高效液相色谱法测定德拉昔布咀嚼片的体外溶出度

The Dissolution rate of Deracoxib Chewable Tablets in vitro Determinated by HPLC Method

关键词:  德拉昔布咀嚼片  HPLC法  溶出度检测

Key words:  deracoxib chewable tablets  HPLC  Dissolution determination

摘要:

建立检测德拉昔布咀嚼片溶出度的HPLC检测方法,并采用HPLC法对德拉昔布咀嚼片、Deramaxx咀嚼片的溶出度进行比较。采用桨法50 r/min,溶出介质选择900 mL的0.8%十二烷基硫酸钠,分别于5、10、15、20、30、40、50 min分别采样1 mL,经0.22 μm滤膜滤过后,注入HPLC 进样测定,色谱柱为Wasters C18(4.6×250mm,5μm)；流动相为磷酸盐缓冲液(pH=4.5)∶乙腈(52∶48,v/v)；检测波长252 nm；柱温30℃。结果表明,德拉昔布在浓度5μg/mL ~25 μg/mL范围内呈良好线性相应 (r²=0.999 2)。检测限与定量限分别为0.81 μg/mL与2.57 μg/mL；方法的平均回收率为(101.8±0.91)%；德拉昔布咀嚼片溶出度(87.78±1.91)%与Deramaxx溶出度(88.76±2.05) %均＞85%符合有关规定。结论,所建立的HPLC法简便,准确,专属性强,可用于德拉昔布咀嚼片溶出度的测定。

Abstract:

In order to establish a HPLC method for the determination of the dissolution of deracoxib chewable tablets, the dissolution of deracoxib chewable tablets and Deramaxx chewable tablets were compared by HPLC method. The paddle method was used for 50 r/min, and the dissolution medium was 900 mL 0.8% sodium dodecyl sulfate, 1 mL sample was collected at 5, 10, 15, 20, 30, 40 and 50 min respectively. After filtration with a 0.22 μm filter, the samples were injected into HPLC for determination. The chromatographic column was Wasters C18 (4.6×250 mm,5 μm). The mobile phase was phosphate buffer (pH=4.5) : acetonitrile (52 : 48, V/V).Detection wavelength 252 nm; column temperature 30 ℃. The results showed that deracoxibshowed a good linear response in the range of 5~25 μg/mL (r²=0.999 2). The detection limit and quantitative limit were 0.81 g/mL and 2.57 μg/mL respectively. The average recovery of the method was (101.8±0.91) %. The dissolution of deracoxib chewable tablets (87.78±1.91)% and Deramaxx (88.76±2.05) % were both > 85% in accordance with relevant regulations. Conclusion, the HPLC method was simple, accurate and specific, which can be used for the determination of the dissolution of deracoxib chewable tablets.