Comprehensive stability‐indicating high‐performance liquid chromatography coupled with diode array detection method for simultaneous determination of amprolium hydrochloride and ethopabate in powder dosage form for veterinary use

This research deals with the development of a stability‐indicating high‐performance liquid chromatography method for simultaneous determination of amprolium hydrochloride and ethopabate. To the best of our knowledge, no comprehensive stability‐indicating method has been reported for analysis of this mixture. Separation was achieved using Kromasil cyano column with gradient elution of the mobile phase composed of sodium hexane sulfonate solution and methanol. Quantification was based on measuring peak areas at 266 nm. Amprolium and ethopabate peaks eluted at retention times 10.42 and 18.53 min, respectively. The proposed procedure was validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Linearity ranges for amprolium and ethopabate were 1.5–240 and 1–160 μg/mL, respectively. Analytes were subjected to stress conditions of hydrolysis, oxidation and thermal degradation. The proposed method enabled resolution of drugs from their forced‐degradation products and amprolium related substance (2‐picoline). Moreover, specificity was verified by resolution of the analytes from about 22 drugs used in antimicrobial veterinary products. The validated method was successfully applied to assay of the combined veterinary powder dosage form, additionally it was implemented in the accelerated stability study of the dosage form when stored for six months at 40°C and 75% relative humidity.     

氧化还原引发制备乙氧酰胺苯甲酯分子印迹微球及其表征

以乙氧酰胺苯甲酯为模板分子,甲基丙烯酸为功能单体,季戊四醇三丙烯酸酯为交联剂,在过氧化苯甲酰和N,N-二甲基苯胺的引发作用下,制备了乙氧酰胺苯甲酯的分子印迹聚合物微球。优化的致孔溶剂为乙腈,模板、单体和交联剂的摩尔比为1∶6∶20。采用高效液相色谱法测定模板分子及其结构类似物的浓度,结合静态平衡吸附实验、吸附动力学实验和选择性评价,对聚合物的吸附性能进行了研究,所得微球的静态吸附量为15.0μmol·g-1,印迹因子为4.93。采用扫描电子显微镜、红外光谱仪和差示扫描量热仪表征聚合物的理化特性,结果表明,微球的形貌规则,印迹效应显著,热稳定性较好。本研究所采用的氧化还原引发方法具有制备简便、成本低以及特异性好等优点,为分子印迹聚合物的引发制备提供了新思路。