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采用薄层色谱法和密度测定法以丹磺酰氯新霉素衍生物形式测定新霉素。

Determination of neomycin in the form of neomycin derivative with dabsyl chloride by thin layer chromatography and densitometry.

作者信息

Hubicka Urszula, Zuromska-Witek Barbara, Piotrowska Joanna, Krzek Jan

出版信息

Acta Pol Pharm. 2015 Jan-Feb;72(1):31-7.

PMID:25850198
Abstract

A thin layer chromatographic-densitometric method has been developed for identification and quantitative determination of neomycin derivative with dabsyl chloride. The analysis of antibiotic was achieved on the silica gel TLC plates with fluorescent indicator with n-butanol--2-butanone--25% ammonia--water (10 : 6 : 2 : 2, v/v/v/v) as the mobile phase. The densitometric measurements were made at 460 nm. Under these conditions good separation of chosen aminoglycoside antibiotic from reagent used to make a complex was obtained. The method is characterized by high sensitivity, LOD from 0.1953 μg per band and LOQ from 0.5918 μg per band, wide linearity range from 0.5918 to 2.1960 μg per band for neomycin. The precision of the method was good; RSD varied from 1.17 to 2.05%. Satisfactory results of validation of the method were also confirmed by determination of selected antibiotic in pharmaceutical commercial preparation. The results obtained by TLC-densitometric method were compared with those obtained by spectrophotometric method.

摘要

已开发出一种薄层色谱-密度测定法,用于用丹磺酰氯鉴定和定量测定新霉素衍生物。在带有荧光指示剂的硅胶TLC板上,以正丁醇-2-丁酮-25%氨水-水(10:6:2:2,v/v/v/v)作为流动相,实现了对抗生素的分析。密度测定在460nm处进行。在这些条件下,所选氨基糖苷类抗生素与用于形成复合物的试剂实现了良好分离。该方法具有高灵敏度,每带的检测限为0.1953μg,定量限为0.5918μg,新霉素每带的线性范围宽,为0.5918至2.1960μg。该方法的精密度良好;相对标准偏差在1.17%至2.05%之间。通过测定市售药物制剂中的所选抗生素,也证实了该方法验证的满意结果。将薄层色谱-密度测定法获得的结果与分光光度法获得的结果进行了比较。

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