Darwish Ibrahim A, Refaat Ibrahim H, Askal Hassan F, Marzouq Mostafa A
Assiut University, Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, Assiut 71526, Egypt.
J AOAC Int. 2006 Mar-Apr;89(2):334-40.
This paper describes the development of a generic spontaneous nonextractive spectrophotometric method for determination of 13 pharmaceutically important 4-quinolone antibiotics. The method was based on the formation of yellow-colored water-soluble ion-pair complexes between 2% (w/v) beta-naphthol reagent and each of the studied drugs in sulfuric acid medium at room temperature. The formed ion-pair chromogens have maximum absorption peaks in the range of 365-391 nm. The concentrations of the reagents and the experimental conditions affecting the reaction were optimized. Under the optimum conditions, linear relationships with good linear coefficients (0.9987-0.9995) were found between the absorbance and concentration of the investigated drugs in the range of 10-350 microg/mL. The assay limits of detection and quantitation were 1-9.9 and 3.4-32.9 microg/mL, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the analysis of the investigated drugs in pure and pharmaceutical dosage forms with good accuracy and precision; the percentages of label claim ranged from 97.8-102.8 +/- 0.35-1.60%. The results obtained by the proposed spectrophotometric method were comparable with those obtained by the official or reported methods. The proposed method is superior to all the previously reported ion-pair formation-based methods in terms of simplicity because it did not involve extraction procedures for the ion-pair complex. Therefore, this method might be recommended for routine use in quality control laboratories for analysis of the investigated 4-quinolone antibiotics in their pure forms, as well as in pharmaceutical dosage forms.
本文描述了一种通用的自发非萃取分光光度法的开发,用于测定13种具有药学重要性的4-喹诺酮类抗生素。该方法基于在室温下,2%(w/v)β-萘酚试剂与每种被研究药物在硫酸介质中形成黄色水溶性离子对络合物。形成的离子对显色剂在365 - 391 nm范围内有最大吸收峰。对试剂浓度和影响反应的实验条件进行了优化。在最佳条件下,在所研究药物浓度为10 - 350μg/mL范围内,吸光度与浓度之间呈现良好的线性关系,线性系数为0.9987 - 0.9995。该方法的检测限和定量限分别为1 - 9.9μg/mL和3.4 - 32.9μg/mL。方法的精密度令人满意;相对标准偏差值不超过2%。所提出的方法成功应用于纯品和药物剂型中被研究药物的分析,具有良好的准确度和精密度;标示量的百分比范围为97.8 - 102.8±0.35 - 1.60%。所提出的分光光度法得到的结果与官方或报道方法得到的结果具有可比性。所提出的方法在简单性方面优于所有先前报道的基于离子对形成的方法,因为它不涉及离子对络合物的萃取过程。因此,该方法可推荐用于质量控制实验室常规分析所研究的4-喹诺酮类抗生素的纯品以及药物剂型。