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分析方法的开发和验证,用于分光荧光光度法和分光光度法测定药物中的一些抗菌药物。

Analytical method development and validation of spectrofluorimetric and spectrophotometric determination of some antimicrobial drugs in their pharmaceuticals.

机构信息

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, 35516 Mansoura, Egypt.

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, 35516 Mansoura, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2018 Jan 5;188:525-536. doi: 10.1016/j.saa.2017.07.033. Epub 2017 Jul 24.

Abstract

In this study, three novel, sensitive, simple and validated spectrophotometric and spectrofluorimetric methods have been proposed for estimation of some important antimicrobial drugs. The first two methods have been proposed for estimation of two important third-generation cephalosporin antibiotics namely, cefixime and cefdinir. Both methods were based on condensation of the primary amino group of the studied drugs with acetyl acetone and formaldehyde in acidic medium. The resulting products were measured by spectrophotometric (Method I) and spectrofluorimetric (Method II) tools. Regarding method I, the absorbance was measured at 315nm and 403nm with linearity ranges of 5.0-140.0 and 10.0-100.0μg/mL for cefixime and cefdinir, respectively. Meanwhile in method II, the produced fluorophore was measured at λ 488nm or 491nm after excitation at λ 410nm with linearity ranges of 0.20-10.0 and 0.20-36.0μg/mL for cefixime and cefdinir, respectively. On the other hand, method III was devoted to estimate nifuroxazide spectrofluorimetrically depending on formation of highly fluorescent product upon reduction of the studied drug with Zinc powder in acidic medium. Measurement of the fluorescent product was carried out at λ 335nm following excitation at λ 255nm with linearity range of 0.05 to 1.6μg/mL. The developed methods were subjected to detailed validation procedure, moreover they were used for the estimation of the concerned drugs in their pharmaceuticals. It was found that there is a good agreement between the obtained results and those obtained by the reported methods.

摘要

在这项研究中,提出了三种新颖、灵敏、简单和经过验证的分光光度法和荧光光度法,用于估计一些重要的抗菌药物。前两种方法是为了估计两种重要的第三代头孢菌素抗生素,即头孢克肟和头孢地尼。这两种方法都是基于研究药物的伯氨基与乙酰丙酮和甲醛在酸性介质中缩合。所得产物通过分光光度法(方法 I)和荧光光度法(方法 II)进行测量。关于方法 I,在 315nm 和 403nm 处测量吸光度,头孢克肟和头孢地尼的线性范围分别为 5.0-140.0 和 10.0-100.0μg/mL。同时,在方法 II 中,在 410nm 激发后,在 488nm 或 491nm 处测量产生的荧光团,头孢克肟和头孢地尼的线性范围分别为 0.20-10.0 和 0.20-36.0μg/mL。另一方面,方法 III 致力于通过在酸性介质中用锌粉还原研究药物来荧光光度法估计硝呋唑酮。在 λ 255nm 激发后,在 λ 335nm 处测量荧光产物的荧光强度,线性范围为 0.05 至 1.6μg/mL。所开发的方法经过详细的验证程序,此外,它们还用于估计其药品中的相关药物。结果表明,所得结果与已报道的方法所得结果之间存在良好的一致性。

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