Rapid Screening Analysis of On-Line Purified Residual Pesticides in Crop Extract Using Accurate Mass Information

Significance of the topic

In food safety pesticide residues are regulated to protect health. The rising variety of pesticides worldwide demands advanced screening methods. High throughput and reliable pesticide analysis supports regulatory compliance and minimizes health risks.

Aims and overview of the study

This study demonstrates rapid screening of residual pesticides in spinach extracts by coupling an online sample cleanup column Revive ILSP with a QTOF mass spectrometer LCMS-9050. The approach is evaluated against conventional QuEChERS to assess speed reproducibility and sensitivity.

Analytical methodology

Spinach samples were frozen ground and extracted with acidified acetonitrile. The extract passed through the Revive ILSP inline cleanup column enabling direct injection. Chromatographic separation used a biphenyl column with a gradient of ammonium formate formic acid in water and methanol. The LCMS-9050 performed polarity switching electrospray ionization and time of flight detection over m/z 50-800. Accurate mass and retention time based screening was applied for 79 pesticides.

Used instrumentation

• Nexera X3 UHPLC system
• Shim-pack Velox Biphenyl analytical column 100 mm × 2.1 mm 2.7 μm
• Revive ILSP Pesticides Single 5 × 2.1 mm cartridge
• LCMS-9050 quadrupole time of flight mass spectrometer

Main results and discussion

All 79 pesticide standards were detected within ±1 mDa mass error ensuring high confidence identification. Total ion and extracted ion chromatograms confirmed clear separation of analytes from the matrix. Calibration curves in solvent and extract showed linearity with R2 greater than 0.99 across 0.5–50 ppb. Sixty eight compounds achieved detection limits of 2.5 ppb or lower. Spike recovery at 2.5 ppb yielded 70–120 percent recovery for 77 pesticides with RSD below 20 percent indicating minimal matrix effects and robust reproducibility.

Benefits and practical applications

The Revive ILSP inline cleanup significantly reduces sample preparation time to one third compared with QuEChERS and lowers solvent and plastic consumption. Accurate mass screening with polarity switching covers a broad pesticide panel in a single run. This workflow streamlines QA/QC in food safety laboratories and enables high throughput monitoring of residue compliance.

Future trends and possibilities

Future developments may include extending this approach to other crop matrices expanding the scope to newer pesticide chemistries and automated data processing with machine learning. Integration with multiresidue libraries and high resolution databases will enhance screening breadth. Green analytical strategies may further reduce waste through miniaturization and alternative solvents.

Conclusion

The combination of an inline cleanup Revive ILSP column and the LCMS-9050 QTOF offers a rapid sensitive and reliable multiresidue pesticide screening platform. High mass accuracy fast sample throughput and robust matrix tolerance support routine analysis in food safety applications.

References

• Lupo SA Romesberg RL Lu X 2020 Automated inline pigment removal for the analysis of pesticide residues in spinach by liquid chromatography tandem mass spectrometry Journal of Chromatography A 1629 461477