Quantification of Cyclosporin A in Human Cerebrospinal Fluid by Liquid Chromatography‐Mass Spectrometry using Atmospheric Pressure Chemical Ionization

Autor: H. Thomas Karnes, Sunil S. Iyer, Gretchen M. Brophy, M. Ross Bullock, Leslie Edinboro
Rok vydání: 2007
Předmět:
Zdroj: Journal of Liquid Chromatography & Related Technologies. 30:1733-1747
ISSN: 1520-572X
1082-6076
Popis: 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.
Databáze: OpenAIRE
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