Analysis of Biogenic Amines by GC/FID and GC/MS
Low 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 G...
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Virginia Tech
2003
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ftvirginiatec:oai:vtechworks.lib.vt.edu:10919/35027 2024-05-19T07:37:49+00:00 Analysis of Biogenic Amines by GC/FID and GC/MS Nakovich, Laura Chemistry McNair, Harold M. Carlier, Paul R. Taylor, Larry T. 2003-07-16 application/pdf http://hdl.handle.net/10919/35027 http://scholar.lib.vt.edu/theses/available/etd-09122003-131120/ unknown Virginia Tech LN_Thesis.pdf etd-09122003-131120 http://hdl.handle.net/10919/35027 http://scholar.lib.vt.edu/theses/available/etd-09122003-131120/ In Copyright http://rightsstatements.org/vocab/InC/1.0/ Gas Chromatography Mass Spectroscopy Propyl Chloroformate Derivatives Biogenic Amines Thesis 2003 ftvirginiatec 2024-05-01T00:31:23Z Low 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, 1.00m 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. Master of Science Thesis Atlantic salmon VTechWorks (VirginiaTech) |
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VTechWorks (VirginiaTech) |
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ftvirginiatec |
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topic |
Gas Chromatography Mass Spectroscopy Propyl Chloroformate Derivatives Biogenic Amines |
spellingShingle |
Gas Chromatography Mass Spectroscopy Propyl Chloroformate Derivatives Biogenic Amines Nakovich, Laura Analysis of Biogenic Amines by GC/FID and GC/MS |
topic_facet |
Gas Chromatography Mass Spectroscopy Propyl Chloroformate Derivatives Biogenic Amines |
description |
Low 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, 1.00m 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. Master of Science |
author2 |
Chemistry McNair, Harold M. Carlier, Paul R. Taylor, Larry T. |
format |
Thesis |
author |
Nakovich, Laura |
author_facet |
Nakovich, Laura |
author_sort |
Nakovich, Laura |
title |
Analysis of Biogenic Amines by GC/FID and GC/MS |
title_short |
Analysis of Biogenic Amines by GC/FID and GC/MS |
title_full |
Analysis of Biogenic Amines by GC/FID and GC/MS |
title_fullStr |
Analysis of Biogenic Amines by GC/FID and GC/MS |
title_full_unstemmed |
Analysis of Biogenic Amines by GC/FID and GC/MS |
title_sort |
analysis of biogenic amines by gc/fid and gc/ms |
publisher |
Virginia Tech |
publishDate |
2003 |
url |
http://hdl.handle.net/10919/35027 http://scholar.lib.vt.edu/theses/available/etd-09122003-131120/ |
genre |
Atlantic salmon |
genre_facet |
Atlantic salmon |
op_relation |
LN_Thesis.pdf etd-09122003-131120 http://hdl.handle.net/10919/35027 http://scholar.lib.vt.edu/theses/available/etd-09122003-131120/ |
op_rights |
In Copyright http://rightsstatements.org/vocab/InC/1.0/ |
_version_ |
1799477188627529728 |