Skip to Content
Merck
CN
  • The development and validation of a rapid method for the determination of antimicrobial agent residues in milk and meat using ultra performance liquid chromatography coupled to quadrupole--Orbitrap mass spectrometry.

The development and validation of a rapid method for the determination of antimicrobial agent residues in milk and meat using ultra performance liquid chromatography coupled to quadrupole--Orbitrap mass spectrometry.

Journal of pharmaceutical and biomedical analysis (2014-10-06)
Guntis Cepurnieks, Jekaterina Rjabova, Dzintars Zacs, Vadims Bartkevics
ABSTRACT

A new multi-class method has been developed for the identification and quantification of the residues of 26 antibiotics from different classes (sulfonamides, macrolides, tetracyclines, penicillins, and quinolones) in milk and meat by ultra performance liquid chromatography coupled to hybrid quadrupole - high resolution Orbitrap mass spectrometry (UPLC-qOrbitrap). The sample preparation included extraction of two analytical portions with acetonitrile and 5% trichloroacetic acid, respectively, followed by centrifugation and filtration. The method was validated over three days at 50% of MRL (maximum residue limit) set in the European Union. Experiments on spiked meat and milk samples showed that the average recovery of the antibiotics ranged from 83% to 112%, and the coefficients of variation were between 8.9% and 39%.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Erythromycin, meets USP testing specifications
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Supelco
Sulfadimethoxine, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Supelco
Sulfadimethoxine, 98.0-102.0%
Sigma-Aldrich
Methanol, purification grade, 99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Erythromycin, potency: ≥850 μg per mg
Sigma-Aldrich
Sulfamethazine, 99.0-101.0% (on dried basis)
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Supelco
Sulfadimethoxine, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Enrofloxacin for system suitability, European Pharmacopoeia (EP) Reference Standard
Marbofloxacin, European Pharmacopoeia (EP) Reference Standard
Supelco
Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
Sulfadimethoxine for peak identification, European Pharmacopoeia (EP) Reference Standard
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Methanol, analytical standard
Supelco
Marbofloxacin, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%