Determination of Sucralose Using HPAE-PAD

Significance of the Topic

Objectives and Study Overview

Methodology and Instrumentation

• System: Dionex BioLC with GP50 microbore pump, AS50 autosampler in thermal compartment and ED50 electrochemical detector.
• Column: CarboPac PA20 analytical column with guard.
• Detection: Pulsed amperometric detection using disposable gold working electrodes; carbohydrate waveform (alternative AAA-Direct waveform for enhanced sensitivity).
• Eluents: Water (A), 40–250 mM NaOH (B), 75–800 mM sodium acetate (C). Both isocratic (40 mM NaOH + 75 mM acetate) and gradient methods were optimized.
• Sample prep: 10 mg/mL sucralose stock in water; Diet Rite diluted 50-fold; Splenda dissolved to 100 mg/mL, diluted to 100 µg/mL.

Main Results and Discussion

• Linearity: Peak area response linear from 1.24 to 250 pmol (r² ≥ 0.9958), extending to 1000 pmol within 20% variance.
• Sensitivity: LOD of 0.28 pmol (0.01 µM) and LOQ of 0.93 pmol (0.04 µM) for a 25 µL injection.
• Precision: Retention time RSD 0.7–1.2% and peak area RSD 2.4–3.0% over seven days (836 injections) with periodic column washes.
• Recovery: Spike recoveries of 92–96% for sucralose in diluted Diet Rite across multiple dilution levels.
• Sample quantification: Sucralose at 155 µg/mL (390 µM) in Diet Rite; in Splenda, sucralose was 1.4% w/w and dextrose 85% w/w.
• Gradient method enabled simultaneous dextrose and sucralose separation, with system peaks identified and excluded from quantification.

Benefits and Practical Applications

• High specificity for oxidizable sweeteners in complex matrices.
• Broad dynamic range covering trace to high concentrations.
• Minimal interference from non-oxidizable components.
• Robustness and reproducibility suitable for routine quality control in food and beverage analysis.

Future Trends and Applications

• Coupling HPAE-PAD with mass spectrometry for confirmatory analyses.
• Development of miniaturized, high-throughput platforms for regulatory screening.
• Advances in electrode materials and pulsed waveforms to enhance sensitivity and electrode lifespan.
• Extension to emerging sweetener analogues and diverse food matrices such as dairy and pharmaceuticals.

Conclusion

References

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