0000000000177651
AUTHOR
I. Manz
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…
Evidence for a surface self-cleaning sputtering mechanism in fast atom bombardment mass spectrometry
Evidence for a surface self-cleaning sputtering mechanism in fast atom bombardment mass spectrometry involving significant sputtering from the bulk of the glycerol matrix has been obtained from (a) the time dependence of sample ion abundances and chemical noise for bioorganic compounds, (b) determinations of the sputtering volume in glycerol solution, and (c) studies of in situ chemical and biochemical reactions. The relevance of these results for optimal sample/matrix preparation in analytical applications is pointed out.
Identification and quantification of metabolite conjugates of activated cyclophosphamide and ifosfamide with mesna in urine by ion-pair extraction and fast atom bombardment mass spectrometry.
The high bladder toxicity of the alkylating oxazaphosphorine anticancer drugs, cyclophosphamide and ifosfamide is effectively reduced by the concomitant administration of mesna (sodium 2-mercaptoethane sulphonate). The formation and rapid urinary excretion of conjugates of the activated (4-hydroxylated) oxazaphosphorine metabolites with mesna has been suggested as the pharmacological basis for the selective detoxification, but separation and identification of such metabolites in vivo have been extremely difficult due to their high polarity and chemical lability. In this study an ion-pair extraction procedure in combination with positive and negative ion fast atom bombardment mass spectromet…