Analysis of Pesticide Residues in Rice with Bond Elut QuEChERS Extraction Kit sand Agilent J&W HP-5ms Ultra Inert GC Column

Significance of the topic

The accurate determination of trace pesticide residues in staple foods such as rice is critical for consumer safety, regulatory compliance, and quality control in the food industry. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) approach combined with high-resolution gas chromatography–mass spectrometry (GC-MS) offers a streamlined workflow for multiresidue analysis, balancing efficiency with robust cleanup and sensitive detection.

Objectives and study overview

This application note evaluates the performance of Agilent Bond Elut QuEChERS EN extraction and dispersive solid-phase extraction (dSPE) kits for isolating 57 GC-amenable pesticide residues from rice. The study validates the method in terms of linearity, recovery, reproducibility, and matrix effects, and demonstrates rapid screening using Agilent’s Retention Time Locking (RTL) pesticide library.

Methodology

• Sample preparation follows the EN 15662:2007 protocol: 5 g of homogenized rice is mixed with water, internal standards, and acetonitrile, then partitioned by adding a QuEChERS salt packet (MgSO₄, NaCl, citrate salts).
• After vigorous shaking and centrifugation, 6 mL of the acetonitrile layer is subjected to dispersive SPE cleanup using PSA sorbent and MgSO₄ to remove co-extractives.
• A 0.5 mL aliquot of the purified extract is transferred to an autosampler vial for GC-MS analysis in splitless injection mode.

Used Instrumentation

• Gas chromatograph: Agilent 7890 GC with split/splitless inlet
• Mass spectrometer: Agilent 5975C inert MSD operating in EI-SIM/Scan mode
• Column: Agilent J&W HP-5ms Ultra Inert capillary (30 m × 0.25 mm, 0.25 µm)
• Autosampler: Agilent 7683 ALS
• QuEChERS kits: Bond Elut QuEChERS EN extraction (p/n 5982-5650) and dispersive SPE (p/n 5982-5156)

Main results and discussion

• Linearity: All 57 pesticides exhibited excellent calibration linearity in rice matrix (R² ≥ 0.991, average R² = 0.9990) over 50–400 ng/mL.
• Recoveries and precision: Spiking at 50, 100, and 200 ng/g yielded recoveries between 80 % and 110 % for most analytes, with an average RSD of 5.5 %.
• Chromatographic performance: Total ion chromatograms demonstrated baseline separation of diverse classes (organochlorines, organophosphates, pyrethroids) within 36 min. Retention Time Locking ensured reproducible compound identification against the RTL pesticide library.
• Matrix effects: Minimal interference was observed, indicating effective cleanup by QuEChERS dSPE and reliable quantitation in complex rice extracts.

Benefits and practical applications

• Streamlined workflow: The combined QuEChERS extraction and dSPE cleanup reduces solvent use, labor, and analysis time compared with traditional methods.
• Broad scope: Validation across 57 pesticides covers multiple chemical classes, supporting comprehensive monitoring in food safety laboratories.
• High throughput: Compatibility with GC-MS SIM and RTL software allows rapid screening and confirmation, accelerating routine testing.

Future trends and potential applications

• Expanding analyte lists to include emerging pesticide metabolites and polar compounds using hybrid GC-MS/MS and LC-MS/MS platforms.
• Integration of automated QuEChERS workflows and robotics to enhance reproducibility and sample throughput in large-scale monitoring programs.
• Development of advanced data-processing algorithms, including machine learning-based deconvolution, for improved identification in complex matrices.

Conclusion

The combination of Agilent Bond Elut QuEChERS EN kits with J&W HP-5ms Ultra Inert GC column and MSD offers a rapid, robust, and cost-effective approach for multiresidue pesticide analysis in rice. The validated method demonstrates excellent linearity, recovery, reproducibility, and minimal matrix effects, making it well suited for routine food safety and quality control applications.

References

1. Anastassiades M, Lehotay SJ. Fast and Easy Multiresidue Method Employment Acetonitrile Extraction/Partitioning and Dispersive Solid Phase Extraction for the Determination of Pesticide Residues in Produce. J AOAC Int. 2003;86:412–431.
2. Lehotay SJ. Use of Buffering and Other Means to Improve Results of Problematic Pesticides in a Fast and Easy Method for Residue Analysis of Fruits and Vegetables. J AOAC Int. 2005;88:615–629.
3. European Committee for Standardization. Foods of plant origin: Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and cleanup by dispersive SPE-QuEChERS method. CEN/TC 275; 2007.
4. Payá P, Anastassiades M. Analysis of pesticide residues using the QuEChERS multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem. 2007;389:1697–1714.
5. Giarocco V, Quimby B, Klee M. Retention Time Locking: Concepts and Applications. Agilent Technologies publication 5966-2469EN.
6. Wylie PL. Screening for 926 Pesticides and Endocrine Disruptor by GC/MS with Deconvolution Reporting Software and a New Pesticide Library. Agilent Technologies publication 5989-5076EN.