Determination of acidic catecholamine metabolites in plasma and cerebrospinal fluid using gas chromatography-negative-ion mass spectrometry.
A method for the assay of acidic catecholamine metabolites in biological fluids using capillary gas chromatography--electron-capture negative-ion mass spectrometry is described. The method combines acetylation of phenolic hydroxy groups in buffered aqueous solution followed by pentafluorobenzyl ester formation and acetylation of aliphatic hydroxy groups under anhydrous conditions. The resulting per-O-acetyl carboxypentafluorobenzyl esters provided excellent negative-ion mass spectra with intense and diagnostic anions. The sensitivity of the analysis using electron-capture negative-ion mass spectrometry exceeds that using electron-impact mass spectrometry by two to three orders of magnitude. Analysis of acidic catecholamine metabolites in human lumbar cerebrospinal fluid and plasma were performed with good precision (sigma rel less than 5%) at the low nanomoles per litre level.
D015102:3,4-Dihydroxyphenylacetic Acid / Q000097:blood / Q000134:cerebrospinal fluid; D000107:Acetylation; D000328:Adult; D002395:Catecholamines / Q000097:blood / Q000134:cerebrospinal fluid / Q000378:metabolism*; D008401:Gas Chromatography-Mass Spectrometry; D006719:Homovanillic Acid / Q000097:blood / Q000134:cerebrospinal fluid; D006801:Humans; D013696:Temperature; D014642:Vanilmandelic Acid / Q000097:blood / Q000134:cerebrospinal fluid
D002395:Catecholamines; D015102:3,4-Dihydroxyphenylacetic Acid; D014642:Vanilmandelic Acid; D006719:Homovanillic Acid