【摘要】 目的建立格列喹酮片体外溶出度HPLC检测方法及溶出曲线评价。方法色谱柱为Diamonsil@Plus C18(150 mm×4.6 mm,5μm);流动相为磷酸二氢铵溶液(取磷酸二氢铵1.725 g,加水300 m L溶解后,用磷酸调节p H值至3.5±0.1)-乙腈(3∶5);体积流量1.0 m L/min;检测波长为310 nm,进样量20μL,柱温为35℃,外标法计算。结果空白辅料、溶出介质不干扰测定;格列喹酮在3.13~50.02μg/m L线性关系良好(r=0.999 8,n=7);格列喹酮平均回收率为100.2%(RSD=0.83%,n=9);格列喹酮溶出度溶液在0~24 h内稳定性良好(RSD=0.51%,n=7);弃去10 m L初滤液后滤膜吸附达到饱和。自研品和参比制剂在7种不同p H溶出介质中溶出行为一致。结论经方法学考察,反相高效液相色谱法测定格列喹酮片溶出度专属性强,准确可靠,易于操作。更多还原

【Abstract】 Objective To develop a HPLC method for determinating the dissolution of gliquidone tablet in vitro and evaluate the dissolution profiles. Methods The chromatographic conditions included Colum Diamonsil@Plus C18(150 mm × 4.6 mm,5 μm) and 0.05 mol/L NH4 H2 PO4(adjusted to p H 3.5 ± 0.1 with diluted phosphoric acid)-acetonitrile(3∶5) as the mobile phase, at a flow rate of 1.0 m L/min, detected at 310 nm, injection volum was 20 μL, the column temperature was 35℃, using external standard method to calculate. Results gliquidone could be determined really, blank excipients and dissolution media were uninfluenced for determination. There was a good linearity in the range of 3.13—50.02 μg/m L(r = 0.999 8, n = 7), the average recovery of gliquidone was 100.2%(RSD = 0.83%, n = 9). Through 48 h stability test, the solution of gliquidone was good. The adsorption of the filter membrane reached saturation after abandoning 10 m L initial filtrate. The self-prepared formulation and reference preparation are consistent dissolution behavior in different seven media. Conclusion The established method is high selective, simple and accurate. The method can be used for the determination of dissolution for gliquidone tablets.更多还原