摘要
目的对硫酸多黏菌素中的低含量成分进行纯化和鉴定。方法利用两次反相色谱纯化制备得到单组份,并通过Nα-(2,4-二硝基-5-氟苯基)-L-丙氨酰胺(Nα-(2,4-Dinitro-5-fluorophenyl)-L-alaninamide,FDAA)试剂衍生法研究组分的组成氨基酸及其构型。基于二级质谱和氨基酸组成的结果对化合物进行了结构鉴定。结果多黏菌素E2的氨基酸组成、分子量与文献报道一致;杂质3和杂质9结构中含有L-Leu残基和羟基化的脂肪酸链;杂质6含有L-Val残基。结论杂质3、杂质6和杂质9分别为3-OHE2、Val-E2和3-OH-E1。
Objective The purification and identification of minor components in colistin E. Methods Each single component was purified by using reverse-phase chromatography twice, and derivatization using the reagent FDAA was performed to analyze the amino acid composition and the stereochemistry of each component. Structural identification was based on the secondary mass spectrometry and amino acid composition. Results The amino acid composition and molecular weight of colistin E2 were consistent with those published reports. Both impurities 3 and 9 contained L-Leu residues and hydroxylated fatty acid chains. The impurity 6 contained an L-Val residue. Conclusion Impurity 3, impurity 6, and impurity 9 were 3-OH-E2, Val-E2, and 3-OH-E 1, respectively.
出处
《中国抗生素杂志》
CAS
CSCD
2018年第1期59-63,共5页
Chinese Journal of Antibiotics
关键词
多黏菌素E
纯化
结构鉴定
Colistin E
Purification
Structure elucidation
