Journal
TALANTA
Volume 78, Issue 2, Pages 638-642Publisher
ELSEVIER
DOI: 10.1016/j.talanta.2008.12.025
Keywords
Capillary electrophoresis-mass spectrometry; Sol-gel concentrator; Preconcentration; Cerebrospinal fluid; Methionine enkephalin
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In this study, a CE-MS method using a monolithic sol-gel concentrator for in-line solid-phase extraction (SPE) is evaluated for the analysis of methionine enkephalin in biological samples. Operational SPE parameters such as sample pH, loading volume, elution volume and composition have been studied. After optimization of the in-line preconcentration methodology, a 40-fold preconcentration was demonstrated for a methionine enkephalin test solution using a loading volume of 3200 nL. The method was linear in the range from 62.5 to 1000 ng/mL (R-2 > 0.99). R.S.D. values for migration times and peak areas were 1.2% and 8.4%, respectively. Finally, the analysis of cerebrospinal fluid samples spiked with methionine enkephalin and deproteinized with perchloric acid (1: 1, v/v) showed a detection limit (S/N = 3) of approximately 1 ng/mL (ca. 5 nM). The recoveries of methionine enkephalin for three concentration levels (100, 10 and I ng/mL) were in the range of 74-91%, demonstrating the promising potential of the methodology for the analysis of biological samples. (C) 2008 Elsevier B.V. All rights reserved.
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