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Using the Nexera UC Online SFE-SFC-MS System to Analyze Residual Pesticides in Agricultural Products

Applications | 2015 | ShimadzuInstrumentation
Sample Preparation, LC/MS, LC/MS/MS, LC/QQQ, SFC
Industries
Food & Agriculture
Manufacturer
Shimadzu

Summary

Importance of the Topic



Supercritical fluid extraction coupled with chromatography and mass spectrometry addresses the growing need for fast and reliable quantitation of pesticide residues in food. The automated integration reduces sample preparation time, solvent consumption and manual errors while achieving sensitive detection across a broad polarity range.

Objectives and Study Overview



The aim of this work was to demonstrate the performance of an online system that unifies supercritical fluid extraction, supercritical fluid chromatography and tandem mass spectrometry to analyze over 500 pesticide compounds in agricultural products. Emphasis was placed on throughput, repeatability, linearity and recovery in both standard mixtures and real matrix samples.

Methodology and Instrumentation



Sample preparation was streamlined to mixing one gram of crushed produce with a dehydrating agent. The mixture was loaded into an extraction vessel and subjected to static and dynamic extraction using supercritical CO2 with a methanol based modifier. Extract flow was split to protect the analytical column before gradient separation on a reverse phase SFC column. Detection was performed by a triple quadrupole mass spectrometer operating in MRM mode.

Key Results and Discussion



Each analysis was completed in approximately 45 minutes. Of 327 pesticides in the standard mixture, peak area RSD remained below 30 percent across 1 to 100 ng/g and calibration curves exhibited R2 values above 0.99. Tomato samples spiked with 510 compounds yielded 248 analytes with recoveries between 70 and 120 percent and RSD below 20 percent. The system effectively covered analytes with log Pow values from -1.4 to 6.9.

Benefits and Practical Applications


  • Automated end to end workflow reduces manual labor and error risk
  • High throughput supports continuous analysis of up to 48 samples
  • Lower solvent usage and waste generation compared to traditional workflows
  • Broad polarity coverage from highly polar to nonpolar pesticides
  • Robust performance ensures compliance with regulatory residue limits


Future Trends and Potential Applications



Anticipated developments include expansion of analyte libraries, adaptation to diverse food and environmental matrices, integration with high resolution mass spectrometry for untargeted screening, and advanced multiplexed extraction modules to further boost throughput.

Conclusion



The online SFE-SFC-MS platform provides a powerful, automated solution for routine pesticide residue analysis. By combining extraction and separation in a single sequence it delivers rapid, precise and environmentally friendly performance ideal for laboratory QA/QC and regulatory testing.

Used Instrumentation


  • Supercritical fluid extraction unit with CO2 supply
  • Supercritical fluid chromatograph with reverse phase UC-RP column
  • Binary pump for methanol based modifier
  • Back pressure regulators controlling static and dynamic modes
  • Triple quadrupole mass spectrometer in MRM mode
  • Automated rack changer handling up to 48 samples

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