Meeting European Union Maximum Residue Level Regulations for Pesticides in Tea and Honey
Applications | 2019 | Agilent TechnologiesInstrumentation
Pesticide residues in food products pose health and regulatory challenges worldwide. Rising use of agricultural chemicals and stricter maximum residue level regulations drive the need for sensitive, multiresidue analytical methods. Tea and honey represent complex matrices where low-level quantitation is essential to meet European Union standards and ensure consumer safety.
This study evaluates a robust workflow for multiresidue pesticide screening, confirmation, and quantitation in loose leaf black tea and organic honey. The method combines the Agilent Intuvo 9000 gas chromatograph with a 7000C triple quadrupole GC/MS platform and aims to achieve regulatory compliance with EU maximum residue levels while maintaining high accuracy and reproducibility.
Samples are homogenized and extracted using the QuEChERS approach. Three grams of tea or five grams of honey are mixed with water and acetonitrile, followed by salting out with magnesium sulfate and cleanup via dispersive solid phase extraction. Extracts are stored at low temperature prior to GC injection. Multiple reaction monitoring minimizes matrix interference and enhances selectivity.
Agilent Intuvo 9000 gas chromatograph with modular inert flowpath and midcolumn backflush
Agilent 7693B autosampler for precise injection control
Agilent 7000C triple quadrupole GC/MS operated in dynamic MRM mode
Intuvo HP5-MS Ultra Inert columns and a multimode inlet with guard chip for reduced maintenance
Calibration for targeted pesticides demonstrated excellent linearity with over 97 percent of compounds showing R2 values at or above 0.990 between 5 and 500 ppb. In honey extracts all limits of quantitation fell below 7 ppb against EU limits of 10 to 50 ppb. For tea 94 percent of compounds achieved LOQs under 100 ppb within MRL ranges of 20 to 200 ppb. Repeatability studies yielded relative standard deviations of 30 percent or less and recovery errors under 30 percent, confirming the method's robustness.
The presented workflow offers rapid sample throughput, streamlined maintenance, and reliable performance across challenging food matrices. It enables laboratories to meet regulatory requirements, supports routine monitoring of pesticide residues, and reduces downtime through an inert flowpath and guard chip system.
Advancements in GC/MS hardware and data processing will expand multiresidue methods to additional food and environmental matrices. Automation of sample preparation and integration of high resolution mass spectrometry may further lower detection limits. Continuous updates to regulatory standards will drive method adaptation and extend applications in global food safety monitoring.
The combination of QuEChERS extraction and Agilent Intuvo 9000 GC with a 7000C triple quadrupole system delivers a reliable multiresidue pesticide analysis for tea and honey. Meeting EU MRLs with low detection limits, strong linearity, and reproducible results demonstrates the method's suitability for routine food safety testing.
GC/MSD, GC/MS/MS, GC/QQQ
IndustriesFood & Agriculture
ManufacturerAgilent Technologies
Summary
Significance of the Topic
Pesticide residues in food products pose health and regulatory challenges worldwide. Rising use of agricultural chemicals and stricter maximum residue level regulations drive the need for sensitive, multiresidue analytical methods. Tea and honey represent complex matrices where low-level quantitation is essential to meet European Union standards and ensure consumer safety.
Objectives and Study Overview
This study evaluates a robust workflow for multiresidue pesticide screening, confirmation, and quantitation in loose leaf black tea and organic honey. The method combines the Agilent Intuvo 9000 gas chromatograph with a 7000C triple quadrupole GC/MS platform and aims to achieve regulatory compliance with EU maximum residue levels while maintaining high accuracy and reproducibility.
Methodology and Sample Preparation
Samples are homogenized and extracted using the QuEChERS approach. Three grams of tea or five grams of honey are mixed with water and acetonitrile, followed by salting out with magnesium sulfate and cleanup via dispersive solid phase extraction. Extracts are stored at low temperature prior to GC injection. Multiple reaction monitoring minimizes matrix interference and enhances selectivity.
Used Instrumentation
Agilent Intuvo 9000 gas chromatograph with modular inert flowpath and midcolumn backflush
Agilent 7693B autosampler for precise injection control
Agilent 7000C triple quadrupole GC/MS operated in dynamic MRM mode
Intuvo HP5-MS Ultra Inert columns and a multimode inlet with guard chip for reduced maintenance
Results and Discussion
Calibration for targeted pesticides demonstrated excellent linearity with over 97 percent of compounds showing R2 values at or above 0.990 between 5 and 500 ppb. In honey extracts all limits of quantitation fell below 7 ppb against EU limits of 10 to 50 ppb. For tea 94 percent of compounds achieved LOQs under 100 ppb within MRL ranges of 20 to 200 ppb. Repeatability studies yielded relative standard deviations of 30 percent or less and recovery errors under 30 percent, confirming the method's robustness.
Benefits and Practical Applications
The presented workflow offers rapid sample throughput, streamlined maintenance, and reliable performance across challenging food matrices. It enables laboratories to meet regulatory requirements, supports routine monitoring of pesticide residues, and reduces downtime through an inert flowpath and guard chip system.
Future Trends and Applications
Advancements in GC/MS hardware and data processing will expand multiresidue methods to additional food and environmental matrices. Automation of sample preparation and integration of high resolution mass spectrometry may further lower detection limits. Continuous updates to regulatory standards will drive method adaptation and extend applications in global food safety monitoring.
Conclusion
The combination of QuEChERS extraction and Agilent Intuvo 9000 GC with a 7000C triple quadrupole system delivers a reliable multiresidue pesticide analysis for tea and honey. Meeting EU MRLs with low detection limits, strong linearity, and reproducible results demonstrates the method's suitability for routine food safety testing.
Reference
- United States Department of Agriculture Foreign Agriculture Service Maximum Residue Limits Database 2016
- Churley M Lowering Detection Limits for Routine Analysis of Pesticide Residues in Foods Using the Agilent 7000C Triple Quadrupole GC/MS Agilent Technologies Application Note 5991-4131EN 2015
- Veeneman R Multiresidue Pesticide Analysis with the Agilent Intuvo 9000 GC and Agilent 7000 Series Mass Spectrometer Agilent Technologies Application Note 5991-7216EN 2016
- Churley M Reduce Cost of Pesticide Residue Analysis Agilent Technologies Application Note 5991-6069EN 2015
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