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, M. Ross Bullock

Research output: Contribution to journalArticlepeer-review

4 Scopus citations

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

Keywords

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

ASJC Scopus subject areas

  • Analytical Chemistry
  • Clinical Biochemistry

Fingerprint Dive into the research topics of 'Quantification of cyclosporin a in human cerebrospinal fluid by liquid chromatography-mass spectrometry using atmospheric pressure chemical ionization'. Together they form a unique fingerprint.

Cite this