Histamine and tele-methylhistamine quantification in cerebrospinal fluid from narcoleptic subjects by liquid chromatography tandem mass spectrometry with precolumn derivatization
Section snippets
Materials
Histamine dihydrochloride, tele-methylhistamine (1-methylhistamine) dihydrochloride, (R)-α-methylhistamine dihydrochloride, 4-bromobenzenesulfonyl chloride (4-BBS), triethylamine, and bovine serum albumin (BSA) were purchased from Sigma–Aldrich (France). Artificial CSFs were obtained from Harvard Apparatus (France). Acetonitrile, water (LC–MS grade), and formic acid were obtained from Fischer (France).
Analyses were performed on a UPLC™–MS/MS system consisting of a Quattro Premier® XE
Evaluation and validation of HA and t-MHA assays
The derivatization conditions led to a single derivative on the primary amine group and not the imidazole nucleus (Scheme 2).
Derivatization yields, as determined over three distinct experiments by comparing areas of HA and t-MHA (at six concentrations of a calibration curve) that had been derivatized during the assay to corresponding areas of authentic derivatized amines, were 103.0 ± 2.0 and 99.5 ± 1.2% for HA and t-MHA, respectively (means ± standard errors [SEMs], n = 36). For IS, derivatization
Discussion
We have developed and validated a new method for the combined assay of HA and t-MHA in human CSF based on precolumn derivatization of both amines [21], [22], [23], [24], [25] as para-bromobenzenesulfonamides followed by UPLC™–MS/MS analysis and positive ESI. The interest of the process lies on easier isolation of the hydrophobic derivatives on a UPLC™ column of the C18 type and the sensitive mass spectrometric detection of bromine-containing compounds, leading to stronger isotopic signals with
Acknowledgments
The contribution of Stéphanie Le Meur and Anthony Chéné in chemical synthesis is gratefully acknowledged. This work was supported by Bioprojet Biotech and Institut National de la Santé et de la Recherche Médicale (INSERM U888).
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