Mycotoxin Analysis in Infant Formula Using Captiva EMR—Lipid Cleanup and LC/MS/MS

Importance of the Topic

Infant formula is a highly regulated food matrix requiring sensitive and accurate detection of trace mycotoxins. Due to its high protein and lipid content, traditional sample preparation can struggle to remove interfering compounds, complicating analysis at low concentration levels.

Study Objectives and Overview

This study evaluates a streamlined workflow combining QuEChERS extraction with Agilent Captiva EMR—Lipid cleanup for simultaneous determination of 13 mycotoxins in both powdered and liquid infant formulas. Key goals include method validation, assessment of lipid removal efficiency, and comparison with a competing pass-through cleanup product.

Methodology

A QuEChERS protocol was applied using acetonitrile fortified with 2 % formic acid and extraction salts (MgSO₄, NaCl). After centrifugation, the acetonitrile layer was diluted and passed through Captiva EMR—Lipid 3 mL or 6 mL tubes by gravity followed by vacuum. The cleaned extract was prepared with ammonium formate/acetic acid solution for LC/MS/MS analysis.

Instrumentation

• Liquid Chromatography: Agilent 1290 Infinity II system with Poroshell 120 EC-C18 analytical (2.1 × 100 mm, 2.7 µm) and guard columns, operated at 40 °C, gradient elution (5 mM ammonium formate/0.1 % formic acid and ACN:methanol/0.1 % formic acid), 0.5 mL/min flow.
• Mass Spectrometry: Agilent 6490 triple quadrupole with Jet Stream source, dynamic MRM in positive/negative mode, optimized gas temperatures, flows, voltages, and collision energies for each mycotoxin.
• GC/MS Full Scan: Employed to quantify lipid removal by comparing chromatographic peak areas before and after cleanup.

Main Results and Discussion

Calibration curves for all 13 mycotoxins exhibited linearity (R² ≥ 0.992). Method recoveries ranged from 70.4 % to 106.8 % with RSD < 18 % across low, mid, and high spike levels. Incorporation of 2 % formic acid enhanced fumonisin extraction. GC/MS data demonstrated approximately 90 % lipid removal post-Captiva EMR—Lipid cleanup. Comparative testing against a competitive pass-through sorbent showed superior recovery—especially for hydrophobic analytes such as zearalenone, ochratoxin A, and sterigmatocystin—while maintaining precision.

Benefits and Practical Applications

The described workflow requires minimal specialized equipment and expertise, offering food testing laboratories a robust, high-throughput approach for multiclass mycotoxin analysis in fatty matrices. Its selectivity reduces matrix effects and extends instrument uptime by preventing lipid buildup.

Future Trends and Potential Applications

Emerging applications may include expansion to other multiclass contaminant panels such as veterinary drugs and pesticide metabolites. Integration with automated sample-prep platforms and high-resolution mass spectrometry could further enhance throughput and selectivity. Continued development of sorbent chemistries promises broader matrix compatibility and direct-injection capabilities.

Conclusion

The combination of QuEChERS extraction with Captiva EMR—Lipid cleanup and LC/MS/MS detection provides a reliable, sensitive, and efficient method for quantifying low-level mycotoxins in infant formula. This approach simplifies sample preparation while delivering high recovery, excellent precision, and effective lipid removal.

References

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3. European Commission Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs. 2006.
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