title: Rapid determination of acetone in human blood by derivatization with pentafluorobenzyl hydroxylamine followed by headspace liquid-phase microextraction and gas chromatography/mass spectrometry.
abstract: In the current work, a simple, rapid, accurate and inexpensive method was developed for the determination of acetone in human blood. The proposed method is based on derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), followed by headspace liquid-phase microextraction (HS-LPME) and gas chromatography/mass spectrometry (GC/MS). In the present method, acetone in blood samples was derivatized with PFBHA and acetone oxime formed in several seconds. The formed oxime was enriched by HS-LPME using the organic solvent film (OSF) formed in a microsyringe barrel as extraction interface. Finally, the enriched oxime was analyzed by GC/MS in electron ionization (EI) mode. HS-LPME parameters including solvent, syringe plunger withdrawal rate, sampling volume, and extraction cycle were optimized and the method reproducibility, linearity, recovery and detection limit were studied. The proposed method was applied to determination of acetone in diabetes blood and normal blood. It has been shown that derivatization with HS-LPME and GC/MS is an alternative method for determination of the diabetes biomarker, acetone, in blood samples.
authors.affiliation: Department of Chemistry, Fudan University, Shanghai 200433, China.
authors.forename: Chunhui
authors.initials: C
authors.lastname: Deng
authors.forename: Ning
authors.initials: N
authors.lastname: Li
authors.forename: Xiaochuan
authors.initials: X
authors.lastname: Wang
authors.forename: Xiangmin
authors.initials: X
authors.lastname: Zhang
authors.forename: Jia
authors.initials: J
authors.lastname: Zeng
mesh_terms: D000096:Acetone / Q000097:blood* / Q000737:chemistry*; D015415:Biomarkers / Q000097:blood; D001774:Blood Chemical Analysis / Q000379:methods*; D003920:Diabetes Mellitus / Q000097:blood* / Q000175:diagnosis; D017022:Flow Injection Analysis / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006898:Hydroxylamines / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D005466:Fluorocarbons
chemical_list: D000096:Acetone; D015415:Biomarkers; D006898:Hydroxylamines; C010277:Florox Reagent; D005466:Fluorocarbons