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基于其胺部分与乙酰丙酮/甲醛和邻苯二醛/苯乙醛试剂的选择性缩合反应,建立了测定奈替米星的灵敏光谱荧光法。

Development of Sٍٍensitive Spectrofluorimetric Methods for Determining Netilmicin Based on Selective Condensation Reactions of its Amine Moiety with each Acetylacetone/Formaldehyde and Ninhydrin/Phenylacetaldehyde Reagents.

机构信息

Department of Chemistry, College of Science, University of Jeddah, P.O. Box 80327, Jeddah 21589, Saudi Arabia.

Department of Chemistry, College of Science, Princess Nourah bint Abdulrahman University, P.O. Box 84428, Riyadh 11671, Saudi Arabia.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2023 Oct 15;299:122839. doi: 10.1016/j.saa.2023.122839. Epub 2023 May 11.

DOI:10.1016/j.saa.2023.122839
PMID:37201330
Abstract

Netilmicin is an aminoglycoside antibiotic used to treat infections caused by a broad spectrum of Gram-negative and Gram-positive bacteria and is pharmaceutically formulated in ophthalmic dosage forms. In this study, two spectrofluorimetric approaches were designed and developed to switch-on the fluorescence activity of NTC. The first method, or Hantzsch (HNZ) method, was relied on measuring the generated fluorescence intensity upon the condensation of NTC with acetylacetone and formaldehyde (Hantzsch reaction) at λ=483 nm/λ=425.5 nm. While the second fluorometric method (NHD method) was relied on measuring the generated fluorescence intensity upon the condensation of NTC with ninhydrin/phenylacetaldehyde at λ=482.2 nm/λ=385.8 nm. The reaction conditions for the two approaches were well investigated and optimized. The selectivity study for the methods was investigated by determining NTC in the presence of the co-formulated drug (dexamethasone) and pharmaceutical excipients. The validation for two approaches was performed based on ICH guidelines, and ranges of linearity were 0.1-1.2 and 1.5-6.0 µg/mL, while LOD values were 0.039 and 0.207 µg/mL for the HNZ method and the NHD method, respectively. Finally, NTC has been determined in different ophthalmic preparations by the proposed approaches with adequate recovery values.

摘要

奈替米星是一种氨基糖苷类抗生素,用于治疗由广谱革兰氏阴性和革兰氏阳性菌引起的感染,并且在眼科制剂中配制成药物。在这项研究中,设计并开发了两种分光荧光方法来开启 NTC 的荧光活性。第一种方法,或 Hantzsch(HNZ)方法,依赖于在 NTC 与乙酰丙酮和甲醛(Hantzsch 反应)缩合时测量生成的荧光强度,在 λ=483nm/λ=425.5nm 处。而第二种荧光方法(NHD 方法)则依赖于在 NTC 与邻苯二醛/苯乙醛缩合时测量生成的荧光强度,在 λ=482.2nm/λ=385.8nm 处。两种方法的反应条件都经过了充分的研究和优化。通过测定 NTC 在共同配制成药物(地塞米松)和药物赋形剂存在下的方法选择性研究。两种方法的验证均基于 ICH 指南进行,线性范围分别为 0.1-1.2 和 1.5-6.0μg/mL,而 HNZ 方法和 NHD 方法的 LOD 值分别为 0.039 和 0.207μg/mL。最后,通过所提出的方法在不同的眼科制剂中测定了 NTC,并具有足够的回收率值。

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