Headspace in-tube extraction gas chromatography-mass spectrometry for the analysis of hydroxylic methyl-derivatized and volatile organic compounds in blood and urine.
A novel headspace in-tube extraction gas chromatography-mass spectrometry (ITEX-GC-MS) approach was developed for broad-scale analysis of low molecular weight organic compounds in blood and/or urine. One sample was analyzed following in-vial derivatization with dimethyl sulfate for ethylene glycol (EG), glycolic acid (GA), formic acid (FA), other hydroxylic compounds, and another sample for underivatized volatile organic compounds. Tenax adsorbent resin was used in the microtrap, and a porous layer, open tubular GC capillary column was used for separation. MS was operated in the full-scan mode, identification was based on the Automated Mass Spectral Deconvolution and Identification System, and quantification was based on extracted ions. The limits of quantification for EG, GA, and FA in blood were 10, 50, and 30 mg/L, respectively, and the expanded uncertainties of measurement were 20%, 16%, and 14%, respectively. The procedure allowed for the first time the inclusion of EG and GA as their methyl derivatives within a quantitative HS analysis. The ITEX method described here was more sensitive for analysis of volatile organic compounds than the corresponding static headspace analysis as demonstrated for 11 representative compounds.
Rasanen
Ilpo
I
Department of Forensic Medicine, Kytösuontie 11,University of Helsinki, Finland.
Viinamäki
Jenni
J
Vuori
Erkki
E
Ojanperä
Ilkka
I
D000438:Alcohols / Q000032:analysis* / Q000097:blood / Q000737:chemistry / Q000652:urine; D000818:Animals; D002264:Carboxylic Acids / Q000032:analysis* / Q000097:blood / Q000737:chemistry / Q000652:urine; D002417:Cattle; D005591:Chemical Fractionation / Q000379:methods*; D019855:Ethylene Glycol / Q000032:analysis / Q000097:blood / Q000737:chemistry / Q000652:urine; D005561:Formates / Q000032:analysis / Q000097:blood / Q000737:chemistry / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006016:Glycolates / Q000032:analysis / Q000097:blood / Q000737:chemistry / Q000652:urine; D006801:Humans; D020407:Internet; D008745:Methylation; D015203:Reproducibility of Results; D012984:Software; D013463:Sulfuric Acid Esters / Q000737:chemistry; D055549:Volatile Organic Compounds / Q000097:blood* / Q000652:urine*
D000438:Alcohols; D002264:Carboxylic Acids; D005561:Formates; D006016:Glycolates; D013463:Sulfuric Acid Esters; D055549:Volatile Organic Compounds; C031149:glycolic acid; C030544:formic acid; D019855:Ethylene Glycol; C007482:dimethyl sulfate