Reduce Cost of Pesticide Residue Analysis
Applications | 2015 | Agilent TechnologiesInstrumentation
Ensuring the safety of food products by accurately quantifying pesticide residues is critical for protecting public health and meeting regulatory limits. Laboratories are under pressure to lower per-sample costs without sacrificing sensitivity or reliability.
This study evaluates a miniaturized QuEChERS extraction combined with GC/MS/MS using a high-efficiency source to reduce solvent and consumable usage, lower maintenance, and achieve limits of quantitation (LOQs) below established maximum residue limits (MRLs) for common pesticides in carrot, tomato, and celery matrices.
Samples of 2 g homogenized produce were extracted with 2 mL acetonitrile containing 1% acetic acid, using mechanical shaking and a scaled-down QuEChERS salt mixture. Dispersive SPE cleanup was performed using sorbents tailored for each matrix. Extracts were injected at 0.5 μL into an Agilent GC with backflushing and a high-efficiency source coupled to a triple quadrupole MS in MRM mode. Calibration curves covered 0.5 to 50 ng/g with 1/x weighting.
Calibration demonstrated R² ≥ 0.992 for 97% of 126 pesticides. LOQs of 1 ng/g were achieved for 86–90% of analytes, and ≤ 5 ng/g for 95–98% across the three matrices. Base-sensitive compounds captan and folpet reached LOQs of 5 ng/g in carrot and tomato and 1 ng/g in celery using deuterated internal standards. Mini-QuEChERS reduced solvent and sorbent usage, yielding cost savings of 43–48% per sample and less frequent instrument maintenance due to lower injection volumes.
This approach offers substantial reductions in solvent, sorbent, and labeled standard consumption while maintaining regulatory compliance. The combination of miniaturized sample prep and high-efficiency ion source enables high throughput, improved data quality at low levels, and streamlined laboratory workflows.
Further miniaturization, integration with automated platforms, expansion to diverse complex matrices, and adoption of advanced mass spectrometry sources can drive additional cost savings and sensitivity improvements. Incorporating more isotopically labeled standards can enhance accuracy for challenging analytes.
Miniaturized QuEChERS extraction coupled with a high-efficiency GC/MS/MS source achieves robust, cost-effective pesticide residue analysis with LOQs well below default MRLs. This method enhances laboratory efficiency, lowers operational costs, and ensures reliable monitoring of food safety.
GC/MSD, GC/MS/MS, Sample Preparation, GC/QQQ
IndustriesFood & Agriculture
ManufacturerAgilent Technologies
Summary
Significance of the topic
Ensuring the safety of food products by accurately quantifying pesticide residues is critical for protecting public health and meeting regulatory limits. Laboratories are under pressure to lower per-sample costs without sacrificing sensitivity or reliability.
Study objectives and overview
This study evaluates a miniaturized QuEChERS extraction combined with GC/MS/MS using a high-efficiency source to reduce solvent and consumable usage, lower maintenance, and achieve limits of quantitation (LOQs) below established maximum residue limits (MRLs) for common pesticides in carrot, tomato, and celery matrices.
Methodology
Samples of 2 g homogenized produce were extracted with 2 mL acetonitrile containing 1% acetic acid, using mechanical shaking and a scaled-down QuEChERS salt mixture. Dispersive SPE cleanup was performed using sorbents tailored for each matrix. Extracts were injected at 0.5 μL into an Agilent GC with backflushing and a high-efficiency source coupled to a triple quadrupole MS in MRM mode. Calibration curves covered 0.5 to 50 ng/g with 1/x weighting.
Used instrumentation
- Agilent 7890 GC with electronic pneumatic control and backflush
- Agilent 7010 Triple Quadrupole GC/MS with high-efficiency source
- Agilent 7693A Automatic Liquid Sampler
- Geno/Grinder mechanical shaker and Heraeus centrifuge
Key results and discussion
Calibration demonstrated R² ≥ 0.992 for 97% of 126 pesticides. LOQs of 1 ng/g were achieved for 86–90% of analytes, and ≤ 5 ng/g for 95–98% across the three matrices. Base-sensitive compounds captan and folpet reached LOQs of 5 ng/g in carrot and tomato and 1 ng/g in celery using deuterated internal standards. Mini-QuEChERS reduced solvent and sorbent usage, yielding cost savings of 43–48% per sample and less frequent instrument maintenance due to lower injection volumes.
Benefits and practical applications
This approach offers substantial reductions in solvent, sorbent, and labeled standard consumption while maintaining regulatory compliance. The combination of miniaturized sample prep and high-efficiency ion source enables high throughput, improved data quality at low levels, and streamlined laboratory workflows.
Future trends and potential applications
Further miniaturization, integration with automated platforms, expansion to diverse complex matrices, and adoption of advanced mass spectrometry sources can drive additional cost savings and sensitivity improvements. Incorporating more isotopically labeled standards can enhance accuracy for challenging analytes.
