NEW Custom “Dispersive” SPE Products for Pesticide and Acrylamide Analysis
Applications | | MerckInstrumentation
The reliable detection of pesticide residues and acrylamide in food products is critical for regulatory compliance, consumer safety, and quality control. Efficient sample preparation methods that reduce analysis time and instrument maintenance are essential to support high‐throughput testing in agricultural, environmental, and industrial laboratories.
This article describes the development and validation of dispersive solid‐phase extraction (dispersive SPE) workflows for multi‐residue pesticide analysis and acrylamide determination. It highlights a new custom product service offering pre‐weighed sorbents and salts optimized for use with QuEChERS‐based protocols to streamline sample cleanup and improve laboratory productivity.
Dispersive SPE combines salting‐out extraction with direct addition of sorbent and drying agents to acetonitrile extracts. Key steps include:
Main detection platforms include gas chromatography–mass spectrometry (GC-MS), liquid chromatography–mass spectrometry (LC-MS), and tandem LC-MS/MS.
For pesticide residues, the dispersive SPE protocol enabled the simultaneous cleanup of over 200 compounds in diverse matrices such as fruits and vegetables. An interlaboratory validation involving 15 laboratories across seven countries confirmed consistent recoveries and low matrix interference. In acrylamide analysis, hexane defatting followed by salting‐out and PSA cleanup produced extracts free of lipids and other interferences, supporting accurate quantification in starchy foods.
Advances may include expanded sorbent chemistries for targeted cleanup, integration with automated platforms to further increase throughput, miniaturized formats for microscale extractions, and coupling with high‐resolution mass spectrometry for comprehensive contaminant profiling.
Dispersive SPE methods paired with QuEChERS extraction provide a robust, efficient, and cost‐effective approach for the analysis of pesticide residues and acrylamide in food matrices. Custom pre-weighed products simplify the workflow and support high‐volume testing demands in regulatory and industrial settings.
1. Lehotay SJ. Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) Approach for Pesticide Residue Determination. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
2. Schenck FJ, Lehotay SJ, Vega V. Comparison of SPE Sorbents for Cleanup in Pesticide Residue Analysis of Fresh Fruits and Vegetables. J Sep Sci. 2002;25:883–890.
3. Anastassiades M, Lehotay SJ, Stajnbaher A, Schenck FJ. Fast and Easy Multiresidue Method Using Acetonitrile Extraction and Dispersive SPE for Pesticide Residues in Produce. J AOAC Int. 2003;86:412–431.
4. Lehotay SJ, de Kok A, Hiemstra M, van Bodegraven P. Validation of a Fast Method for 229 Pesticides in Fruits and Vegetables by GC and LC–MS. J AOAC Int. 2005;88:595–614.
5. Lehotay SJ, Mastovska K, Lightfield AR. Use of Buffering to Improve Problematic Pesticide Results in a Fast Residue Analysis Method. J AOAC Int. 2005;88:615–629.
6. Lehotay SJ. Interlaboratory Validation of the QuEChERS Method for Pesticide Residues in Fruits and Vegetables. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
7. Mastovska K, Lehotay SJ. Development of a Fast and Easy Method for Acrylamide Analysis in Food Matrices. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
Sample Preparation, Consumables
IndustriesFood & Agriculture
ManufacturerMerck
Summary
Importance of the Topic
The reliable detection of pesticide residues and acrylamide in food products is critical for regulatory compliance, consumer safety, and quality control. Efficient sample preparation methods that reduce analysis time and instrument maintenance are essential to support high‐throughput testing in agricultural, environmental, and industrial laboratories.
Objectives and Overview
This article describes the development and validation of dispersive solid‐phase extraction (dispersive SPE) workflows for multi‐residue pesticide analysis and acrylamide determination. It highlights a new custom product service offering pre‐weighed sorbents and salts optimized for use with QuEChERS‐based protocols to streamline sample cleanup and improve laboratory productivity.
Methodology and Instrumentation
Dispersive SPE combines salting‐out extraction with direct addition of sorbent and drying agents to acetonitrile extracts. Key steps include:
- Salting‐out extraction of homogenized food samples using acetonitrile with magnesium sulfate and sodium salts
- Partitioning of matrix components into organic and aqueous phases
- Cleanup by mixing acetonitrile aliquots with bulk PSA sorbent and anhydrous magnesium sulfate
- Centrifugation to separate cleaned extract for analysis
Main detection platforms include gas chromatography–mass spectrometry (GC-MS), liquid chromatography–mass spectrometry (LC-MS), and tandem LC-MS/MS.
Main Results and Discussion
For pesticide residues, the dispersive SPE protocol enabled the simultaneous cleanup of over 200 compounds in diverse matrices such as fruits and vegetables. An interlaboratory validation involving 15 laboratories across seven countries confirmed consistent recoveries and low matrix interference. In acrylamide analysis, hexane defatting followed by salting‐out and PSA cleanup produced extracts free of lipids and other interferences, supporting accurate quantification in starchy foods.
Benefits and Practical Applications
- Reduced sample handling and faster preparation compared to traditional SPE cartridges
- Lower solvent and consumable usage, cutting costs
- Custom pre‐weighed sorbent/salt kits minimize weighing steps and improve throughput
- Flexible compatibility with GC-MS and LC-MS workflows for routine monitoring and quality assurance
Future Trends and Potential Applications
Advances may include expanded sorbent chemistries for targeted cleanup, integration with automated platforms to further increase throughput, miniaturized formats for microscale extractions, and coupling with high‐resolution mass spectrometry for comprehensive contaminant profiling.
Conclusion
Dispersive SPE methods paired with QuEChERS extraction provide a robust, efficient, and cost‐effective approach for the analysis of pesticide residues and acrylamide in food matrices. Custom pre-weighed products simplify the workflow and support high‐volume testing demands in regulatory and industrial settings.
Reference
1. Lehotay SJ. Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) Approach for Pesticide Residue Determination. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
2. Schenck FJ, Lehotay SJ, Vega V. Comparison of SPE Sorbents for Cleanup in Pesticide Residue Analysis of Fresh Fruits and Vegetables. J Sep Sci. 2002;25:883–890.
3. Anastassiades M, Lehotay SJ, Stajnbaher A, Schenck FJ. Fast and Easy Multiresidue Method Using Acetonitrile Extraction and Dispersive SPE for Pesticide Residues in Produce. J AOAC Int. 2003;86:412–431.
4. Lehotay SJ, de Kok A, Hiemstra M, van Bodegraven P. Validation of a Fast Method for 229 Pesticides in Fruits and Vegetables by GC and LC–MS. J AOAC Int. 2005;88:595–614.
5. Lehotay SJ, Mastovska K, Lightfield AR. Use of Buffering to Improve Problematic Pesticide Results in a Fast Residue Analysis Method. J AOAC Int. 2005;88:615–629.
6. Lehotay SJ. Interlaboratory Validation of the QuEChERS Method for Pesticide Residues in Fruits and Vegetables. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
7. Mastovska K, Lehotay SJ. Development of a Fast and Easy Method for Acrylamide Analysis in Food Matrices. Proceedings AOAC Annual Meeting; 2004; St. Louis, MO, USA.
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