Histamine and tele-methylhistamine quantification in cerebrospinal fluid from narcoleptic subjects by liquid chromatography tandem mass spectrometry with precolumn derivatization

An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™–MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard ( N- tele-( R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The...

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Published in	Analytical biochemistry Vol. 409; no. 1; pp. 28 - 36
Main Authors	Croyal, Mikaël, Dauvilliers, Yves, Labeeuw, Olivier, Capet, Marc, Schwartz, Jean-Charles, Robert, Philippe
Format	Journal Article
Language	English
Published	United States Elsevier Inc 01.02.2011
Subjects	acetonitrile Adolescent Adult Aged Aged, 80 and over Calibration Cerebrospinal fluid Child Chromatography, High Pressure Liquid - methods Chromatography, High Pressure Liquid - standards Derivatization formic acid Histamine Histamine - cerebrospinal fluid Histamine - standards Humans ionization Liquid chromatography Mass spectrometry metabolites Methylhistamines - cerebrospinal fluid Methylhistamines - standards Middle Aged Narcolepsy Narcolepsy - cerebrospinal fluid patients primary amines reversed-phase liquid chromatography tandem mass spectrometry Tandem Mass Spectrometry - methods Tandem Mass Spectrometry - standards tele-Methylhistamine ultra-performance liquid chromatography tele-Methylhistamine Histamine Liquid chromatography Narcolepsy Cerebrospinal fluid Derivatization Mass spectrometry
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Abstract	An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™–MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard ( N- tele-( R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5 min on an Acquity® BEH C 18 column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50–5000 pM for each amine (5.5–555 pg/ml for histamine and 6.25–625 pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean ± standard error levels of these amines between a group of narcoleptic patients (histamine = 392 ± 64 pM, tele-methylhistamine = 2431 ± 461 pM, n = 7) and of neurological control subjects (histamine = 402 ± 72 pM, tele-methylhistamine = 2209 ± 463 pM, n = 32).
AbstractList	An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™-MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard (N-tele-(R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5 min on an Acquity® BEH C(18) column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50-5000 pM for each amine (5.5-555 pg/ml for histamine and 6.25-625 pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean ± standard error levels of these amines between a group of narcoleptic patients (histamine=392 ± 64 pM, tele-methylhistamine=2431 ± 461 pM, n=7) and of neurological control subjects (histamine=402 ± 72 pM, tele-methylhistamine=2209 ± 463 pM, n=32). An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™–MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard (N-tele-(R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5min on an Acquity® BEH C₁₈ column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50–5000pM for each amine (5.5–555pg/ml for histamine and 6.25–625pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean±standard error levels of these amines between a group of narcoleptic patients (histamine=392±64pM, tele-methylhistamine=2431±461pM, n=7) and of neurological control subjects (histamine=402±72pM, tele-methylhistamine=2209±463pM, n=32). An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™-MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard (N-tele-(R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5 min on an Acquity® BEH C(18) column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50-5000 pM for each amine (5.5-555 pg/ml for histamine and 6.25-625 pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean ± standard error levels of these amines between a group of narcoleptic patients (histamine=392 ± 64 pM, tele-methylhistamine=2431 ± 461 pM, n=7) and of neurological control subjects (histamine=402 ± 72 pM, tele-methylhistamine=2209 ± 463 pM, n=32).An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™-MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard (N-tele-(R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5 min on an Acquity® BEH C(18) column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50-5000 pM for each amine (5.5-555 pg/ml