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 in | Journal of chromatography. B, Biomedical sciences and applications Vol. 696; no. 1; pp. 53 - 58 |
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Main Authors | , |
Format | Journal Article |
Language | English |
Published |
Amsterdam
Elsevier B.V
15.08.1997
Elsevier Science |
Subjects | |
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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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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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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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