Target screening of 105 veterinary drug residues in milk using UHPLC/ESI Q-Orbitrap multiplexing data independent acquisition
- 750 Downloads
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.
KeywordsUHPLC/ESI Q-Orbitrap Veterinary drug residues Compound database Target screening Milk Multiplexing data-independent acquisition
Compliance with ethical standards
Conflict of interest
There is no potential conflict of interest in current study.
- 5.Schiffmann AP, Schütz M, Wiesner HU. False negative and positive results in testing for inhibitory substances in milk. Milchwissenschaft. 1992;47:712–5.Google Scholar
- 11.Wang J, Leung D, Chow W, Chang J, Wong JW. Development and validation of a multiclass method for analysis of veterinary drug residues in milk using ultrahigh performance liquid chromatography electrospray ionization quadrupole Orbitrap mass spectrometry. J Agric Food Chem. 2015;63:9175–87.CrossRefPubMedGoogle Scholar
- 15.Wang J, Chow W, Chang J, Wong JW. Development and validation of a qualitative method for target screening of 448 pesticide residues in fruits and vegetables using UHPLC/ESI Q-Orbitrap based on data-independent acquisition and compound database. J Agric Food Chem. 2017;65:473–93.CrossRefPubMedGoogle Scholar
- 16.Pérez-Ortega P, Lara-Ortega FJ, Gilbert-López B, Moreno-González D, García-Reyes JF, Molina-Díaz A. Screening of over 600 pesticides, veterinary drugs, food-packaging contaminants, mycotoxins, and other chemicals in food by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Food Anal Method. 2017;10:1216–44.CrossRefGoogle Scholar
- 17.European Union. Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. SANTE/11945/2015 Supersedes SANCO/12571/2013 Implemented by 01/01/2016. http://ec.europa.eu/food/plant/docs/pesticides_mrl_guidelines_wrkdoc_11945.pdf. Accessed 10 Oct 2016
- 19.Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. 2002/657/EC. Off J Eur Communities 2002;L221:8–36Google Scholar