达那唑胶囊溶出试验测定方法优化  

Optimization of Dissolution Test Method for Danazol Capsules

作　　者：沈景芬 刘文丽 查萍萍 张震 史学礼 王蓉[4] SHEN Jing-fen;LIU Wen-li;ZHA Ping-ping;ZHANG Zhen;SHI Xue-li;WANG Rong(Lu an Food and Drug Inspection Center,Anhui Lu an 237000;Chizhou Food and Drug Inspection Center,Anhui Chizhou 247000;Bozhou Food and Drug Inspection Center,Anhui Bozhou 236800;BozhouVocational Technology,Anhui Bozhou 236800,China)

机构地区：[1]六安市食品药品检验中心,安徽六安237000 [2]池州市食品药品检验中心,安徽池州247000 [3]亳州市食品药品检验中心,安徽亳州236800 [4]亳州职业技术学院,安徽亳州236800

出　　处：《广州化工》2023年第24期74-77,共4页GuangZhou Chemical Industry

摘　　要：建立达那唑胶囊溶出度和含量测定的高效液相色谱法。采用浆法,加用沉降篮,75转速,对达那唑胶囊在不同溶出介质及不同时间点的溶出液取样测定。溶出液采用高效液相色谱法测定其相应溶出量,与药典检测方法相比,有效避免辅料对主成分测定的干扰。新方法选用的溶出介质未使用有机溶剂,更加科学、客观模拟达那唑在体内的释放过程。新方法以C18柱,二极管阵列检测器,流速每分钟1.0 mL;柱温40℃;检测波长:284 nm,采用pH 1.2、4.0、6.8和水来模拟消化道内不同pH值的体液,以便直观反映药物在体内的溶出行为。经方法学验证,达那唑检测HPLC法线性方程为y=20.827x-11.737,检测限为23.03 ng/mL。在达那唑浓度5.118 7~204.748 8μg/mL范围内,线性关系良好(r=0.999 9),达那唑回收率试验结果为99.8%,RSD为0.9%(n=6)。3批样品中达那唑的平均溶出度分别为89.1%、86.0%、88.3%。该方法操作简便、专属性强、准确度高,可应用于检测达那唑胶囊溶出度和含量测定。A high-performance liquid chromatography(HPLC)method was established for the determination of the dissolution rate and content of Danazol capsules.The paddle method was employed with the addition of a sinker basket at 75 rpm to sample and measure the dissolution solution of Danazol capsules at different time points and in various dissolution media.The dissolution solution was analyzed using HPLC to determine its corresponding dissolution amount.Compared to the pharmacopoeia detection method,this method effectively avoided interference from excipients on the determination of the main component.The dissolution media used in the new method did not contain organic solvents,providing a more scientific and objective simulation of Danazol release in vivo.The new method utilized a C 18 column,a diode array detector,with a flow rate of 1.0 mL/min,column temperature set at 40℃,detection wavelength at 284 nm,pH 1.2,4.0,6.8,and water were used as dissolution media to simulate different pH values in the gastrointestinal tract,reflecting the dissolution behavior of the drug in vivo.Through method validation,the linear equation for Danazol detection by HPLC was y=20.827 x-11.737,with a detection limit of 23.03 ng/mL.Within the concentration range of 5.1187~204.7488μg/mL for Danazol,a good linear relationship was observed(r=0.9999).The recovery rate of Danazol was 99.8%,with an RSD of 0.9%(n=6).The average dissolution rates of Danazol in three batches of samples were 89.1%,86.0%,and 88.3%,respectively.This method was simple to operate,had strong specificity,high accuracy,and could be applied to the determination of dissolution rate and content of Danazol capsules.

关 键 词：达那唑胶囊 溶出曲线 溶出限度 含量测定 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]