Determination of Total Inorganic Arsenic in Fruit Juice Using High-Pressure Capillary Ion Chromatography
Applications | 2016 | Thermo Fisher ScientificInstrumentation
The accurate determination of total inorganic arsenic in fruit juices is vital to ensure consumer safety and compliance with regulatory standards. While organic arsenic species pose lower toxicity, inorganic forms such as arsenate (As(V)) and arsenite (As(III)) are highly toxic. Concerns over arsenic levels in apple juice have heightened due to media reports, although regulatory agencies report typical levels well below limits. A robust analytical approach is therefore needed to selectively determine total inorganic arsenic and profile acid content in complex juice matrices.
This study demonstrates the development and validation of a high-pressure capillary ion chromatography (HPIC) method with suppressed conductivity detection for simultaneous separation of 27 organic and inorganic anions and quantification of total inorganic arsenic in fruit juices. Key aims include optimizing chromatographic conditions, establishing detection limits for arsenic species, and applying the method to a variety of commercial juice samples.
Using a Dionex ICS-5000+ HPIC system equipped with capillary pumps, an EGC−KOH eluent generator cartridge, and an ACES 300 anion capillary suppressor, separation was achieved on a Thermo Scientific Dionex IonPac AS11-HC-4µm column (0.4 × 250 mm) at 30 °C. A potassium hydroxide gradient (1.5 to 65 mM) was delivered at 0.015 mL/min. Juice samples were filtered (0.20 µm), diluted 50-fold, and spiked with arsenate. Calibration standards ranged from 0.2 to 100 mg/L arsenate.
The method resolved 27 target anions in under 40 minutes, with arsenate eluting at approximately 32.9 minutes. Calibration yielded a linear response (r² = 0.9996) for arsenate from 0.2 to 100 mg/L. Limits of detection and quantification for arsenate were 0.026 and 0.088 mg/L, respectively, corresponding to 0.014 and 0.047 mg/L total inorganic arsenic. Arsenite injected as As(III) converted quantitatively to As(V) under the basic gradient conditions, enabling total inorganic arsenic measurement as arsenate. Among tested juices, only apple juices contained detectable arsenate levels.
Advancements may include coupling capillary HPIC to mass spectrometry for enhanced sensitivity and speciation, further miniaturization for field-portable analysis, integration with greener chromatographic techniques to minimize reagent use, and expanding the method to other food, environmental, and clinical matrices. Automation and high-throughput screening could streamline quality control in the food and beverage industry.
The developed capillary IC method with suppressed conductivity detection provides a robust, sensitive, and efficient approach for determining total inorganic arsenic in fruit juices while delivering comprehensive organic acid profiles. Its performance meets regulatory requirements, offering a valuable tool for both routine monitoring and research applications.
Ion chromatography
IndustriesFood & Agriculture
ManufacturerThermo Fisher Scientific
Summary
Significance of the topic
The accurate determination of total inorganic arsenic in fruit juices is vital to ensure consumer safety and compliance with regulatory standards. While organic arsenic species pose lower toxicity, inorganic forms such as arsenate (As(V)) and arsenite (As(III)) are highly toxic. Concerns over arsenic levels in apple juice have heightened due to media reports, although regulatory agencies report typical levels well below limits. A robust analytical approach is therefore needed to selectively determine total inorganic arsenic and profile acid content in complex juice matrices.
Objectives and Study Overview
This study demonstrates the development and validation of a high-pressure capillary ion chromatography (HPIC) method with suppressed conductivity detection for simultaneous separation of 27 organic and inorganic anions and quantification of total inorganic arsenic in fruit juices. Key aims include optimizing chromatographic conditions, establishing detection limits for arsenic species, and applying the method to a variety of commercial juice samples.
Methodology and Instrumentation
Using a Dionex ICS-5000+ HPIC system equipped with capillary pumps, an EGC−KOH eluent generator cartridge, and an ACES 300 anion capillary suppressor, separation was achieved on a Thermo Scientific Dionex IonPac AS11-HC-4µm column (0.4 × 250 mm) at 30 °C. A potassium hydroxide gradient (1.5 to 65 mM) was delivered at 0.015 mL/min. Juice samples were filtered (0.20 µm), diluted 50-fold, and spiked with arsenate. Calibration standards ranged from 0.2 to 100 mg/L arsenate.
Used Instrumentation
- Dionex ICS-5000+ HPIC system with DC and DP modules
- Thermo Scientific IonPac AS11-HC-4µm capillary column
- EGC-KOH capillary eluent generator cartridge
- ACES 300 capillary anion electrolytic suppressor
- Thermo Scientific Dionex Chromeleon 7.2 CDS software
Main Results and Discussion
The method resolved 27 target anions in under 40 minutes, with arsenate eluting at approximately 32.9 minutes. Calibration yielded a linear response (r² = 0.9996) for arsenate from 0.2 to 100 mg/L. Limits of detection and quantification for arsenate were 0.026 and 0.088 mg/L, respectively, corresponding to 0.014 and 0.047 mg/L total inorganic arsenic. Arsenite injected as As(III) converted quantitatively to As(V) under the basic gradient conditions, enabling total inorganic arsenic measurement as arsenate. Among tested juices, only apple juices contained detectable arsenate levels.
Benefits and Practical Applications
- Simultaneous profiling of organic acids and total inorganic arsenic in a single run
- Reduced eluent consumption through capillary format
- High-resolution separation with 4 µm particles under high pressure
- Detection limits suitable for regulatory monitoring of arsenic in beverages
Future Trends and Potential Applications
Advancements may include coupling capillary HPIC to mass spectrometry for enhanced sensitivity and speciation, further miniaturization for field-portable analysis, integration with greener chromatographic techniques to minimize reagent use, and expanding the method to other food, environmental, and clinical matrices. Automation and high-throughput screening could streamline quality control in the food and beverage industry.
Conclusion
The developed capillary IC method with suppressed conductivity detection provides a robust, sensitive, and efficient approach for determining total inorganic arsenic in fruit juices while delivering comprehensive organic acid profiles. Its performance meets regulatory requirements, offering a valuable tool for both routine monitoring and research applications.
References
- Segura M, Muñoz J, Madrid Y, Cámara C. Transformation of Inorganic Arsenic Species in Varied pH Conditions. Anal Bioanal Chem. 2002;374:513–519.
- Thermo Fisher Scientific. Dionex ICS-5000+ System Installation Manual. Doc No. 065447. Sunnyvale, CA; 2012.
- Thermo Fisher Scientific. TN 131: Configuring High-Pressure Capillary IC on the Modular IC System. TN70352_E. Sunnyvale, CA; 2013.
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