Analysis of Multiresidue Pesticides in Salmon Using Agilent Captiva EMR—Lipid with GC/MS/MS

Significance of the topic

The presence of pesticide residues in aquaculture products such as salmon poses food safety and environmental risks. Salmon’s high lipid and protein content complicates residue analysis, demanding robust cleanup strategies to prevent matrix interferences. Reliable multiresidue methods enable compliance with regulatory limits and support quality assurance in food testing laboratories.

Objectives and overview

This study aimed to develop and validate a streamlined GC/MS/MS method for simultaneous determination of 38 pesticides in salmon. The approach integrates solid–liquid extraction, Agilent Captiva EMR—Lipid cleanup, and analysis by Agilent Intuvo 9000 GC coupled to a 7010B triple quadrupole mass spectrometer. A 20-minute run time on an HP-5ms Ultra Inert column was established to deliver rapid, high-throughput results.

Methodology and instrumentation used

Sample preparation involved:

• Weighing 2.5 g homogenized salmon, spiking as needed.
• Two-step extraction with 5 mL each of 80:20 acetonitrile/ethyl acetate, followed by centrifugation.
• Addition of water and loading onto a 3 mL Captiva EMR—Lipid cartridge for lipid removal.
• Elution with 16:64:20 ethyl acetate/acetonitrile/water, vacuum drying, and back-exchange into isooctane for GC/MS/MS.

The instrumental setup comprised:

• Agilent Intuvo 9000 GC with electronic pneumatic control and 7693 autosampler.
• Agilent 7010B Triple Quadrupole MS operating in dynamic multiple reaction monitoring (dMRM).
• HP-5ms Ultra Inert column (30 m×0.25 mm, 0.25 µm) with ultra-inert inlet liners.
• Helium carrier gas, electron impact ionization, and nitrogen collision gas.

Main results and discussion

Method validation demonstrated:

• Linearity: calibration curves over 0.5–25 µg/kg (2–100 µg/kg matrix levels) with R2 ≥ 0.990 for all pesticides.
• Limits of quantification (LOQs) at 25 µg/kg for 36 compounds; two analytes at 50 µg/kg.
• Recoveries between 83% and 125% across three spiking levels (25, 50, 100 µg/kg).
• Precision: relative standard deviations below 25% for all analytes; majority <15% RSD.

The use of dynamic MRM and ultra-inert column liners effectively minimized active-site interactions, ensuring sharp peaks and reproducible responses. Captiva EMR—Lipid selectively removed major lipid interferences, enhancing method robustness.

Benefits and practical application

The developed workflow offers:

• Efficient lipid removal and cleanup without extensive solvent evaporation or SPE steps.
• Short analysis time (20 minutes) and high throughput suitable for routine testing.
• Compatibility with both GC/MS/MS and LC/MS/MS platforms to accommodate diverse analyte classes.
• Reduced system maintenance and prolonged column/instrument lifetime due to cleaner extracts.

Practical applications include regulatory monitoring, quality control in food industry laboratories, and large-scale surveillance of pesticide residues in fatty matrices.

Future trends and opportunities

Emerging directions include:

• Integration of automated, miniaturized extraction and cleanup modules for higher throughput.
• Extension of the EMR—Lipid approach to other complex matrices (dairy, meat, plant-based products).
• Adoption of high-resolution mass spectrometry for non-target screening of emerging contaminant classes.
• Development of multi-analyte methods combining pesticides, mycotoxins, and veterinary drug residues.

Conclusion

A validated GC/MS/MS method employing Agilent Captiva EMR—Lipid cleanup delivers accurate, precise, and rapid detection of 38 pesticides in salmon. The approach simplifies sample preparation, achieves low LOQs, and ensures compliance with maximum residue limits, making it suitable for routine implementation in food safety laboratories.

Reference

1. Food and Agriculture Organization of the United Nations (FAO). The State of World Fisheries and Aquaculture, 2018.
2. Agilent Technologies. Determination of 19 Polycyclic Aromatic Hydrocarbon Compounds in Salmon and Beef. Application Note 5994-0553EN, 2019.
3. Agilent Technologies. Challenging Pesticide Analysis Using an Agilent J&W DB-35ms Ultra Inert GC Column. Application Note 5990-6595EN, 2010.
4. Agilent Technologies. Better Pesticide Analysis with Agilent J&W Ultimate Plus Tubing in an Inert Flow. Application Note 5991-5404EN, 2014.