Tsou Tai-Li, Huang Yu-Chuan, Lee Chiu-Wey, Lee An-Rong, Wang Hsian-Jenn, Chen Su-Hwei
Graduate Institute of Pharmaceutical Sciences, College of Pharmacy, Kaohsiung Medical University, Kaohsiung, Taiwan, ROC.
J Sep Sci. 2007 Oct;30(15):2407-13. doi: 10.1002/jssc.200600529.
An accurate and reproducible method for the simultaneous determination of ampicillin (AMP), sulbactam (SUL), and cefoperazone (CFP) in pharmaceutical formulations by using HPLC with beta-CD stationary phase was developed. It involved the use of the added tetraethylammonium acetate (TEAA) reagent, pH, and methanol as the significant parameters to find the optimum separation condition. A high resolution and selectivity of analytes was obtained by running the mobile phase in methanol-5 mM TEAA buffer = 35:65 (v/v, pH 4.5) at 280 nm. The mean recoveries ranged from 96.6 to 103.3% for AMP in the synthetic mixture, 97.6 to 103.0% for SUL, and 97.0 to 104.0% for CFP. The low LOD (<1.8 microg/mL) and low CV (<0.9%) assured that this method was sensitive and reproducible. The assay of analytes in commercial products exhibited that it was convenient and reproducible for routine analyses of these components in sterilized H(2)O, saline, or 5% dextrose injection solutions.
开发了一种使用含β-环糊精固定相的高效液相色谱法同时测定药物制剂中氨苄西林(AMP)、舒巴坦(SUL)和头孢哌酮(CFP)的准确且可重现的方法。该方法涉及使用添加的四乙基醋酸铵(TEAA)试剂、pH值和甲醇作为重要参数来寻找最佳分离条件。通过在280nm波长下以甲醇 - 5mM TEAA缓冲液 = 35:65(v/v,pH 4.5)作为流动相运行,获得了高分辨率和高选择性的分析物分离效果。在合成混合物中,AMP的平均回收率为96.6%至103.3%,SUL为97.6%至103.0%,CFP为97.0%至104.0%。低检测限(<1.8μg/mL)和低变异系数(<0.9%)确保了该方法灵敏且可重现。对市售产品中分析物的测定表明,该方法对于在灭菌水、生理盐水或5%葡萄糖注射液中对这些成分进行常规分析既方便又可重现。