Separation of cyclosporins by high-performance liquid chromatography and mass spectrometric study of cyclosporin metabolites

Jari Tuominen (Corresponding Author), Tapani Suortti, K. Ishikawa, J. Lundell, Y. Koga

Research output: Contribution to journalArticleScientificpeer-review

5 Citations (Scopus)

Abstract

A semi‐preparative (high‐performance liquid chromatography) method for separation of cyclosporin metabolites in a fungal fermentation sample was developed.
By using the optimized chromatographic separation, 20 cyclosporin metabolites in a process sample were isolated, and their molecular masses measured by double focusing sector mass spectrometry. The structures of some of the cyclosporin congeners were investigated by tandem sector mass spectrometry using fast atom bombardment ionization.
The isobaric cyclosporins D ([Val2]CS) and G ([Nva2]CS) were differentiated by significantly different relative intensities of a fragment ion at m/z 30 [CH4N]+ from a precursor ion at m/z 72 [C4H10N]+. Otherwise the tandem mass spectrometry (MS/MS) spectra of the fragment ions of the two isomers are very similar.
Cyclosporin A and iso‐cyclosporin A were also analysed by high energy MS/MS. No significant fragment ions were found to provide distinctions between them.
Relatively good overviews of process samples containing very similar structures were achieved by combining LC separation, molecular ion recognition and MS/MS characterization.
Original languageEnglish
Pages (from-to)1085-1091
JournalRapid Communications in Mass Spectrometry
Volume12
Issue number16
DOIs
Publication statusPublished - 1998
MoE publication typeA1 Journal article-refereed

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Cyclosporins
High performance liquid chromatography
Metabolites
Cyclosporine
Ions
Mass spectrometry
Liquid chromatography
Molecular mass
Isomers
Fermentation
Ionization
Atoms

Cite this

Tuominen, Jari ; Suortti, Tapani ; Ishikawa, K. ; Lundell, J. ; Koga, Y. / Separation of cyclosporins by high-performance liquid chromatography and mass spectrometric study of cyclosporin metabolites. In: Rapid Communications in Mass Spectrometry. 1998 ; Vol. 12, No. 16. pp. 1085-1091.
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abstract = "A semi‐preparative (high‐performance liquid chromatography) method for separation of cyclosporin metabolites in a fungal fermentation sample was developed. By using the optimized chromatographic separation, 20 cyclosporin metabolites in a process sample were isolated, and their molecular masses measured by double focusing sector mass spectrometry. The structures of some of the cyclosporin congeners were investigated by tandem sector mass spectrometry using fast atom bombardment ionization. The isobaric cyclosporins D ([Val2]CS) and G ([Nva2]CS) were differentiated by significantly different relative intensities of a fragment ion at m/z 30 [CH4N]+ from a precursor ion at m/z 72 [C4H10N]+. Otherwise the tandem mass spectrometry (MS/MS) spectra of the fragment ions of the two isomers are very similar. Cyclosporin A and iso‐cyclosporin A were also analysed by high energy MS/MS. No significant fragment ions were found to provide distinctions between them. Relatively good overviews of process samples containing very similar structures were achieved by combining LC separation, molecular ion recognition and MS/MS characterization.",
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Separation of cyclosporins by high-performance liquid chromatography and mass spectrometric study of cyclosporin metabolites. / Tuominen, Jari (Corresponding Author); Suortti, Tapani; Ishikawa, K.; Lundell, J.; Koga, Y.

In: Rapid Communications in Mass Spectrometry, Vol. 12, No. 16, 1998, p. 1085-1091.

Research output: Contribution to journalArticleScientificpeer-review

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T1 - Separation of cyclosporins by high-performance liquid chromatography and mass spectrometric study of cyclosporin metabolites

AU - Tuominen, Jari

AU - Suortti, Tapani

AU - Ishikawa, K.

AU - Lundell, J.

AU - Koga, Y.

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AB - A semi‐preparative (high‐performance liquid chromatography) method for separation of cyclosporin metabolites in a fungal fermentation sample was developed. By using the optimized chromatographic separation, 20 cyclosporin metabolites in a process sample were isolated, and their molecular masses measured by double focusing sector mass spectrometry. The structures of some of the cyclosporin congeners were investigated by tandem sector mass spectrometry using fast atom bombardment ionization. The isobaric cyclosporins D ([Val2]CS) and G ([Nva2]CS) were differentiated by significantly different relative intensities of a fragment ion at m/z 30 [CH4N]+ from a precursor ion at m/z 72 [C4H10N]+. Otherwise the tandem mass spectrometry (MS/MS) spectra of the fragment ions of the two isomers are very similar. Cyclosporin A and iso‐cyclosporin A were also analysed by high energy MS/MS. No significant fragment ions were found to provide distinctions between them. Relatively good overviews of process samples containing very similar structures were achieved by combining LC separation, molecular ion recognition and MS/MS characterization.

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