Determination of Elemental Nutrients and Micronutrients in Functional Foods by ICP-OES

Význam tématu

Functional foods enriched with vitamins and minerals play an increasingly important role in modern nutrition. Accurate quantification of essential macro- and micronutrients supports proper labeling, regulatory compliance, and consumer confidence in product quality and safety. Analytical methods capable of handling complex food matrices, delivering low detection limits, and providing high throughput are critical for routine testing in food and supplement laboratories.

Cíle a přehled studie

This study adapts the US FDA Elemental Analysis Manual (EAM) 4.4 method for functional food analysis using the Agilent 5900 Synchronous Vertical Dual View (SVDV) ICP-OES. The primary objectives are to develop a robust procedure for simultaneous determination of Ca, Cu, Fe, K, Mg, Mn, Na, P, and Zn in elderberry-based supplements; to verify method accuracy; and to demonstrate high productivity using advanced software tools.

Použitá metodika a instrumentace

Sample Preparation:

• Three commercial elderberry products (natural syrup, effervescent tablet, syrup with additives) and NIST 2385 Slurried Spinach SRM.
• Microwave digestion: 0.5 g sample, 8 mL HNO₃, 1 mL H₂O₂; ramp to 200 °C over 25 min, hold 15 min; dilute to 50 mL.

Instrumentation and Software:

• Agilent 5900 SVDV ICP-OES with SPS 4 autosampler, SeaSpray nebulizer, cyclonic spray chamber, 1.8 mm quartz injector torch.
• Synchronous Vertical Dual View captures axial and radial signals in one reading, improving analysis speed and element coverage.
• IntelliQuant Screening for semiquantitative element profiling and rapid wavelength selection.
• Fitted Background Correction (FBC) automatically corrects complex matrix interferences.

Calibration and Quantitative Conditions:

• Calibration standards in 10% HNO₃, 0.01–500 ppm range, correlation coefficients >0.9996.
• Internal standard: Y at 371.029 nm (5 ppm) for matrix compensation.
• Instrument parameters: 1.2 kW RF power, 20 s uptake delay, 5 s read time, three replicates.

Hlavní výsledky a diskuse

Instrumental Performance:

• Limits of detection (LODs) and quantification (LOQs) met or exceeded EAM 4.4 requirements for all elements.
• Automatic FBC successfully removed background structures, e.g., OH overlaps on Ca 315.887 nm.
• Method demonstrated stability over 10 h (360 analyses) with <3% drift and <1.5% RSD.

Method Accuracy:

• SRM recoveries for all analytes within ±10% of certified values, complying with ±20% FDA criteria.
• Spike recoveries in method blanks and samples ranged 90–109%, meeting acceptance limits.

Sample Results:

• Effervescent tablet showed very high Na and K levels compared to syrups, reflecting matrix composition.
• Blended syrup contained elevated levels of most elements versus natural syrup, likely due to added minerals.

Přínosy a praktické využití metody

The combined use of SVDV, IntelliQuant, and FBC delivers:

• Simultaneous multi-element analysis with single reading, halving analysis time and argon consumption.
• Rapid method development through semiquantitative screening.
• Accurate quantification in varied food matrices, supporting regulatory labeling and quality control.
• Enhanced laboratory productivity and reproducibility for high-throughput food testing.

Budoucí trendy a možnosti využití

Advancements in ICP-OES technology and software are expected to further streamline analysis of complex samples. Future directions include expanded semiquantitative screening libraries, real-time matrix correction algorithms, integration with workflow automation, and application to an even broader range of nutraceuticals, botanical extracts, and novel functional food formulations.

Závěr

The Agilent 5900 SVDV ICP-OES method adapted from FDA EAM 4.4 provides accurate, robust, and high-throughput determination of essential elements in functional foods. The incorporation of smart tools significantly reduces development time, ensures data quality, and meets stringent regulatory requirements, establishing a powerful platform for routine nutrition and contaminant testing.

Reference

1. Granato D., Barba F.J., Bursać Kovačević D., Lorenzo J.M., Cruz A.G., Putnik P. Functional foods: Product development, technological trends, efficacy testing, and safety. Annual Review of Food Science and Technology, 2020, 11(1), 93–118.
2. Lordan R. Dietary supplements and nutraceuticals market growth during the coronavirus pandemic – Implications for consumers and regulatory oversight. PharmaNutrition, 2021, 18, 100282.
3. Grand View Research, Inc. Nutraceuticals market size and share report, 2021–2030.
4. Mindak W.R., Dolan S.P. FDA Elemental Analysis Manual 4.4: ICP-AES determination of elements in food using microwave digestion, 2010.
5. Agilent Technologies. Synchronous Vertical Dual View (SVDV) for High Productivity and Low Cost of Ownership, 5994-1513EN.
6. Agilent Technologies. IntelliQuant Screening, 5994-1518EN.
7. Agilent Technologies. Fitted Background Correction (FBC) – Fast, Accurate and Fully Automated Background Correction, 5991-4836EN.