Conclusion
Miniaturized QuEChERS extraction coupled with a high-efficiency GC/MS/MS source achieves robust, cost-effective pesticide residue analysis with LOQs well below default MRLs. This method enhances laboratory efficiency, lowers operational costs, and ensures reliable monitoring of food safety.
References
- Anastassiades M, Lehotay SJ, Štajnbaher D, Schenck FJ. Fast and Easy Multiresidue Method Employing Acetonitrile Extraction/Partitioning and Dispersive SPE for the Determination of Pesticide Residues in Produce. J AOAC Int. 2003;86:412–431.
- Lehotay SJ, Maštovská K, Lightfield AR. 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.
- Lehotay SJ. Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study. J AOAC Int. 2007;90:485–520.
- European Committee for Standardization. EN 15662: Foods of Plant Origin–Determination of Pesticide Residues Using QuEChERS. 2008.
- Meng CK. Improving Productivity and Extending Column Life with Backflush. Agilent Technologies Application Note 5989-6018EN. 2006.
- Maštovská K, Wylie PL. Evaluation of a New Column Backflushing Setup in GC-MS Analysis of Pesticide Residues in Dietary Supplements. J Chrom A. 2012;1265:155–164.
- Agriculture Marketing Service. US Department of Agriculture Pesticide Data Program. http://www.ams.usda.gov/AMSv1.0/PDP (Accessed 2015).
- European Commission. Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/12571/2013. 2013.
- US EPA. Food Quality Protection Act of 1996. Public Law 104-170. 1996.
- Churley M, Stevens J. Optimize Food Analysis with Miniaturized QuEChERS and Agilent 7010 Triple Quad GC/MS. Agilent Technologies Application Note 5991-5507EN. 2015.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.
Similar PDF
Breaking Bad: Change lab habits with more ions
2016|Agilent Technologies|Presentations
Breaking Bad: Change lab habits with more ions Melissa Churley Joan Stevens Applications Scientists Agilent Technologies Old Habits Maintained New Approach Meeting QA/QC Maintained Maintenance need Injected volume 0.5 µl 2 µl Sample Preparation 15 g 2g 7/15/2016 2 Optimizing…
Key words
cost, costquechers, quechershabits, habitssample, sampleendosulfan, endosulfanless, lessachievable, achievabledspe, dspemini, miniloqs, loqswhat, whatpreparation, preparationsavings, savingsminiaturizing, miniaturizingminiaturize
Optimize Food Analysis with Miniaturized QuEChERS and Agilent 7010 Triple Quad GC/MS
2015|Agilent Technologies|Applications
Optimize Food Analysis with Miniaturized QuEChERS and Agilent 7010 Triple Quad GC/MS Application Note Food Testing and Agriculture Authors Abstract Melissa Churley and Joan Stevens There are many advantages in miniaturizing sample preparation. The use of less Agilent Technologies, Inc.…
Key words
quechers, quechersextraction, extractionpesticide, pesticideresponses, responsescounts, countspesticides, pesticidespartitioning, partitioningacquisition, acquisitiondispersive, dispersiverelative, relativemrl, mrlbroccoli, broccoliagriculture, agriculturerecovery, recoveryhomogenizers
NACRW: Representative, Two-gram Incurred Food Samples Using Mini-QuEChERS, Cryomilling and GC/MS/MS Analysis with a High Efficiency Ion Source
2016|Agilent Technologies|Posters
Representative, Two-gram Incurred Food Samples Using Mini-QuEChERS, Cryomilling and GC/MS/MS Analysis with a High Efficiency Ion Source Joan Stevens1, Phil Wylie1 and Melissa Churley2 1Agilent Technologies Inc., 2850 Centerville Road, Wilmington, DE 19808 USA Cost savings ranged between 42-48% due…
Key words
cryomilling, cryomillingquechers, quechersmini, minicost, costhomogenized, homogenizedsample, samplefrozen, frozendspe, dspecommodites, commoditescryomilled, cryomilledcentrifuge, centrifugesavings, savingsmulti, multicoupe, couperesidue
Representative, Tw o-gram Incurred Food Samples Using Mini-QuEChERS, Cryomilling and GC/MS/MS Analysis with a High Efficiency Ion Source
2016|Agilent Technologies|Posters
Representative, Two-gram Incurred Food Samples Using Mini-QuEChERS, Cryomilling and GC/MS/MS Analysis with a High Efficiency Ion Source 1Agilent Technologies Inc., 2850 Centerville Road, Wilmington, DE 19808 USA Introduction Analytical results for a 2 g sample correlated with those using a…
Key words
cryomilling, cryomillingquechers, quechersmini, minihomogenized, homogenizedcost, costresidue, residuepesticide, pesticideincurred, incurredmulti, multihomogenization, homogenizationsample, samplefrozen, frozenpersample, persamplecentrifuge, centrifugecommodites