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采用液相色谱-质谱联用法鉴定比替米星的组成成分。

Identification of the components of bitespiramycin by liquid chromatography-mass spectrometry.

机构信息

Department of Antibiotics, National Institutes for Food and Drug control, Beijing 100050, PR China.

出版信息

J Pharm Biomed Anal. 2012 Jul;66:402-10. doi: 10.1016/j.jpba.2012.03.013. Epub 2012 Mar 15.

DOI:10.1016/j.jpba.2012.03.013
PMID:22482901
Abstract

Reversed-phase liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was used to characterize the components of bitespiramycin, a group of 4"-acylated spiramycins produced by bioengineered strains. In total 38 components were characterized in commercial samples, including 12 impurities that had never been reported before and 12 other that were partially characterized. The structures of these unknown compounds were deduced by comparison of their fragmentation patterns with those of known major components. Their ultraviolet spectra were used to confirm the presence of an α-, β-, γ-, δ-unsaturated butadiene in the macrocyclic lactone. Compared with the classical method, LC/ESI-MS/MS is particularly advantageous in terms of sensitivity and efficiency to characterize minor components at trace levels in multi-component antibiotics.

摘要

反相液相色谱-电喷雾串联质谱联用(LC/ESI-MS/MS)用于对由生物工程菌株产生的一组 4”-酰化螺旋霉素的成分进行分析。在商业样品中总共鉴定了 38 个成分,包括 12 种以前从未报道过的杂质和 12 种其他部分鉴定的杂质。通过比较这些未知化合物的碎片模式与已知主要成分的碎片模式,推断出这些未知化合物的结构。通过它们的紫外光谱来确定在大环内酯中存在α-、β-、γ-、δ-不饱和丁二烯。与经典方法相比,LC/ESI-MS/MS 在灵敏度和效率方面具有特别的优势,可用于分析多组分抗生素中痕量水平的微量成分。

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