The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

Abstract

This paper discusses the analytical challenges to develop a generic extraction procedure to analyze or screen multi-class veterinary drugs in milk and honey using ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC QqTOF MS). The veterinary drugs in this study included aminoglycosides, endectocides, fluoroquinolones, ionophores, b-lactams or penicillins, macrolides, NSAIDs, phenicols, sulfonamides and tetracyclines. Veterinary drugs were extracted using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which entailed the use of acetonitrile containing 1% acetic acid, sodium acetate, ethylenediaminetetra acetic acid disodium (EDTA) and magnesium sulfate, and no clean-up was performed. Chromatographic separation was achieved on a reversed-phase Acquity UPLC BEH C 18 , 100 Â 2.1 mm, 1.7 mm column with 0.1% formic acid and 10 mM ammonium formate in water, and acetonitrile as mobile phases. Due to poor chromatographic retention, aminoglycosides were first dropped from the list, and because of poor extractability, b-lactams and tetracyclines were also excluded from the method. The method was able to quantify 31 or screen up to 54 drugs (unbound) in honey, and to quantify 34 or screen up to 59 drugs in milk. UHPLC QqTOF data were acquired in TOF MS full-scan mode that allowed both quantification and confirmation of veterinary drugs and identification of their degradation products in samples. The method could achieve detection limits as low as 1 mg/kg with analytical range from 1 to 100 mg/kg. The developed method was intended to be used for screening of as many analytes as possible in one single analysis, or unequivocal confirmation of positive findings and degradation product identification based on accurate mass measurement and isotopic patterns.

Comprehensive analysis of toxics (pesticides, veterinary drugs and mycotoxins) in food by UHPLC-MS

“…Wang et al developed a method to be used for screening as many analytes as possible in a single analysis, and aminoglycosides, endectocides, ionophores, NSAIDs were included in the study. However, some families, such as aminoglycosides, ß-lactams and tetracyclines, were excluded from the study [35] because of the diversity of their physicochemical properties.…”

Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry

“…However, there is an increasing effort in the development of multi-class analytical methods capable of detecting a wide range of residues with different chemical and physical properties in the same sample (Kaufmann 2009;Kaufmann, Butcher et al 2011). Several multi-class analytical methods in honey are described in the literature (Debayle, Dessalces et al 2008;Hammel, Mohamed et al 2008;Lopez, Pettis et al 2008;Vidal, Aguilera-Luiz et al 2009;Hou, Xie et al 2011;Bohm, Stachel et al 2012;Gómez-Pérez, Plaza-Bolaños et al 2012;Wang and Leung 2012;Wang, Shi et al 2013;Galarini, Saluti et al 2015;Shendy, Al-Ghobashy et al 2016). Most of these methods are based on solid phase extraction (SPE) for sample preparation and purification, with the aim of enhancing the sensitivity of detection and reduce interferences.…”

Reported prevalence and quantitative LC-MS methods for the analysis of veterinary drug residues in honey: a review

“…Muscle, liver, milk, corn sillage and honey were tested. Aminoglycosides, tetracyclines, macrolides and β-lactams were not recovered well or with satisfactory precision to recommend the QuEChERS approach for the quantification of antimicrobial residues in honey (Filigenzi et al 2011;Wang & Leung 2012).…”

“…While this type of instrumentation does have full-scan capability, it is not designed for the identification of unknown trace contaminants. Triple quadrupole instrumentation tends to give better quantitative precision and improved sensitivity than alternative configurations, making it a superior choice for routine analysis of specific targeted contaminants (Stolker et al 2004;Wang & Leung 2012;Wang & Turnipseed 2012). …”