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Display Title

A-91: Analysis of selected aldehydes in packaged beer by solid-phase microextraction (SPME)-gas chromatography-negative chemical ionization mass spectrometry (GC-NCIMS)

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R. M. ORTIZ (1); (1) MillerCoors, Milwaukee, WI, U.S.A.

Poster

Unambiguous identification and quantification of certain aldehydes in packaged beer measured at low- to sub-ppb levels is challenging due to the vast number of compounds that can interfere with the measurement of the target aldehydes. This difficulty in resolution has hindered the quantitation and subsequent connection with the sensory data. Successful techniques to overcome the challenges of sensitivity and selectivity have been established, particularly utilizing SPME-GC/electron ionization (EI) MS, derivatization with O-2,3,4,5,6-(pentafluorobenzyl) hydroxylamine hydrochloride (PFBHA), and selected ion monitoring (SIM) at m/z 181. This work builds on earlier methods using this technique to improve both sensitivity and selectivity. Resolution improvement can be achieved by operating the mass spectrometer in the negative chemical ionization (NCI) mode, as opposed to the EI mode: first, by taking advantage of the derivatization reagent PFBHA, which serves to magnify the signal intensity by virtue of the five fluorine atoms accepting the electrons produced from the interaction of the ion filament and the reagent gas methane. This is classified as the electron capture mechanism, often referred to as high-pressure electron-capture mass spectrometry (HPECMS) and is responsible for the increased sensitivity compared to operating in EI mode. Second, the production of characteristic fragment ions inherent to NCI mode results in improved selectivity of the target aldehydes. This is especially useful when attempting to measure aldehydes at the sub-ppb levels. Even at these levels, many aldehydes can impart significant undesirable flavor characteristics. Other aldehydes provide information related to the specific degradation reactions and metric levels surrounding fresh beer profiles. Changes in the levels of these selected aldehydes during controlled storage conditions over time can be used to improve brewing practice’s, make better comparisons with flavor characteristics, and assess ingredient/contact material changes. As an example of this technique and improved analytical method, a fresh batch of lager beer was profiled at selected times over a 17 week period, and changes in target aldehydes were reported.

Roman Ortiz received a B.S. degree in chemistry from California State Polytechnic University in Pomona. He began employment with Miller Brewing Company (now MillerCoors) in 2000 as a quality assurance technician in the production laboratory of the Irwindale, CA, brewery. In 2006 he was promoted to chemist for the analytical laboratory in the Technical Center; in August 2013 he was promoted to senior chemist. He has also served as an ASBC Technical Subcommittee chair (2010–2011).

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