Determination of Organic Acids in Fruit Juices and Wines by High-Pressure IC
Applications | 2013 | Thermo Fisher ScientificInstrumentation
Organic acid profiling in fruit juices and wines is critical for flavor, stability, microbiological control and authenticity testing. Quantitative analysis of individual acids guides quality assurance in production and helps detect adulteration.
This work presents development of a high‐pressure ion chromatography method with suppressed conductivity detection to determine organic acids in fruit juices and wines. Key goals were high resolution of up to 30 inorganic and organic anions, accurate quantitation, and robust authenticity assessment.
The method uses a Thermo Scientific Dionex ICS‐5000+ HPIC system with:
Samples (apple, grape, pomegranate, blueberry juices and Merlot, Chardonnay, White Zinfandel wines) were diluted 1:20, filtered and spiked for recovery studies.
The AS11‐HC‐4 µm column delivered superior peak efficiencies and resolution over the 9 µm version, especially for closely eluting pairs (acetate/glycolate, succinate/malate, malonate/tartrate, fumarate/oxalate). Calibration for galacturonate, malate, tartrate and citrate showed quadratic fits (r2 > 0.999) over 1–500 mg/L, limits of detection 0.036–0.069 mg/L and quantitation 0.12–0.23 mg/L. Typical reproducibility was <4 % RSD in peak area and <0.04 % in retention time. Authenticity markers such as low tartaric acid in pure pomegranate juice and presence of galacturonic and quinic acids in apple and blueberry blends were demonstrated. Wine profiles reflected fermentation acids (lactic, succinic) and grape acids (tartaric, malic) in characteristic ratios.
Advances may include coupling with mass spectrometry for structural confirmation, further miniaturization and automation for on‐line process monitoring, rapid screening kits for field testing, and expansion to other food and environmental matrices.
The validated IC method using the AS11‐HC‐4 µm column and suppressed conductivity detection enables high‐resolution, sensitive and reproducible determination of organic acids in fruit juices and wines, supporting quality control and authenticity verification.
Ion chromatography
IndustriesFood & Agriculture
ManufacturerThermo Fisher Scientific
Summary
Importance of the Topic
Organic acid profiling in fruit juices and wines is critical for flavor, stability, microbiological control and authenticity testing. Quantitative analysis of individual acids guides quality assurance in production and helps detect adulteration.
Objectives and Study Overview
This work presents development of a high‐pressure ion chromatography method with suppressed conductivity detection to determine organic acids in fruit juices and wines. Key goals were high resolution of up to 30 inorganic and organic anions, accurate quantitation, and robust authenticity assessment.
Methodology and Instrumentation
The method uses a Thermo Scientific Dionex ICS‐5000+ HPIC system with:
- IonPac AS11‐HC‐4 µm guard and analytical columns
- EGC 500 KOH eluent generator cartridge and CR‐ATC 500 anion trap column
- ASRS 300 self‐regenerating suppressor operated in external water mode
- Suppressed conductivity detection
- Hydroxide gradient elution with 1–60 mM KOH and 7–11 % methanol
- Flow rate 0.4 mL/min, injection volume 2.5 µL
Samples (apple, grape, pomegranate, blueberry juices and Merlot, Chardonnay, White Zinfandel wines) were diluted 1:20, filtered and spiked for recovery studies.
Main Results and Discussion
The AS11‐HC‐4 µm column delivered superior peak efficiencies and resolution over the 9 µm version, especially for closely eluting pairs (acetate/glycolate, succinate/malate, malonate/tartrate, fumarate/oxalate). Calibration for galacturonate, malate, tartrate and citrate showed quadratic fits (r2 > 0.999) over 1–500 mg/L, limits of detection 0.036–0.069 mg/L and quantitation 0.12–0.23 mg/L. Typical reproducibility was <4 % RSD in peak area and <0.04 % in retention time. Authenticity markers such as low tartaric acid in pure pomegranate juice and presence of galacturonic and quinic acids in apple and blueberry blends were demonstrated. Wine profiles reflected fermentation acids (lactic, succinic) and grape acids (tartaric, malic) in characteristic ratios.
Advantages and Practical Applications of the Method
- High sensitivity for low UV‐absorbing acids without derivatization
- Minimal sample preparation and rapid throughput
- Wide dynamic range for multiple acids in a single run
- Robust authenticity testing and quality monitoring in beverage industry
Future Trends and Applications
Advances may include coupling with mass spectrometry for structural confirmation, further miniaturization and automation for on‐line process monitoring, rapid screening kits for field testing, and expansion to other food and environmental matrices.
Conclusion
The validated IC method using the AS11‐HC‐4 µm column and suppressed conductivity detection enables high‐resolution, sensitive and reproducible determination of organic acids in fruit juices and wines, supporting quality control and authenticity verification.
Reference
- Mato I Suárez-Luque S Huidobro JF A review of the analytical methods to determine organic acids in grape juices and wines Food Res Int 2005 38 1175-1188
- Ehling S Cole S Analysis of organic acids in fruit juices by LC-MS as an enhanced tool for authenticity testing J Agric Food Chem 2011 59 2229-2234
- Kiss J Sass-Kiss A Protection of originality of Tokaji Aszú by amines and organic acids in botrytized wines by HPLC J Agric Food Chem 2005 53 10042-10050
- Hajós P Nagy L Retention behaviors and separation of carboxylic acids by ion-exchange chromatography J Chromatogr B 1998 717 27-38
- Masson P Influence of organic solvents on determination of carboxylic acids and inorganic anions in grape juice by IC J Chromatogr A 2000 881 387-394
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- Tezcan F Gültekin-Özgüven M Diken T Özçelik B Erim FB Antioxidant activity and total phenolic organic acid and sugar content in commercial pomegranate juices Food Chem 2009 115 873-877
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- Fuleki T Pelayo E Palabay RB Carboxylic acid composition of varietal juices from fresh and stored apples J Agric Food Chem 1995 43 598-607
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- Dionex Application Note 143 Determination of organic acids in fruit juices Sunnyvale CA 2003
- Dionex Application Note 273 Higher resolution separation of organic acids and common inorganic anions in wine Sunnyvale CA 2011
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