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Rapid Rinse and Shoot: Screening Workflow for Pesticides in Fruit by GC/MSD in Under Six Minutes

Applications | 2020 | Agilent TechnologiesInstrumentation
GC/MSD, GC/SQ
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Significance of the Topic


The presence of trace pesticide residues on fruit surfaces poses a global concern for food safety. Laboratories and distribution centers require workflows that balance broad target coverage with rapid turnaround and minimal sample preparation. The development of high speed gas chromatography mass spectrometry methods supports efficient screening and prioritization of samples for detailed analysis.

Study Objectives and Overview


This study presents a rinse and shoot workflow for rapid screening of surface pesticides on various fruits using an Agilent Intuvo 9000 gas chromatograph coupled to a 5977B mass selective detector. Sample rinsates collected with acetone are directly injected and analyzed with a 3.4 minute GC method and mass spectral deconvolution. Compound identification is achieved through library matching and time filtering using linear retention indices to ensure confident screening within a total workflow time below six minutes.

Methodology and Instrumentation


  • Sample preparation consists of rinsing fruit surfaces with high purity acetone and collecting the rinsate in amber vials.
  • The gas chromatography system employs an Agilent Intuvo 9000 GC with direct heating oven at 250 °C per minute ramp, a multimode inlet, and an Intuvo MMI Guard Chip for matrix protection.
  • Mid column backflushing using an Intuvo PSD module prevents high boiling species from reaching the column head and extends maintenance intervals.
  • The mass spectrometer is an Agilent 5977B MSD operating in full scan mode with spectral deconvolution performed by MassHunter Unknowns Analysis software.
  • Time filtering based on linear retention indices calibrated with a C9 to C34 n alkane ladder reduces false positives and supports confident library matches.

Main Results and Discussion


  • The rinse and shoot workflow enables a 3.4 minute chromatographic separation, with complete sample to report in under six minutes.
  • Screening of strawberry, banana, lemon, cherry and peach rinsates identified multiple pesticides such as fenhexamid, fludioxonil, thiabendazole and captan, alongside matrix related compounds.
  • Spectral deconvolution and retention index time filtering improved identification confidence for coeluting compounds, lifting match scores for key pesticides.
  • Backflush eliminated carryover peaks and allowed for extended analytical sequences without column trimming.
  • A slower 20 °C per minute ramp delivered increased chromatographic resolution for confirmatory analysis, further improving library match scores.
  • System robustness was demonstrated over 235 injections, with minimal retention time shift and rapid restoration of response via simple guard chip, liner and septum replacement.

Benefits and Practical Applications


  • High throughput screening with broad pesticide coverage and minimal sample handling.
  • Rapid triage of samples in remote or nontraditional lab environments thanks to compact footprint and standard power requirements.
  • Extended maintenance free runtime reduces downtime and workflow disruptions.
  • Flexible reporting and library management using MassHunter Unknowns Analysis permits customized result output.

Future Trends and Potential Applications


Advances in high resolution mass spectrometry libraries and automation will support expanded target scopes and improved quantitation. Integration with artificial intelligence for data review and the development of comprehensive surface residue screens may further streamline food safety workflows. The adoption of similar fast screening methods could extend to environmental monitoring, regulatory compliance and on site quality control across the supply chain.

Conclusion


The Agilent Intuvo 9000 GC/MSD rapid rinse and shoot method demonstrates fast, reliable pesticide screening on fruit surfaces. Combining direct heating, spectral deconvolution and retention index time filtering achieves confident identifications in under six minutes while simplifying maintenance via backflushing and guard chip protection. This approach enables efficient sample triage and high throughput analysis for food safety and quality monitoring.

Reference


  1. Andrianova A and Quimby B Westland J Quantitation of Pesticides in Strawberries at Tolerance Levels by GC triple quadrupole systems Agilent application note 5994 0799EN 2019
  2. Nieto S et al Contaminants Screening Using High Resolution GC Q TOF and an Expanded Accurate Mass Library Agilent application note 5994 1346EN 2019
  3. Andrianova A Quimby B Westland J GC MSD Pesticide Screening in Strawberries Using Deconvoluted Spectra Agilent application note 5994 0915EN 2019
  4. Andrianova A Quimby B Westland J Pesticide Screening in Strawberries Using GC 8860 with 5977B and SureTarget Deconvolution application note 5994 0916EN 2019
  5. Churley M Wylie P Peterson D 60 Second Screening of Foods Using the Agilent QuickProbe GC MSD application note 5994 1505EN 2019
  6. Sandy C Butler I Sullivan R MassHunter Quant Software Incorporating Retention Index Results technical brief 2017

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