Analytical and Bioanalytical Chemistry

, Volume 411, Issue 7, pp 1433–1442 | Cite as

Critical assessment of two sample treatment methods for multiresidue determination of veterinary drugs in milk by UHPLC-MS/MS

  • Delia Castilla-Fernández
  • David Moreno-González
  • Miriam Beneito-Cambra
  • Antonio Molina-DíazEmail author
Research Paper


In this work, two sample treatment procedures have been evaluated for the determination of veterinary drug residues in milk. In order to cover a wide range of polarities, a total of 66 veterinary drugs with log Kow ranging from − 1 to 5 were selected. Two sample cleanup steps, (i) dispersive solid-phase extraction (dSPE) using enhanced matrix removal lipid as sorbent and (ii) solid-phase extraction (in pass-through mode) using Oasis HLB PRiME cartridges, were critically assessed in terms of sample throughput, recovery, matrix effect, cleanliness of extracts, limit of quantification, and repeatability. The veterinary drugs tested (viz. benzimidazoles, cephalosporins, imidazothiazoles, macrolides, NSAIDs, penicillins, quinolones, steroids, sulfonamides, and β-agonists) were analyzed by ultra-high-performance liquid chromatography tandem mass spectrometry. According to the results, both methods exhibited similar recovery rates between 70 and 120% for most of compounds tested. Matrix effects were satisfactory for both methodologies, although the tolerance to matrix effects was slightly higher with HLB PRiME with nearly negligible matrix effects in most cases. Limits of quantitation were also well below the current maximum residue levels established by the European Union. Notably, sample throughput was higher in the case of HLB PRiME, since this pass-through SPE cleanup approach involved fewer steps than the EMR-Lipid dSPE approach. The results in terms of analysis time, sensitivity, precision, cleanliness of extracts, and matrix effect showed the suitability of both procedures for the monitoring of veterinary drugs residues in milk samples in a single run.

Graphical abstract


Sample treatment Veterinary drugs Milk HLB PRiME EMR-Lipid UHPLC-MS/MS 



D.C.F. thanks the Andalusian government and European Union for Youth Guarantee research contract (SNGJ-JINV-P-010). D.M.G. thanks the Spanish Ministerio de Economía y Competitividad (MINECO) for a Juan de la Cierva Formación postdoctoral fellowship (Ref. FJCI-2014-19573).

Funding information

This study received funding from Ministerio de Economía y Competitividad (MINECO) (Ref. CTQ-2015-71321-P).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no competing interests.

Supplementary material

216_2019_1582_MOESM1_ESM.pdf (202 kb)
ESM 1 (PDF 201 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • Delia Castilla-Fernández
    • 1
  • David Moreno-González
    • 1
  • Miriam Beneito-Cambra
    • 1
  • Antonio Molina-Díaz
    • 1
    • 2
    Email author
  1. 1.Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, Campus Las LagunillasUniversity of JaénJaénSpain
  2. 2.Center for Advanced Studies in Olives Grove and Olive Oils (CEAOAO), Science and Technology Park GEOLITMengíbarSpain

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