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Analytical and Bioanalytical Chemistry

, Volume 410, Issue 22, pp 5373–5389 | Cite as

Target screening of 105 veterinary drug residues in milk using UHPLC/ESI Q-Orbitrap multiplexing data independent acquisition

  • Jian Wang
  • Daniel Leung
  • Willis Chow
  • James Chang
  • Jon W. Wong
Paper in Forefront
Part of the following topical collections:
  1. Food Safety Analysis

Abstract

This paper presents a multi-class target screening method for the detection of 105 veterinary drug residues from 11 classes in milk using ultra-high performance liquid chromatography electrospray ionization quadrupole Orbitrap mass spectrometry (UHPLC/ESI Q-Orbitrap). The method is based on a non-target approach of full mass scan and multiplexing data-independent acquisition (Full MS/mDIA). The veterinary drugs include endectocides, fluoroquinolones, ionophores, macrolides, nitroimidazole, NSAIDs, β-lactams, penicillins, phenicols, sulfonamides, and tetracyclines. Veterinary drug residues were extracted from milk using a salting-out and solid-phase extraction (SOSPE) procedure, which entailed the precipitation of milk proteins by an extraction buffer (oxalic acid and EDTA, pH 3) and acetonitrile, a salting-out acetonitrile/water phase separation using ammonium sulfate, and solid-phase extraction for clean-up using polymeric reversed-phase sorbent cartridges. The Q-Orbitrap Full MS/dd-MS2 (data-dependent acquisition) was used to acquire product-ion spectra of individual veterinary drugs to build a compound database and a mass spectral library, whereas its Full MS/mDIA was utilized to acquire sample data from milk for target screening of veterinary drugs fortified at 1.0 or 10.0 μg/kg. The in-spectrum mass correction or solvent background lock-mass correction was used to minimize mass error when building the compound database from experimental dd-MS2 accurate mass data. Retention time alignment and response threshold adjustment were used to eliminate or reduce false negatives and/or false positive rates. The validated method was capable of screening 58% and 96% of 105 veterinary drugs at 1.0 and 10.0 μg/kg, respectively, without manually evaluating every compound during data processing, which will reduce the workload in routine practice.

Keywords

UHPLC/ESI Q-Orbitrap Veterinary drug residues Compound database Target screening Milk Multiplexing data-independent acquisition 

Notes

Compliance with ethical standards

Conflict of interest

There is no potential conflict of interest in current study.

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Jian Wang
    • 1
  • Daniel Leung
    • 1
  • Willis Chow
    • 1
  • James Chang
    • 2
  • Jon W. Wong
    • 3
  1. 1.Calgary LaboratoryCanadian Food Inspection AgencyCalgaryCanada
  2. 2.ThermoFisher ScientificSan JoseUSA
  3. 3.Center for Food Safety and Applied NutritionUS Food and Drug AdministrationCollege ParkUSA

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