Analysis of Biogenic Amines by GC/FID and GC/MS

dc.contributor.authorNakovich, Lauraen
dc.contributor.committeechairMcNair, Harold M.en
dc.contributor.committeememberCarlier, Paul R.en
dc.contributor.committeememberTaylor, Larry T.en
dc.contributor.departmentChemistryen
dc.date.accessioned2014-03-14T20:45:18Zen
dc.date.adate2003-09-18en
dc.date.available2014-03-14T20:45:18Zen
dc.date.issued2003-07-16en
dc.date.rdate2003-09-18en
dc.date.sdate2003-09-12en
dc.description.abstractLow levels of biogenic amines occur naturally, but high levels (FDA sets 50 ppm of histamine in fish as the maximum allowable level) can lead to scombroid poisoning. Amines in general are difficult to analyze by Gas Chromatography (GC) due to their lack of volatility and their interaction with the GC column, often leading to significant tailing and poor reproducibility. Biogenic amines need to be derivatized before both GC and HPLC analyses. The objective of this research was to develop a relatively fast, reproducible method to derivatize and quantitate biogenic amines in fish at trace levels using GC/FID. The derivatizing reagent used in the experiments was propyl chloroformate, useful for aqueous samples. To confirm the identity of six derivatized biogenic amines GC/MS was used. To our knowledge no reference spectra for these derivatives has been published. It was concluded that best results are obtained using a Cold-On-Column (C.O.C.) inlet with a short column (15 meters), thick film stationary phase (ZB-5, 1.00μm df), and with recommendations to cut 40 cm from the inlet end of the column every 25 injections when using C.O.C. Duplicate samples of Atlantic Salmon were analyzed on days 0, 3, and 5. Levels of histamine were below 50 ppm for days 0 and 3, but day 5 showed average levels of 160 pm (cadaverine), 1000 ppm (histamine), and 350 ppm (tyramine). Good precision of six amine stardards at 50 ppm was shown: heptylamine 5.2%, putrescine 5.6%, cadaverine 5.0%, histamine 9.9%, tyramine 5.1%, and spermidine 6.2% RSD.en
dc.description.degreeMaster of Scienceen
dc.identifier.otheretd-09122003-131120en
dc.identifier.sourceurlhttp://scholar.lib.vt.edu/theses/available/etd-09122003-131120/en
dc.identifier.urihttp://hdl.handle.net/10919/35027en
dc.publisherVirginia Techen
dc.relation.haspartLN_Thesis.pdfen
dc.rightsIn Copyrighten
dc.rights.urihttp://rightsstatements.org/vocab/InC/1.0/en
dc.subjectGas Chromatographyen
dc.subjectMass Spectroscopyen
dc.subjectPropyl Chloroformate Derivativesen
dc.subjectBiogenic Aminesen
dc.titleAnalysis of Biogenic Amines by GC/FID and GC/MSen
dc.typeThesisen
thesis.degree.disciplineChemistryen
thesis.degree.grantorVirginia Polytechnic Institute and State Universityen
thesis.degree.levelmastersen
thesis.degree.nameMaster of Scienceen

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