Analyses of Fish Tissue by Vacuum Distillation/Gas Chromatography/Mass Spectrometry

1997 ◽  
Vol 69 (6) ◽  
pp. 1127-1134 ◽  
Author(s):  
Michael H. Hiatt
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Vacuum Distillation ◽  
Fish Tissue ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

scholarly journals Rapid Determination and Confirmation of Biogenic Amines in Tuna Loin by Gas Chromatography/Mass Spectrometry Using Ethylchloroformate Derivative

2006 ◽  
Vol 89 (6) ◽  
pp. 1591-1599 ◽  
Author(s):  
Heidi S Marks (Rupp) ◽  
Collin R Anderson
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Biogenic Amines ◽  
Rapid Determination ◽  
Fish Tissue ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Trichloroacetic Acid Solution ◽  
Fresh Frozen ◽  
Peak Areas

Abstract A gas chromatography-mass spectrometry (GC/MS) method is described for the easy rapid determination and simultaneous confirmation of the biogenic amines putrescine (PUT), cadaverine (CAD), histamine (HTA), and spermidine (SPD) in fresh frozen tuna loin. The method can also be used to monitor tyramine (TYR). The method involves homogenization of fish tissue, extraction of biogenic amines into trichloroacetic acid solution, centrifugation, alkalization, and derivatization of supernatant with ethylchloroformate. All seafood species were fortified to contain 2.5, 5.0, 10.0, 12.5, and 25.0 μg/g (ppm) PUT, CAD, and SPD; and 10.0, 20.0, 40.0, 50.0, and 100.0 μg/g (ppm) HTA. Determination was based on standard curves for each analyte using peak areas with matrix standards equivalent to a concentration range bracketing the spike level. A set of 5 matrix controls (unfortified tuna tissue) was also analyzed; only endogenous SPD was found in all samples. The interassay average recoveries ranged from 57 to 79% across analytes and spike levels.

scholarly journals Development and Validation of a Gas Chromatography/Mass Spectrometry Procedure for Confirmation of Para-Toluenesulfonamide in Edible Fish Fillet Tissue

2004 ◽  
Vol 87 (5) ◽  
pp. 1098-1108 ◽  
Author(s):  
Olutosin R Idowu ◽  
Philip J Kijak ◽  
Jeffery R Meinertz ◽  
Larry J Schmidt
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Solution ◽  
Gas Chromatography ◽  
Methylene Chloride ◽  
Fish Tissue ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Chloramine T ◽  
Development And Validation ◽  
Edible Fish

Abstract Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb.

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