Determination of 3-hydroxy-2-butanone (acetoin) in beer.
The method is suitable for beers of brewed to any original gravity or of any alcohol content.
The compound 3-hydroxy-2-butanone (acetoin) is derived from diacetyl and is created through the reductive activity of yeast. One further reaction mechanism for the formation of 3-hydroxy-2-butanone is condensation of both free and activated (bound to thiamine pyrophosphate [TPP]) acetaldehyde.
3-Hydroxybutanone is oxidized to 2,3-butanedione (diacetyl) by iron chloride in the presence of iron sulfate and determined using gas chromatography and the headspace analysis method.
Malt intended for use in beer brewing or elsewhere in the food industry
A (modified) Congress wort is produced from malt samples prior to analysis. NDMA present in the Congress wort is extracted using dichloromethane followed by concentration of the eluate. The determination is performed with a gas chromatograph using a packed Carbowax 20M column with a specific TEA detector (thermal energy analyzer); nitrosodipropylamine (NDPA) serves as an internal standard.
This detector analyzes nitrosamine according to the following procedure:
After exiting the GC column, the separated substances are heated to 500 °C in a pyrolyzer. At this temperature, the N-NO bond of the nitrosamine is broken, thus forming an NO radical (NO۰):
The gas mixture then flows through a special filter (CTRTM gas stream filter), which only allows the carrier gas and the NO radicals to pass. After exiting the filter, the NO radicals flow into a reaction chamber along with ozone, which is created by a special generator. The following chemical reactions take place in the chamber:
|
NO• + O3 |
→ |
NO2• |
|
NO2• |
→ |
NO2 + h•ν |
These NO radicals react with ozone, forming nitrogen dioxide in an excited state (NO2•). The NO2• molecules decompose spontaneously to form nitrogen dioxide in its common form (NO2), emitting radiation (h•ν) with a wavelength of approx. 600 nm.