μg/ml（r=1）for promethazine hydrochloride,and forcaffeine 4-400 μg/ml（r=0.9999）,respectively. The detection limit and quantification limit of promethazine hydrochloride were 15 and 40 ng/ml,and caffeine 2 and 10 ng/ml,respectively. The recoveries of promethazine hydrochloridum and caffeine were（100.04±1.39）%（n=9）and（99.42±1.07）%（n=9）,respectively. And the stability of working solutions was acceptable in 12 h. The method of dissolution tests for the tablet was established with 900 ml p H 1.2 hydrochloric acid solution as dissolution medium,paddle rotation speed of 50 r/min,and dissolution time30 min. Conclusion The method is convenient,fast,sensitive and reproducible,with good precision,specificity and accuracy. So it can be used for simultaneous determination and dissolution of promethazine hydrochloride and caffeine tablet.

关 键 词：高效液相色谱法 盐酸异丙嗪 咖啡因 含量测定 溶出度 

分 类 号：R927.2[医药卫生—药学] O657.72[理学—分析化学]