for histamine and 6.25-625 pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean ± standard error levels of these amines between a group of narcoleptic patients (histamine=392 ± 64 pM, tele-methylhistamine=2431 ± 461 pM, n=7) and of neurological control subjects (histamine=402 ± 72 pM, tele-methylhistamine=2209 ± 463 pM, n=32). An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™–MS/MS) assay was developed for the simultaneous analysis of histamine, its major metabolite tele-methylhistamine, and an internal standard ( N- tele-( R)-α-dimethylhistamine) from human cerebrospinal fluid (CSF) samples. The method involves derivatization of primary amines with 4-bromobenzenesulfonyl chloride and subsequent analysis by reversed phase liquid chromatography with mass spectrometry detection and positive electrospray ionization. The separation of derivatized biogenic amines was achieved within 3.5 min on an Acquity® BEH C 18 column by elution with a linear gradient of acetonitrile/water/formic acid (0.1%). The assay was linear in the concentration range of 50–5000 pM for each amine (5.5–555 pg/ml for histamine and 6.25–625 pg/ml for tele-methylhistamine). For repeatability and precision determination, coefficients of variation (CVs) were less than 11.0% over the tested concentration ranges, within acceptance criteria. Thus, the developed method provides the rapid, easy, highly sensitive, and selective requirement to quantify these amines in human CSF. No significant difference was found in the mean ± standard error levels of these amines between a group of narcoleptic patients (histamine = 392 ± 64 pM, tele-methylhistamine = 2431 ± 461 pM, n = 7) and of neurological control subjects (histamine = 402 ± 72 pM, tele-methylhistamine = 2209 ± 463 pM, n = 32).
Author	Robert, Philippe Labeeuw, Olivier Dauvilliers, Yves Schwartz, Jean-Charles Croyal, Mikaël Capet, Marc
Author_xml	– sequence: 1 givenname: Mikaël surname: Croyal fullname: Croyal, Mikaël organization: Bioprojet Biotech, Saint Grégoire 35762, France – sequence: 2 givenname: Yves surname: Dauvilliers fullname: Dauvilliers, Yves organization: Department of Neurology, Gui de Chauliac Hospital, CHU Montpellier, INSERM U888, National Reference Network for Orphan Diseases (Narcolepsy, Hypersomnia, and Kleine–Levin Syndrome), Montpellier 34295, France – sequence: 3 givenname: Olivier surname: Labeeuw fullname: Labeeuw, Olivier organization: Bioprojet Biotech, Saint Grégoire 35762, France – sequence: 4 givenname: Marc surname: Capet fullname: Capet, Marc organization: Bioprojet Biotech, Saint Grégoire 35762, France – sequence: 5 givenname: Jean-Charles surname: Schwartz fullname: Schwartz, Jean-Charles organization: Bioprojet Biotech, Saint Grégoire 35762, France – sequence: 6 givenname: Philippe surname: Robert fullname: Robert, Philippe email: p.robert@bioprojet.com organization: Bioprojet Biotech, Saint Grégoire 35762, France
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Keywords	tele-Methylhistamine Histamine Liquid chromatography Narcolepsy Cerebrospinal fluid Derivatization Mass spectrometry
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Snippet	An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™–MS/MS) assay was developed for the simultaneous analysis of histamine, its major... An ultra-performance liquid chromatography tandem mass spectrometry (UPLC™-MS/MS) assay was developed for the simultaneous analysis of histamine, its major...
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SubjectTerms	acetonitrile Adolescent Adult Aged Aged, 80 and over Calibration Cerebrospinal fluid Child Chromatography, High Pressure Liquid - methods Chromatography, High Pressure Liquid - standards Derivatization formic acid Histamine Histamine - cerebrospinal fluid Histamine - standards Humans ionization Liquid chromatography Mass spectrometry metabolites Methylhistamines - cerebrospinal fluid Methylhistamines - standards Middle Aged Narcolepsy Narcolepsy - cerebrospinal fluid patients primary amines reversed-phase liquid chromatography tandem mass spectrometry Tandem Mass Spectrometry - methods Tandem Mass Spectrometry - standards tele-Methylhistamine ultra-performance liquid chromatography
Title	Histamine and tele-methylhistamine quantification in cerebrospinal fluid from narcoleptic subjects by liquid chromatography tandem mass spectrometry with precolumn derivatization
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