Simultaneous GC-MS quantitation of o-phosphoric, aliphatic and aromatic carboxylic acids, proline, hydroxymethylfurfurol and sugars as their TMS derivatives: In honeys

Abstract

SummaryA GC-MS procedure is described for the simultaneous quantitatation of the minor and major constituents of honeys, as their trimethylsilyl derivatives, from one solution, by one injection. Selected minor components (aliphatic and aromatic carboxylic acids, members of various homologous series, together with o-phosphoric acid, proline and hydroxymethylfurfurol), have been determined on the basis of their characteristic fragment ions, in the presence of extremely high excess of honeysaccharides. Selective fragmentation of these minor compounds in the ion trap detector provided possibilities for distinguishing them. The method permitted the simultaneous quantitation of o-phosphoric, malic, shikimic, citric/isocitric, quinic, margaric, oleic and stearic acids, hydroxymethylfurfurol and proline with the extremely high sugar contents of honeys (fructose, glucose, galacturonic acid, inositol, sucrose, trehalose, turanose, maltose, gentiobiose, isomaltose, raffinose, erlose, melezitose, maltotriose, panose, isomaltotriose) and allowed the fast evaluation of sugar and acid constituents of fifteen honeys from various floral and geological origin. Results revealed that (i) the minor components varied in the concentration range of 0.0001 to 0.43 %, and, (ii) together with the saccharides of honeys made up the total of identified and determined constituents from 87.8 % to 98.5 %. Quantitative evaluation of Presented at: Balaton Symposium on High-Performance Separation Methods, Si6fok, Hungary, September 3-5, 1997 the minor constituents was performed on the basis of their selective fragment ion values with an average reproducibility of 6.7 % (RSD).

Carbohydrate composition and physico chemical properties of artisanal honeys from Madrid (Spain): occurrence of Echium sp honey

“…The studied honey samples always presented α,β-trehalose in higher amounts than α,α-trehalose. Although α,β-trehalose was isolated from honey by crystallisation 43 and detected by HPLC, 44 previous analyses by GC 17,18,25,45,46 only described the presence of α,α-trehalose but not that of its α,β isomer. GC retention data relative to sucrose were, in our conditions, 1.069 for α,α-trehalose and 1.086 for α,β-trehalose.…”

Determination of Impurities in Bioproduced Succinic Acid

“…Most of these studies characterize food products, focusing on relevant species occurring in fairly high concentration [4][5][6][7][8][9][16][17][18]. To our knowledge, no shortchain (i.e., highly volatile) monocarboxylic acids were reported.…”

“…The most common approach is derivatization with hydroxylamine in pyridine in combination with hexamethyldisilazane (HMDS) with trifluoroacetic acid [5][6][8][9][10], where hydroxylamine reacts with the saccharide carbonyl group while HMDS functionalizes the moiety containing a reactive hydrogen atom, i.e., carboxyl, hydroxyl and phenyl groups. However, the use of two derivatization agents may lead to uncertainties as the optimal conditions for two different derivatizations may not match.…”

“…Numerous studies addressing acids, saccharides and polyalcohols were performed using GC-MS with trimethylsilylation [5][6][7][8][9][10][11][12][13][14][15][16][17][18][19] (Supplemental Table S.1 for their overview). Most of these studies characterize food products, focusing on relevant species occurring in fairly high concentration [4][5][6][7][8][9][16][17][18].…”

Identification, quantification and carbon stable isotopes determinations of organic acids in monofloral honeys. A powerful tool for botanical and authenticity control

“…Many other acids are also present in much lower quantities, most of them originating from bees. [24][25][26][27] All these acids confer a relatively acidic pH for honey, between 3.2 and 6.1. [28] The aim of this work was to characterize honeys of different botanical origins using data from isotopic and chromatographic analyses of organic acids, in order to replace proteins as internal standard.…”