液相色谱-质谱联用法鉴定必特螺旋霉素中多组分

采用 Kromasil C18色谱柱 ( 5μm粒径 ,2 0 0× 4.6mm内径 ) ,流动相为乙腈 -1 0 mmol/ L乙酸铵溶液 ( V(乙腈 )∶V(乙酸铵 ) =60∶ 45 ) ,建立快速分析抗生素新药必特螺旋霉素中复杂多组分的分析方法。采用电喷雾离子化源 ,以正离子检测方式进行一级、二级全扫描质谱分析。研究表明 :其中含有 1 0种螺旋霉素类衍生物并推断出化学结构 ,通过与对照品的色谱和质谱行为对比得到验证。采用液相色谱 -质谱联用技术 ( LC-MSn)可以快速阐明复杂多组分抗生素新药必特螺旋霉素类的化学组成 ,并且可以作为一种简单、便捷的分析方法对大环内酯类新抗生素进行高通量筛选。

Analysis of Multicomponent in Bitespiramycin by High-performance Liquid Chromatography-Mass Spectrometry

A method was developed to rapidly analyze complex multicomponent in a novel antibiotic bitespiramycin. A Kromasil C 18 column (200×4.6 mm, 5 μm particle size) was used. The mobile phase consists of acetonitrile -10 mmol/L ammonium acetate ( V (acetonitrile)∶ V (ammonium acetate)=60∶45). An electrospray ionization source was used for mass analysis and detection. The full scan and two stage scans were performed in the positive ion detection mode. The results showed that ten spiramycin derivatives were found in bitespiramycin. Their chemical structures were deduced and identified by the reference substances of them, respectively. It indicated that high performance liquid chromatography mass spectrometry was successfully applied to profile components in a novel antibiotic bitespiramycin and should be intended as a simple and convenient way for the high throughput analysis of screening novel macrolide antibiotics.