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N-溴代琥珀酰亚胺作为分光光度法测定氟喹诺酮类抗生素的新型分析试剂的评估。

Evaluation of N-bromosuccinimide as a new analytical reagent for the spectrophotometric determination of fluoroquinolone antibiotics.

作者信息

Askal Hassan, Refaat Ibrahim, Darwish Ibrahim, Marzouq Mostafa

机构信息

Department of Pharmaceutical Analytical Chemistry, Assiut University, Assiut 71526, Egypt.

出版信息

Chem Pharm Bull (Tokyo). 2007 Nov;55(11):1551-6. doi: 10.1248/cpb.55.1551.

Abstract

Analytical studies were carried out, for the first time, to evaluate the use of N-bromosuccinimide (NBS) as an analytical reagent for the spectrophotometric determination of eleven therapeutically important fluoroquinolone antibiotics (FQA). The procedures involved the reaction of the FQA with NBS and subsequent measurement of the excess NBS by its reaction with p-phenylenediamine (PDA) to give a violet colored product that was measured at 530 nm. Different variables affecting the reaction (concentration of NBS, concentration of PDA, pH of reaction medium, reaction time, and the diluting solvents) were carefully studied and optimized. The molar ratio and mechanism of the reaction between each of the studied FQA with NBS were proposed using UV-vis, IR, and NMR techniques. Under the optimum reaction conditions, the analytical method was developed and validated. Beer's law was obeyed in the general concentration range of 3-25 microg/ml. The assay limits of detection and quantitation were 0.33-1.29 and 1.10-4.31 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 FQA in their pure and pharmaceutical dosage forms without interference from the common excipients (label claim values were 99.85-100.17+/-0.13-0.59%). Interference from ascorbic acid, that is co-formulated as a stabilizer for the ampoule form, was avoided by its pre-oxidation with potassium bromate before applying the analytical procedure. The results obtained by the proposed method were comparable with those obtained by the official and reported methods.

摘要

首次开展了分析研究,以评估使用N-溴代琥珀酰亚胺(NBS)作为分析试剂,通过分光光度法测定11种具有重要治疗意义的氟喹诺酮类抗生素(FQA)。该方法包括FQA与NBS的反应,随后通过NBS与对苯二胺(PDA)反应测定过量的NBS,生成一种在530nm处测定的紫色产物。仔细研究并优化了影响反应的不同变量(NBS浓度、PDA浓度、反应介质的pH值、反应时间和稀释溶剂)。利用紫外可见光谱、红外光谱和核磁共振技术,提出了所研究的每种FQA与NBS之间的反应摩尔比和反应机理。在最佳反应条件下,建立并验证了该分析方法。在3-25μg/ml的一般浓度范围内符合比尔定律。检测限和定量限分别为0.33-1.29和1.10-4.31μg/ml。该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所研究FQA的分析,不受常见辅料的干扰(标示值为99.85-100.17±0.13-0.59%)。对于作为安瓿剂稳定剂共同配制的抗坏血酸的干扰,在应用分析程序之前通过用溴酸钾对其进行预氧化来避免。所提出的方法获得的结果与官方方法和报道方法获得的结果相当。

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