Screen Beer by GC/MS Static Headspace with the Agilent J&W DB-624 Ultra Inert Capillary Column
Applications | 2012 | Agilent TechnologiesInstrumentation
Small‐batch craft brewing has grown in popularity, driving demand for rapid and reliable flavor profiling to monitor fermentation progress, ensure batch quality, and explore novel ingredient effects.
This work demonstrates the application of static headspace GC/MS using Agilent J&W DB-624 Ultra Inert (UI) capillary columns for screening aldehydes, fusel alcohols, esters, and organic acids in complex beer matrices. Key aims were to assess chromatographic inertness and selectivity, compare beer styles (pale ale vs. lager), and benchmark organic acid performance against a competitor’s 624 phase.
Beer samples (pale ale, pilsner) were analyzed neat (≤10% ethanol) in 20 mL headspace vials. Standards were prepared at 2 µL/L (aldehydes, alcohols, acetates) and acids at ng levels via liquid injection.
Instrumentation:
• In SCAN mode at 2 µL/L, all aldehyde, fusel alcohol, and acetate standards matched NIST spectra and exhibited sharp, symmetric peaks, including resolution of positional isomers on the 30 m column.
• Pale ale vs. lager profiles revealed common and unique volatiles; additional esters (e.g., ethyl hexanoate, ethyl octanoate) and organic acids were detected in trace levels.
• Organic acids required liquid injection: the DB-624UI column detected acetic, propionic, butanoic, and octanoic acids at 0.125–1 ng on‐column with minimal tailing.
• Compared to a premium competitor’s 624 phase, the DB-624UI column delivered superior acid recovery and peak shape; the competitor column failed to detect one acid at 1 ng and showed severe tailing.
• High inertness yields reliable, reproducible screening of reactive analytes such as aldehydes and organic acids.
• Comprehensive flavor profiling supports fermentation monitoring, QA/QC, and R&D in brewing.
• Short run times and resolution of isomeric compounds on a 30 m column streamline routine analysis.
• Integration of SIM/SCAN and targeted quantitation for lower detection limits.
• Extension to other fermented beverages and food matrices.
• Development of real‐time monitoring and at‐line process control.
• Exploration of novel stationary phases for enhanced selectivity.
The Agilent J&W DB-624UI GC columns provide exceptional inertness and selectivity for static headspace GC/MS beer profiling. Superior organic acid performance and sharp peak shapes across volatile classes make the DB-624UI the preferred choice for comprehensive flavor analysis in complex beer samples.
GC/MSD, HeadSpace, GC/SQ
IndustriesFood & Agriculture
ManufacturerAgilent Technologies
Summary
Importance of the Topic
Small‐batch craft brewing has grown in popularity, driving demand for rapid and reliable flavor profiling to monitor fermentation progress, ensure batch quality, and explore novel ingredient effects.
Study Objectives and Overview
This work demonstrates the application of static headspace GC/MS using Agilent J&W DB-624 Ultra Inert (UI) capillary columns for screening aldehydes, fusel alcohols, esters, and organic acids in complex beer matrices. Key aims were to assess chromatographic inertness and selectivity, compare beer styles (pale ale vs. lager), and benchmark organic acid performance against a competitor’s 624 phase.
Methodology and Instrumentation Used
Beer samples (pale ale, pilsner) were analyzed neat (≤10% ethanol) in 20 mL headspace vials. Standards were prepared at 2 µL/L (aldehydes, alcohols, acetates) and acids at ng levels via liquid injection.
Instrumentation:
- GC/MS system: Agilent 7890 GC with 5975C MSD (triple‐axis detector), split/splitless inlet, MMI, and FID
- Headspace sampler: Agilent 7697A (111-position tray) and 7693 autosampler
- Columns: DB-624UI 30 m×0.25 mm×1.4 µm for MS; DB-624UI 30 m×0.32 mm×1.8 µm for FID
- Carrier gas: Helium, constant flow (1.8 mL/min MS; 2.6 mL/min FID)
- Temperature program: 35 °C initial, multiple ramps to 250 °C, total run ~32 min
Key Results and Discussion
• In SCAN mode at 2 µL/L, all aldehyde, fusel alcohol, and acetate standards matched NIST spectra and exhibited sharp, symmetric peaks, including resolution of positional isomers on the 30 m column.
• Pale ale vs. lager profiles revealed common and unique volatiles; additional esters (e.g., ethyl hexanoate, ethyl octanoate) and organic acids were detected in trace levels.
• Organic acids required liquid injection: the DB-624UI column detected acetic, propionic, butanoic, and octanoic acids at 0.125–1 ng on‐column with minimal tailing.
• Compared to a premium competitor’s 624 phase, the DB-624UI column delivered superior acid recovery and peak shape; the competitor column failed to detect one acid at 1 ng and showed severe tailing.
Benefits and Practical Applications of the Method
• High inertness yields reliable, reproducible screening of reactive analytes such as aldehydes and organic acids.
• Comprehensive flavor profiling supports fermentation monitoring, QA/QC, and R&D in brewing.
• Short run times and resolution of isomeric compounds on a 30 m column streamline routine analysis.
Future Trends and Potential Uses
• Integration of SIM/SCAN and targeted quantitation for lower detection limits.
• Extension to other fermented beverages and food matrices.
• Development of real‐time monitoring and at‐line process control.
• Exploration of novel stationary phases for enhanced selectivity.
Conclusion
The Agilent J&W DB-624UI GC columns provide exceptional inertness and selectivity for static headspace GC/MS beer profiling. Superior organic acid performance and sharp peak shapes across volatile classes make the DB-624UI the preferred choice for comprehensive flavor analysis in complex beer samples.
References
- Brewers Association, Craft Brewing Statistics. http://www.brewersassociation.org/pages/business-tools/craft-brewing-statistics/facts
- Goldammer T. The Complete Book to Brewing Beer, 2nd Ed. Apex Publishers, 2008.
- Bickham S. Brewing Techniques, 5 (1997).
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