复方对乙酰氨基酚片溶出度方法研究及溶出行为评价

Study of Dissolution Determination for Compound Paracetamol Tablets and Evaluation of Dissolution Behavior

目的建立复方对乙酰氨基酚片的溶出度方法,并对不同样品进行溶出曲线评价。方法采用HPLC,使用Sepax Amethyst C18-H(4.6 mm×150 mm,5μm)色谱柱,以磷酸盐缓冲液(取0.01 mol·L-1磷酸二氢钾溶液,用磷酸调节pH值至2.6±0.1)-甲醇(70︰30)为流动相;流速:1.0 m L·min-1;柱温:35℃;检测波长:波长切换,0~12.5 min,波长为275 nm,12.5~16 min,波长为303 nm;溶出度试验采用桨法,以900 m L盐酸溶液(稀盐酸24 m L,加水至1 000 m L)为溶出介质,转速为50 r·min-1。结果阿司匹林和水杨酸分别在12.54~501.60μg·m L-1(r=1.000 0)和0.99~39.76μg·m L-1(r=0.999 9)线性关系良好;低、中、高3种浓度的平均回收率分别为98.9%,96.7%,97.7%,RSD分别为0.46%,0.65%,0.31%;溶出度方法较好地反映了不同厂家复方对乙酰氨基酚片溶出行为的差异。结论建立的HPLC溶出度测定方法简单方便,具有较好的专属性、精密度和准确度,溶出方法能较好地体现不同厂家样品间的差异。

OBJECTIVE To establish a method to determine the dissolution of Compound Paracetamol tablets and evaluate the dissolution curves of different samples. METHODS The HPLC was used, and the separation was performed on a Sepax Amethyst C18-H（4.6 mm×150 mm, 5 μm） column with the mobile phase consisted of phosphate buffer（0.01 mol·L-1 potassium dihydrogen phosphate solution adjust pH to 2.6±0.1 by phosphoric acid）-methanol（70︰30） at a flow rate of 1.0 m L·min-1. The column temperature was 35 ℃. The detection wavelength was 275 nm at 0-12.5 min and switched to 303 nm at 12.5-16 min. The paddle method was used for the dissolution test with hydrochloric acid solution（dissolve 24 m L dilute hydrochloric acid in water to 1 000 m L） as the medium and the rotation rate was set at 50 r·min-1. RESULTS Aspirin and salicylic acid revealed good linearities within the range of 12.54-501.60 μg·m L-1（r=1.000 0） and 0.99-39.76 μg·m L-1（r=0.999 9）, respectively. The average recoveries were 98.9%, 96.7%, 97.7% at low, intermediate and high concentration, with the RSD of 0.46%, 0.65%, 0.31%, respectively. The dissolution method was suitable, which showed differences of dissolutions among products of different manufacturers. CONCLUSION The established HPLC method is simple, which shows good specificity, precision and accuracy. The dissolution method can reflect differences among products of different manufacturers.