Gas Chromatography–Mass Spectrometry Method for the Determination of Free Amino Acids as Their Dimethyl-tert-butylsilyl (TBDMS) Derivatives in Animal Source Food

2012 ◽  
Vol 60 (10) ◽  
pp. 2456-2463 ◽  
Author(s):  
Estefanía Jiménez-Martín ◽  
Jorge Ruiz ◽  
Trinidad Pérez-Palacios ◽  
Antonio Silva ◽  
Teresa Antequera
2009 ◽  
Vol 27 (Special Issue 1) ◽  
pp. S417-S420 ◽  
Author(s):  
M. Doležal ◽  
J. Kertisová ◽  
Z. Zelinková ◽  
J. Velíšek

Objective of this work was determination of processing contaminant known as 3-MCPD (3-chloropropane-1,2-diol) in its free and bound form in breads with defined parameters of processing. Selected and analysed were 24 samples, which represented two sets of breads produced in bakeries equipped with a continual line. In all cases determinations were carried out for breadcrumb and crust separately. The first set of samples were wheat-rye breads produced chronologically in ten days in the bakery Michelská pekárna, slightly different in temperatures and times of baking. The second set contained 14 samples of wheat-rye breads with a content of rye flour less than 40% differing in the yeast type and acidity. These breads were produced in the bakery Kontinua. The fat content was determined in all samples by Soxhlet extraction. Free and bound 3-MCPD was determined by gas chromatography–mass spectrometry method. Concentration of free 3-MCPD in samples was at interval < 9–54.5 &mu;g/kg. Concentration of bound 3-MCPD was at interval 1.56–23.60 mg/kg of fat (i.e. 5.7–84.9 &mu;g/kg of sample).


Foods ◽  
2020 ◽  
Vol 9 (1) ◽  
pp. 82 ◽  
Author(s):  
Ángela Alcazar Rueda ◽  
José Marcos Jurado ◽  
Fernando de Pablos ◽  
Manuel León-Camacho

In this paper, the differentiation of three ripening stages, postsalting, drying, and cellar, of Iberian dry-cured ham has been carried out according to their free amino acids contents. Eighteen L-amino acids, alanine, 2-aminobutanoic acid, aspartic acid, cysteine, glutamine, glycine, histidine, hydroxyproline, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tyrosine, and valine have been determined by gas chromatography with derivatization with N,O-bis(trimethylsilyl)-trifluoroacetamide. Gas chromatography–mass spectrometry was used to confirm the presence of the eighteen amino acids in the ham samples, and gas chromatography using a DB-17HT column and flame ionization detector was used for quantitative determination. Extraction with a mixture methanol-acetonitrile has been carried out, achieving recoveries in the range 52–164%. Methimazole was used as internal standard. Limits of detection ranged between 7.0 and 611.7 mg·kg−1. Free amino acids have been used as chemical descriptors to differentiate between the ripening stages. Principal component analysis and linear discriminant analysis have been used as chemometric techniques, achieving complete differentiation between the ripening stages. Alanine, tyrosine, glutamine, proline, 2-aminobutanoic acid, cysteine, and valine were the most differentiating amino acids.


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