GC
IndustriesFood & Agriculture
ManufacturerThermo Fisher Scientific
Importance of the topic
In brewing, nonvolatile sulfur amino acids serve as precursors to volatile sulfur compounds that influence beer flavor and aroma. Methionine, a key sulfur amino acid, leads to formation of dimethyl sulfide and other sensory‐active volatiles under certain conditions. Monitoring methionine levels in beer supports quality control and flavor stability.
Objectives and study overview
This study aimed to optimize and validate a gas chromatography method with a selective flame photometric detector for determination of free methionine in retail samples of Czech and foreign beers. A total of 48 beers, including pale lagers, draft beers, dark varieties, nonalcoholic products and imported lagers, were analyzed.
Methodology and instrumentation
Beer samples were defoamed ultrasonically, derivatized with a propanol–pyridine mixture and ethyl chloroformate, and extracted into chloroform. The dried residue was reconstituted in methanol for analysis.
Used instrumentation
- Gas chromatograph Trace GC Ultra (Thermo Finigan, USA)
- Flame photometric detector selective for sulfur (FPD)
- Capillary column RTX-5 (15 m × 0.32 mm i.d., 0.25 μm; 5% diphenyl–95% dimethylpolysiloxane)
- Injector and detector temperatures: 250 °C and 150 °C, respectively
- Temperature program: 100 °C (0.5 min), ramp to 180 °C at 6 °C/min (3 min), ramp to 280 °C at 10 °C/min (1 min)
- Carrier gas: helium at 1.5 mL/min; make-up nitrogen at 20 mL/min
Main results and discussion
Validation yielded LOD 0.80 mg/L, LOQ 2.5 mg/L, linearity R² = 0.99974 and RSD = 13%. In Czech pale lagers, methionine ranged from 3.4 to 12.9 mg/L (notably higher in sample no. 17). Draft beers contained 4.0–6.0 mg/L, dark beers 3.4–6.3 mg/L and nonalcoholic beers 3.4–3.7 mg/L. Among 13 foreign lagers, values of 4.3–20.8 mg/L were found, with the highest in a Danish sample; nine imported beers were below LOQ.
Benefits and practical application of the method
The optimized GC/FPD assay provides sensitive and selective quantification of methionine in complex malt‐ and barley‐derived matrices. It enables brewers to monitor precursor levels linked to off‐flavor formation and supports process optimization and raw material evaluation.
Future trends and possibilities
Future developments may include coupling to mass spectrometry for enhanced specificity, inline or at‐line monitoring during fermentation and maturation, high‐throughput derivatization workflows and extension to multi‐amino‐acid profiling in quality control.
Conclusion
A validated GC/FPD method for methionine determination in beer was established and applied to a diverse set of Czech and foreign products. Methionine levels exhibited variation by beer type and origin, underlining the importance of routine monitoring to manage flavor‐impacting sulfur precursors.
References
- Vodrážka Z. Biochemie. Praha: Academia; 2002.
- Voet D, Voetová J. Biochemie. Praha: Victoria Publishing; 1995.
- Basařová G, Šavel J, Basař P, Lejsek T. Pivovarství teorie a praxe výroby piva. Praha: VŠCHT; 2010.
- Vacek J, Onofrejová L, Klejdus B, Kubáň V. Hydrophilic interaction chromatography for polar analytes. Chem Listy. 2009;103:381–385.
- Langrock T, Czihal P, Hoffmann R. Amino acid analysis by HILIC‐ESI‐MS. Amino Acids. 2006;30:291–297.
- Hušek P. Chloroformates in GC derivatization. J Chrom B. 1998;717:57–91.
- Hušek P, Matucha P, Vránová A, Šimek P. Rapid GC analysis of homocysteine and related compounds. J Chrom B. 2003;789:311–322.
- Myung S et al. Determination of homocysteine by SPME/GC/MSD. J Chrom B. 1999;727:1–8.
- Mayadunne R, Nguyen T-T, Marriott P. AA analysis by comprehensive GC×GC. Anal Bioanal Chem. 2005;382:836–847.
- Erbe T, Brückner H. Amino acid enantiomers in beer by chromatography. J Chrom A. 2000;881:81–91.
- Mikulíková R et al. Determination of methionine in malt. Kvasny Prum. 2009;55:310–314.
- Barek J et al. Metrological terminology in chemistry. Chem Listy. 2000;94:439–444.
- Spectroscopic Society Jan Marek Marci. Uncertainty in spectroscopic methods. 2001.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.