Determination of Organic Acids in Beer Samples Using a High-Pressure Ion Chromatography System
Applications | 2016 | Thermo Fisher ScientificInstrumentation
Beer is a complex sample matrix containing proteins, carbohydrates, inorganic ions, organic acids and ethanol. Accurate profiling of organic acids is essential for quality control, flavour optimization and detection of microbial spoilage in beer production.
This technical note demonstrates the use of a 4 µm resin anion-exchange column (Dionex IonPac AS11-HC-4µm) combined with a high-pressure ion chromatography system (Dionex ICS-5000+ HPIC). The goals are to achieve high-resolution separation of organic acids and inorganic anions in beer and to compare performance with a 9 µm particle column format, as well as to explore selectivity adjustments using methanol modifiers.
The integration of a 4 µm AS11-HC column with a high-pressure IC system delivers superior separation efficiency, selectivity and operational robustness for organic acid analysis in beer, enhancing quality control and research capabilities.
Ion chromatography
IndustriesFood & Agriculture
ManufacturerThermo Fisher Scientific
Summary
Importance of the Topic
Beer is a complex sample matrix containing proteins, carbohydrates, inorganic ions, organic acids and ethanol. Accurate profiling of organic acids is essential for quality control, flavour optimization and detection of microbial spoilage in beer production.
Objectives and Study Overview
This technical note demonstrates the use of a 4 µm resin anion-exchange column (Dionex IonPac AS11-HC-4µm) combined with a high-pressure ion chromatography system (Dionex ICS-5000+ HPIC). The goals are to achieve high-resolution separation of organic acids and inorganic anions in beer and to compare performance with a 9 µm particle column format, as well as to explore selectivity adjustments using methanol modifiers.
Applied Methodology and Instrumentation
- Sample preparation: degassing by vacuum filtration with ultrasonic agitation, five-fold dilution and 0.20 µm syringe filtration.
- Eluent: electrolytically generated potassium hydroxide gradient (1–60 mM) with optional methanol modifier (2–20%).
- Columns: Dionex IonPac AS11-HC-4µm (4 × 250 mm and 2 × 250 mm) with guard columns.
- System configuration: Thermo Scientific Dionex ICS-5000+ HPIC with SP/DP pump, EG eluent generator, high-pressure degasser, autosampler and Chromeleon CDS.
- Detection: suppressed conductivity using AERS/ASRS suppressors in recycle or external water mode.
Main Results and Discussion
- The 4 µm column delivered 40–50 % higher resolution than a 9 µm column, enabling baseline separation of 40 analytes within 45 min at 0.38 mL/min.
- Critical peak pairs such as lactate/acetate and phosphate/phthalate showed resolution improvements from Rs ≈ 1.2 to Rs > 1.9.
- Methanol addition modified column selectivity, reversing elution order and resolving coeluting species like succinate and malate.
- Analysis of U.S. lager beers revealed distinct organic acid profiles, with variations in chloride, phosphate, citrate, pyruvate and sulfate reflecting brewing ingredient choices and processes.
- Spiked sample testing confirmed the method’s ability to detect spoilage markers (for example, butyrate) in complex beer matrices.
Benefits and Practical Applications of the Method
- High resolution and capacity for complex beer samples.
- Improved signal-to-noise and quantitation accuracy from smaller particle size.
- Adjustable selectivity through organic modifiers for targeted analyte separation.
- Consistent performance across column formats (4 mm, 2 mm and capillary) on HPIC platforms.
- Ideal for routine QA/QC, research and industrial beverage analysis.
Future Trends and Applications
- Adoption of capillary column formats to reduce solvent consumption and enhance sensitivity.
- Coupling with mass spectrometry for structural confirmation of unknown acids.
- Automation of sample preparation and data processing for high-throughput brewery quality control.
- Development of advanced stationary phases for isomeric organic acid separation.
- Extension of the approach to other fermented beverages and food quality monitoring.
Conclusion
The integration of a 4 µm AS11-HC column with a high-pressure IC system delivers superior separation efficiency, selectivity and operational robustness for organic acid analysis in beer, enhancing quality control and research capabilities.
References
- Papazian C. The Complete Joy of Home Brewing. Avon Books, New York, 1983.
- Thermo Fisher Scientific. Application Note 46 Ion Chromatography A Versatile Technique for the Analysis of Beer LPN 0661, Sunnyvale CA, 1997.
- Robinett RSR George HA Herber WK. J Chrom A. 1995;718:319–327.
- Hanko VP Rohrer JS. Anal Biochem. 2000;283:192–199.
- Christison TT De Borba B Rohrer JS. Am Biotechnol Lab. 2009;27(2):13–17.
- Thermo Fisher Scientific. Eluent Generator Cartridges Product Manual PN 065018, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. Continuously Regenerated Trap Columns Product Manual Doc 031910, Sunnyvale CA, 2010.
- Thermo Fisher Scientific. ERS 500 Suppressor Product Manual Doc 031956, Sunnyvale CA, 2013.
- Thermo Scientific Dionex IonPac AS11-HC-4µm Hydroxide Selective Anion Exchange Column Manual LPN 65463, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. TN 129 Configuring High Pressure IC Systems for Analytical Flow Rates TN70317, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. Dionex ICS 5000 Installation Instructions Doc 065447, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. Dionex AS-AP Operator’s Manual Doc 065361, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. Application Note 143 Determination of Organic Acids in Fruit Juices LPN 1415, Sunnyvale CA, 2003.
- Thermo Fisher Scientific. Application Note 182 Determination of Biogenic Amines in Alcoholic Beverages LPN 1888-02, Sunnyvale CA, 2007.
- Thermo Fisher Scientific. Application Note 273 Higher Resolution Separation of Organic Acids and Common Inorganic Anions in Wine LPN 2727, Sunnyvale CA, 2011.
- Thermo Fisher Scientific. Application Brief 117 Determination of Cations in Fruit Juices LPN 2605, Sunnyvale CA, 2010.
- Thermo Fisher Scientific. Application Brief 127 Determination of Carbohydrates in Fruit Juice Using Capillary High Performance Anion Exchange Chromatography AB70465, Sunnyvale CA, 2012.
- Thermo Fisher Scientific. Application Brief 135 Determination of Anions and Organic Acids in Coffee Samples Using Capillary IC AB70455, Sunnyvale CA, 2012.
- Christison T Pang F Lopez L. Technical Note 119 Fast Separations of Organic Acids in an Orange Juice Sample Using High Pressure Capillary IC TN70168, Sunnyvale CA, 2013.
- Christison T Pang F Lopez L. Technical Note 118 Fast Separations of Anions and Organic Acids in a Carbonated Beverage Using High Pressure Capillary IC TN70167, Sunnyvale CA, 2013.
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