Liquid chromatography-mass spectrometry with on-line solid-phase extraction by a restricted-access C18 precolumn for direct plasma and urine injection.

Autor: van der Hoeven RA; Division of Analytical Chemistry, Leiden/Amsterdam Centre for Drug Research, Leiden University, Netherlands., Hofte AJ, Frenay M, Irth H, Tjaden UR, van der Greef J, Rudolphi A, Boos KS, Marko Varga G, Edholm LE
Jazyk: angličtina
Zdroj: Journal of chromatography. A [J Chromatogr A] 1997 Feb 21; Vol. 762 (1-2), pp. 193-200.
DOI: 10.1016/s0021-9673(96)01004-7
Abstrakt: In this paper, the on-line coupling of solid-phase extraction, based on a restricted-access support with liquid chromatography-mass spectrometry (LC-MS), for the analysis of biological samples is described. The system was tested with cortisol and prednisolone for plasma analysis and arachidonic acid for urine analysis. A precolumn packed with a 25-micron C18 alkyl-diol support is used for direct plasma or urine injection. Using column-switching techniques, the analytes enriched on the precolumn are eluted to the analytical column without transfer loss. An on-line heart-cut technique was employed and only the analyte-containing fraction eluting from the LC column is directed to the MS to protect the LC-MS interface and ion-source from contamination. The whole system is operated in a parallel mode, that is, sample pre-treatment and LC-MS analysis are performed simultaneously to provide the shortest possible analysis time. The only off-line sample pre-treatment step required was centrifugation to remove particulate matter. With the fully automated system, total analysis times of 5 and 9.5 min were achieved for cortisol in serum and arachidonic acid in urine, respectively. Cortisol and related compounds were quantitatively recovered from plasma with a detection limit for prednisolone (direct injection of 100 microliters on restricted-access precolumn) of 2 ng/ml.
Databáze: MEDLINE