59785-38-5Relevant academic research and scientific papers
QUANTITATIVE MEASUREMENT OF OCTOPAMINES AND SYNEPHRINES IN URINE USING CAPILLARY COLUMN GAS CHROMATOGRAPHY NEGATIVE ION CHEMICAL IONIZATION MASS SPECTROMETRY.
Ibrahim,Couch,Williams,Budd,Yost,Midgley
, p. 1695 - 1699 (1984)
The isomeric octopamines and synephrines were measured in urine by a new assay which combines ion-exchange chromatography, capillary column gas chromatography, and electron capture negative ion chemical ionization mass spectrometry. Deuterium labeled anal
Simultaneous profiling of multiple neurochemical pathways from a single cerebrospinal fluid sample using GC/MS/MS with electron capture detection
Eckstein, James A.,Ammerman, Gina M.,Reveles, Jessica M.,Ackermann, Bradley L.
experimental part, p. 782 - 790 (2009/04/07)
Biogenic amines and amino acids are widely characterized in the pathways representing neurotransmission. Although several analytical methodologies have been used to detect specific target molecules in relevant fluids such as cerebrospinal fluid (CSF), multiple assays must be used to survey the primary pathways involved. This article describes the development of a GC/MS/MS method capable of analyzing up to 43 analytes (representing 20 amino acids and more than seven neurochemical pathways) from a single 50 μl CSF sample. In this procedure, a CSF sample is first treated with acetonitrile to precipitate proteins. The dried sample is then derivatized with a mixture of 2,2,3,3,3-pentafluoro-1-propanol and pentafluoropropionic acetic anhydride to replace all active hydrogen atoms with fluorine-containing groups. Due to the concentration difference between amino acids and neurotransmitters, these two compound classes are analyzed in separate injections of the same derivatized extract. The total run time for each injection is approximately 15-20 min. An essential feature of the method is the use of argon as a reagent gas for electron capture chemical ionization (ECCI), as the use of the more traditional gas (methane) lacked sufficient durability to be considered for use with the present instrumentation. This article describes the development of this method including a detailed investigation of the chemical ionization conditions used. The resultant conditions allow for the profiling of biogenic amines (e.g. serotonin, norepinephrine, and dopamine) in the low picogram per milliliter range. Copyright
Further Studies on a Site-specific Hydrogen Transfer Observed in Electron Capture Negative Ion Chemical Ionization Mass Spectrometry of Hydroxyamine Pentafluoropropionate Derivatives
Low, G. K.-C.,Duffield, A. M.
, p. 595 - 599 (2007/10/02)
Further studies have demonstrated that the site-specific hydrogen transfer process involved in the formation of the m/z 145 anion of β-hydroxyamine pentafluoropropionate (PFP) derivatives observed under electron capture negative ion chemical ionization conditions occurs when the two functional groups are separated by up to five carbon atoms.Deuterium labelling has established that the site specificity, transfer of a hydrogen atom from the carbon adjacent to nitrogen to the OPFP group, is maintained in 4-amino-butan-1-ol-N,O-(PFP)2.The corresponding PFP derivatives of the N-methylaminoalkanol- (PFP)2 derivatives lack the m/z 145 species with m/z 163, -, being the base anion.Substitution of alkyl groups on the carbon adjacent to oxygen results in a diminution of the ion intensity at m/z 145 with a marked increase in the intensity of m/z 144.The formation of the m/z 145 and 144 anions is proposed to proceed through the intervention of a fluoride ion-molecule complex as outlined in Scheme 1 with the product ion distribution dependent on which of the two pathways is preferred.
