Concentrations of quinolinic acid in cerebrospinal fluid measured by gas chromatography and electron-impact ionisation mass spectrometry: Age-related changes in a paediatric reference population

A simple method for the determination of the excitotoxin, quinolinic acid (QUIN) in cerebrospinal fluid (CSF) is described. QUIN, in lyophilized samples, was silylated by N-methyl- N-( tert.-butyldimethylsilyl)trifluoroacetamide in a single-step reaction at 65 to 70°C to form a di- tert.-butyldimeth...

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Published inJournal of chromatography. B, Biomedical sciences and applications Vol. 696; no. 1; pp. 53 - 58
Main Authors Dobbie, Michael S, Surtees, Robert A.H
Format Journal Article
LanguageEnglish
Published Amsterdam Elsevier B.V 15.08.1997
Elsevier Science
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Abstract A simple method for the determination of the excitotoxin, quinolinic acid (QUIN) in cerebrospinal fluid (CSF) is described. QUIN, in lyophilized samples, was silylated by N-methyl- N-( tert.-butyldimethylsilyl)trifluoroacetamide in a single-step reaction at 65 to 70°C to form a di- tert.-butyldimethylsilyl ester. Neither pre-purification of QUIN from CSF nor post-derivatisation sample clean-up was required. The derivatives were analysed by gas chromatography–electron impact mass spectrometry resulting in a prominent and characteristic [M−57] + fragment ion which was used for quantitation. 2,6-Pyridine dicarboxylic acid, a structural analog of QUIN, was used as the internal standard. The detection limits for injected standards are in the femtomole range. CSF QUIN was found to be age-related and three preliminary reference ranges for CSF QUIN were found: 0 to 1 years, 31±15 n M QUIN (mean±standard deviation); 1.1 to 3 years, 26±15 n M; 3.1 to 14 years, 14±9 n M.
AbstractList A simple method for the determination of the excitotoxin, quinolinic acid (QUIN) in cerebrospinal fluid (CSF) is described. QUIN, in lyophilized samples, was silylated by N-methyl- N-( tert.-butyldimethylsilyl)trifluoroacetamide in a single-step reaction at 65 to 70°C to form a di- tert.-butyldimethylsilyl ester. Neither pre-purification of QUIN from CSF nor post-derivatisation sample clean-up was required. The derivatives were analysed by gas chromatography–electron impact mass spectrometry resulting in a prominent and characteristic [M−57] + fragment ion which was used for quantitation. 2,6-Pyridine dicarboxylic acid, a structural analog of QUIN, was used as the internal standard. The detection limits for injected standards are in the femtomole range. CSF QUIN was found to be age-related and three preliminary reference ranges for CSF QUIN were found: 0 to 1 years, 31±15 n M QUIN (mean±standard deviation); 1.1 to 3 years, 26±15 n M; 3.1 to 14 years, 14±9 n M.
A simple method for the determination of the excitotoxin, quinolinic acid (QUIN) in cerebrospinal fluid (CSF) is described. QUIN, in lyophilized samples, was silylated by N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide in a single-step reaction at 65 to 70 degrees C to form a di-tert.-butyldimethylsilyl ester. Neither pre-purification of QUIN from CSF nor post-derivatisation sample clean-up was required. The derivatives were analysed by gas chromatography-electron impact mass spectrometry resulting in a prominent and characteristic [M-57]+ fragment ion which was used for quantitation. 2,6-Pyridine dicarboxylic acid, a structural analog of QUIN, was used as the internal standard. The detection limits for injected standards are in the femtomole range. CSF QUIN was found to be age-related and three preliminary reference ranges for CSF QUIN were found: 0 to 1 years, 31 +/- 15 nM QUIN (mean +/- standard deviation): 1.1 to 3 years, 26 +/- 15 nM; 3.1 to 14 years, 14 +/- 9 nM.
Author Surtees, Robert A.H
Dobbie, Michael S
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Issue 1
Keywords Quinolinic acid
Human
Biological fluid
Pediatrics
Nervous system diseases
Biological marker
Cerebrospinal fluid
Medical screening
Gas chromatography
Laboratory investigations
Clinical biology
Child
Mass spectrometry
Quantitative analysis
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PublicationTitle Journal of chromatography. B, Biomedical sciences and applications
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PublicationYear 1997
Publisher Elsevier B.V
Elsevier Science
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SubjectTerms Adolescent
Age Factors
Biological and medical sciences
Cerebrospinal fluid (biochemistry, cytology, circulation, manometry). Intracranial pressure determination
Child
Child, Preschool
Gas Chromatography-Mass Spectrometry - methods
Humans
Infant
Infant, Newborn
Investigative techniques, diagnostic techniques (general aspects)
Medical sciences
Quinolinic acid
Quinolinic Acid - cerebrospinal fluid
Quinolinic Acid - chemistry
Reference Standards
Reference Values
Reproducibility of Results
Sensitivity and Specificity
Title Concentrations of quinolinic acid in cerebrospinal fluid measured by gas chromatography and electron-impact ionisation mass spectrometry: Age-related changes in a paediatric reference population
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