Quantification of cyclosporin a in human cerebrospinal fluid by liquid chromatography-mass spectrometry using atmospheric pressure chemical ionization

Sunil S. Iyer, Gretchen M. Brophy, H. Thomas Karnes, Leslie E. Edinboro, Ross Bullock

Research output: Contribution to journalArticle

4 Citations (Scopus)

Abstract

Cyclosporin A (CsA) is widely used as an immunosuppressant in organ transplantation, and the treatment of autoimmune disorders. This is the first publication describing a rapid, sensitive, and selective liquid chromatography-mass spectrometry (LC-MS) method for analysis of CsA in cerebrospinal fluid (CSF). Chromatographic separation was achieved using a reversed-phase column with a linear gradient mobile phase. A column switching procedure was incorporated to minimize contamination in the ion source of the mass spectrometer. The sample volume requirement was 50 μL and no internal standard was employed. Quantification was carried out with selected ion reaction (SIR) monitoring of the protonated sodium ion adduct (m/z=1224.7). Calibration curves were linear from 0.5 ng/mL to 20 ng/mL with a weighting factor of 1/x. Precision and accuracy, and reverse predicted concentration residuals were within 15%. The method has been used successfully for the analysis of CSF samples from a clinical study.

Original languageEnglish
Pages (from-to)1733-1747
Number of pages15
JournalJournal of Liquid Chromatography and Related Technologies
Volume30
Issue number12
DOIs
StatePublished - Jan 1 2007
Externally publishedYes

Fingerprint

Cerebrospinal fluid
Atmospheric Pressure
Liquid chromatography
Liquid Chromatography
Cyclosporine
Atmospheric pressure
Ionization
Mass spectrometry
Cerebrospinal Fluid
Mass Spectrometry
Ions
Transplantation (surgical)
Mass spectrometers
Ion sources
Immunosuppressive Agents
Contamination
Sodium
Organ Transplantation
Calibration
Publications

Keywords

  • APCI-SIR
  • Cerebrospinal fluid
  • Cyclosporin A
  • LC-MS

ASJC Scopus subject areas

  • Analytical Chemistry
  • Clinical Biochemistry

Cite this

Quantification of cyclosporin a in human cerebrospinal fluid by liquid chromatography-mass spectrometry using atmospheric pressure chemical ionization. / Iyer, Sunil S.; Brophy, Gretchen M.; Karnes, H. Thomas; Edinboro, Leslie E.; Bullock, Ross.

In: Journal of Liquid Chromatography and Related Technologies, Vol. 30, No. 12, 01.01.2007, p. 1733-1747.

Research output: Contribution to journalArticle

Iyer, Sunil S. ; Brophy, Gretchen M. ; Karnes, H. Thomas ; Edinboro, Leslie E. ; Bullock, Ross. / Quantification of cyclosporin a in human cerebrospinal fluid by liquid chromatography-mass spectrometry using atmospheric pressure chemical ionization. In: Journal of Liquid Chromatography and Related Technologies. 2007 ; Vol. 30, No. 12. pp. 1733-1747.
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