LC/TOF, LC/HRMS, LC/MS, LC/MS/MS
IndustriesFood & Agriculture
ManufacturerShimadzu
Importance of the Topic
Veterinary drug residue monitoring in poultry is crucial for ensuring food safety and public health. High-resolution mass spectrometry enables comprehensive detection of multiple drug classes in a single run, reducing the risk of undetected contaminants. Advances in sample preparation and analytical sensitivity contribute to faster screening and reliable quantification of trace-level residues.
Objectives and Overview
This study evaluates a quadrupole time-of-flight (Q-TOF) mass spectrometer coupled with an ultra-high-performance liquid chromatography system for the analysis of 39 veterinary drugs in chicken tenders. The work aims to demonstrate method performance, including sensitivity, accuracy, recovery, and linearity, while streamlining sample preparation for routine screening and quantification.
Methodology and Instrumentation
Sample Preparation
- STQ-LC repeated extraction: Freeze and crush 5 g chicken tenders with standard solution and water, followed by acetonitrile, sodium chloride, and magnesium sulfate addition, shaking, and centrifugation.
- Cleanup via Smart-SPE cartridges (C18 plus PSA) with sequential conditioning and elution using acetonitrile and acidified solvents.
- Final volume adjustment and dilution to obtain 0.125 g/mL sample concentration and 1.25 ppb target concentration.
Instrumentation
- UHPLC system: Nexera X3 with Shim-pack Scepter C18-120 column, gradient elution using 0.1% formic acid in water and acetonitrile at 0.2 mL/min, column temperature 40 °C.
- Q-TOF MS: LCMS-9030 with positive ESI, mass range m/z 100–1000, interface temperature 250 °C, high-resolution accurate mass detection within ±5 ppm.
Key Results and Discussion
- Extraction recoveries ranged from 70% to 120% for 32 of 39 analytes, with reproducibility (RSD) generally below 12% and mass errors within ±5 ppm.
- Calibration curves in solvent and matrix showed excellent linearity (R² ≥ 0.99) across 0.25–50 ppb.
- Narrow XIC extraction windows reduced noise and interference, yielding clear chromatographic peaks even in complex extracts.
- Comprehensive detection of sulfonamides, quinolones, and other drug classes was achieved in a single analysis, demonstrating method robustness.
Benefits and Practical Applications
- High-resolution Q-TOF enables simultaneous screening and quantification of a broad spectrum of veterinary drugs without prior target selection.
- Simplified sample preparation reduces turnaround time and solvent usage.
- Reliable mass accuracy and reproducibility support routine quality control and regulatory compliance testing.
Future Trends and Possibilities
- Integration of non-targeted screening workflows using full-scan HRMS data to detect emerging contaminants and metabolites.
- Automation of sample preparation and data processing to increase laboratory throughput and reduce manual errors.
- Application of high-resolution mass spectrometry to other food matrices and environmental samples for comprehensive safety monitoring.
- Development of spectral libraries and machine learning algorithms for rapid compound identification and quantification.
Conclusion
The combination of STQ-LC sample preparation and Q-TOF analysis on the LCMS-9030 platform provides a powerful approach for fast, accurate, and comprehensive determination of veterinary drug residues in chicken. The method demonstrates strong performance metrics across sensitivity, accuracy, and reproducibility, making it suitable for routine screening and regulatory applications.
References
- Shima and colleagues, poster presented at the 114th Annual Meeting of the Japan Society for Food Hygiene and Safety, High-speed Simultaneous Analysis of Veterinary Drugs in Meat by Combining STQ Method and LC/MS/MS (2018).
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