Headspace solid-phase microextraction and gas chromatographic analysis of low-molecular-weight sulfur volatiles with pulsed flame photometric detection and quantification by a stable isotope dilution assay

2017 ◽  
Vol 41 (4) ◽  
pp. 899-909 ◽  
Author(s):  
Sebastian Ullrich ◽  
Sylvia K. Neef ◽  
Hans-Georg Schmarr
2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Christian Philipp ◽  
Phillip Eder ◽  
Walter Brandes ◽  
Elsa Patzl-Fischerleitner ◽  
Reinhard Eder

The perceived pear aroma in wines was associated with various short- and medium-chain ester compounds. A consumer study confirmed this assumption. In total, eight ester compounds from a series of 100 aromatic substances were associated with the pear aroma. In this study, a valid stable isotope dilution assay headspace solid-phase microextraction gas chromatography mass spectroscopy (SIDA-HS-SPME-GC-MS) method was developed for the analysis of these compounds, and 102 Austrian Pinot blanc wines of vintages 2013–2016 were analysed. They were assessed with regard to vintage and origin influences as well as wine styles. However, an attempt was made to capture the synergies of these compounds for the pear aroma. With the detection of ethyl (E,Z)-2,4-decadienoate and methyl (E)-geranoate, two volatile compounds were measured which had not previously been detected in Austrian wines. The eight analysed esters were perceived very differently. Therefore, specific odour activity values for the various sensations could be calculated with a mathematical combination of the analyses and the results of the sensory studies. A vintage influence on the sensorial descriptor “overripe pear” and a relationship between wine style and total pear aroma were determined.


2020 ◽  
Vol 412 (26) ◽  
pp. 7237-7252
Author(s):  
Thomas Bachmann ◽  
Andrea Maurer ◽  
Michael Rychlik

Abstract Vitamin B6 comprises an important set of molecules tightly interwoven with the human amino acid, fatty acid, and carbohydrate metabolism. Analytical methods striving for the quantification of individual B6 vitamers so far mostly rely on methods based on HPLC in combination with fluorescence detection, but their application encounters multiple difficulties due to the chemical divergence of the single vitamers. The present study describes the development of a method based on LC-MS/MS and stable isotope dilution assay (SIDA) for the simultaneous quantification of five vitamers (PN, PL, PM, PMP, and PNG) of the B6 group in food samples. [13C3]-PN, [13C3]-PL, and [13C6]-PNG were applied as internal standards for the analysis of PN, PL, and PNG. PM and PMP were quantified via matrix-matched calibration referring to [13C3]-PN. The developed method was validated using starch matrix. The limits of detection and quantification ranged from 0.0028 to 0.02 mg/kg and from 0.0085 to 0.059 mg/kg, respectively, for all analytes. Calculated recoveries varied from 92 to 111%. Intra-injection precisions ranged from 0 to 9%, inter-day precisions from 4 to 10%, and intra-day precisions from 4 to 10%. A total of 14 plant-based food samples including fruits, vegetables, and cereals were examined for their content of vitamin B6 using the validated method. Furthermore, the first quantitation of PNG without enzymatic steps or divergent internal standards was undertaken utilizing LC-MS/MS and SIDA.


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