0000000000177649
AUTHOR
H. Brückner
Elucidation of structure and microheterogeneity of the polypeptide antibiotics paracelsin and trichotoxin A-50 by fast atom bombardment mass spectrometry in combination with selectivein situ hydrolysis
Specific and sensitive procedures have been developed which enabled the structure elucidation of the polypeptide antibiotics (peptaibols), paracelsin isolated from Trichoderma reesei, and of trichotoxin A-50 from Trichoderma viride, by fast atom bombardment and field desorption mass spectrometry. Both peptides were found to exhibit a pronounced microheterogeneity by single and multiple exchange of amino acids. Separation by analytical and semipreparative high-performance liquid chromatography (HPLC) on octadecylsilyl-bonded, reversed-phase columns afforded a series of sequence analogues for each polypeptide. Unequivocal molecular weight and sequence identifications were obtained by positive…
Methods for the rapid detection, isolation and sequence determination of “peptaibols” and other aib-containing peptides of fungal origin. I. Gliodeliquescin a fromGliocladium deliquescens
A rapid and simple detection procedure of Aib-containing “peptaibol” polypeptide antibiotics (mycotoxins) in fungal culture broths is described which employs alkylsilica (Sep-Pak®) cartridges for a selective enrichment, and the utilization of the unusualα-aminoisobutyric acid (Aib) and amino alcohols as specific marker constituents, which are easily detectable in total hydrolysates. Preparative isolations from fermentation broths is facilitated by adsorber resin (XAD) column chromatography, and purification of crude isolates is achieved by silica gel- and sephadex LH-20 chromatography. Preparative HPLC using spherical, totally porous ODS-bonded phases enables the isolation of uniform peptid…
Chromatographic and mass spectrometric characterization of the structures of the polypeptide antibiotics samarosporin and stilbellin and identity with emerimicin
The structural identity of the polypeptide antibiotics, samarosporin I(II) and stilbellin I(II) with emerimicin IV(III) has been established by thin-layer chromatography, quantitative amino acid analysis by ion-exchange chromatography, gas-liquid chromatography of the N-pentafluoropropionyl amino acid n-propyl esters and N,O-bis-pentafluoropropionyl phenylalaninol with quartz capillaries coated with the chiral stationary phase N-propionyl-L-valine-tert-butylamide, and determination of the relative molecular masses and sequence-specific fragments by field desorption fast atom bombardment mass spectrometry. The separation of closely related sequence analogues of the above polypeptides could b…