LC/MS, LC/MS/MS, LC/QQQ
IndustriesFood & Agriculture
ManufacturerAgilent Technologies
Significance of the Topic
The monitoring of veterinary drug residues in meat products is critical for food safety, regulatory compliance, and consumer health protection. Multi-residue analytical methods enable simultaneous detection of diverse drug classes, streamlining testing and supporting regulatory enforcement.
Objectives and Study Overview
This study aimed to develop and validate a robust, high-throughput method for quantifying 193 veterinary drug residues in pork, beef, lamb, and chicken. The approach integrates Agilent Captiva EMR–Lipid HF cartridge cleanup with ultra-high-performance liquid chromatography coupled to a triple quadrupole mass spectrometer (LC/TQ). Matrix-matched calibration curves were used for accurate quantification across multiple meat matrices.
Methodology
Sample Preparation:
- Weigh 5 g of homogenized meat sample.
- Add Mcllvaine-Na2-EDTA buffer and acidified acetonitrile; vortex and centrifuge.
- Apply crude extract to Captiva EMR–Lipid HF 3 mL cartridge for passthrough lipid removal.
- Dilute eluate, filter via syringe filter, and inject into LC/TQ.
Calibration and Validation:
- Matrix-matched standards at 0.5–100 ng/mL were prepared in blank extracts.
- LOQ and LOD determined at signal-to-noise ratios of ≥10 and ≥3, respectively.
- Recovery assessed at three spike levels (5, 100, 200 μg/kg) in six replicates per matrix.
Used Instrumentation
- Agilent 1290 Infinity II UHPLC system (binary pump, multisampler, column thermostat)
- Agilent G6495C triple quadrupole mass spectrometer with Jet Stream ESI source
- Agilent ZORBAX RRHD Eclipse Plus C18 column (2.1 × 100 mm, 1.8 μm)
- Captiva EMR–Lipid HF cartridges and Captiva RC 0.2 μm syringe filters
Main Results and Discussion
The method exhibited excellent linearity with correlation coefficients (R2) > 0.99 over 0.5–100 ng/mL for most analytes. The LOQ was 5 μg/kg and LOD was 2 μg/kg across meat matrices. Average recoveries ranged from 50 % to 120 % with relative standard deviations below 20 % for 189 of the 193 targets; four compounds (Cefdinir, Amprolium, Doxycycline, Chlorpromazine) showed lower recoveries (< 50 %). The passthrough cleanup provided effective lipid removal while maintaining analyte integrity.
Practical Benefits and Applications
This streamlined workflow reduces sample preparation time and solvent usage compared to traditional methods. It supports high-throughput screening and routine monitoring of veterinary drugs in food safety laboratories, quality control departments, and regulatory agencies.
Future Trends and Applications
Advancements may include expansion of target analyte lists, integration with high-resolution mass spectrometry for non-targeted screening, automated sample handling, and application to complex food matrices beyond meat. Data-processing tools and machine learning algorithms will further enhance identification and quantification capabilities.
Conclusion
The proposed LC/TQ method combined with Captiva EMR–Lipid HF cleanup offers a validated, reliable solution for the simultaneous determination of 193 veterinary drug residues in livestock and poultry meat. Its performance meets regulatory requirements for sensitivity, accuracy, and precision, facilitating comprehensive food safety control.
References
- GB 31650-2019 National Food Safety Standard: Maximum Residue Limits for Veterinary Drugs in Food.
- GB 31650.1-2022 National Food Safety Standard: Maximum Residue Limits for 41 Veterinary Drugs in Food.
- Wang Y. L., Ye N., Yin H., et al. Detection of 199 Drugs and Metabolites Residues in Livestock and Poultry Meat by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry. Chinese Journal of Veterinary Drugs 2024, 58(04), 50–61.
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