Skip to Content
Merck
  • Determination of nitrofuran and chloramphenicol residues by high resolution mass spectrometry versus tandem quadrupole mass spectrometry.

Determination of nitrofuran and chloramphenicol residues by high resolution mass spectrometry versus tandem quadrupole mass spectrometry.

Analytica chimica acta (2015-02-16)
A Kaufmann, P Butcher, K Maden, S Walker, M Widmer
ABSTRACT

An ultra-high performance liquid chromatography based method, coupled to high resolution mass spectrometry (UHPLC-HRMS), was developed to permit the detection and quantification of various nitrofuran and chloramphenicol residues in a number of animal based food products. This method is based on the hydrolysis of covalently bound metabolites and derivatization with 2-nitrobenzaldehyde. Clean-up is achieved by a liquid/liquid and a reversed phase/solid phase extraction. Not only are the four conventional nitrofurans (nitrofurantoin, furazolidone, nitrofurazone and furaltadone) detected, but also nifursol, nitrovin and nifuroxazide. Furthermore, an underivatizable nitrofuran (nifurpirinol) and another banned drug (chloramphenicol) can be quantified as well. The compounds are detected in the form of their precursor ions, [M+H](+) and [M-H](-), respectively. The mass resolving power of 70,000 FWHM, and the applied mass window ensure sufficient selectivity and sensitivity. Confirmation is obtained by monitoring the HRMS resolved product ions which were derived from the unit-mass resolved precursor ions. The multiplexing capability of the utilized Orbitrap instrument provides not only highly selective, but also sensitive confirmatory signals. This method has been validated according to the CD 2002/657/EC for the following matrices: muscle, liver, kidney, fish, honey, eggs and milk.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
2-Nitrobenzaldehyde, 98%
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Hexane, ReagentPlus®, ≥99%
Sigma-Aldrich
Ammonium hydroxide solution, puriss., meets analytical specification of Ph. Eur., 25-30% NH3 basis
Sigma-Aldrich
Ammonium hydroxide solution, puriss., 30-33% NH3 in H2O
Sigma-Aldrich
Hexane, Laboratory Reagent, ≥95%
Sigma-Aldrich
Ammonium hydroxide solution, puriss. p.a. plus, ≥25% NH3 in H2O
Sigma-Aldrich
Ammonium hydroxide solution, puriss. p.a., reag. ISO, reag. Ph. Eur., ~25% NH3 basis
Sigma-Aldrich
Ammonium hydroxide solution, ACS reagent, 28.0-30.0% NH3 basis
Sigma-Aldrich
Ammonium hydroxide solution, 28% NH3 in H2O, ≥99.99% trace metals basis
Sigma-Aldrich
Hexane, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99% (GC)
Supelco
Hexane, analytical standard
Sigma-Aldrich
Hexane, anhydrous, 95%
Sigma-Aldrich
Ammonium hydroxide solution, BioUltra, ~1 M NH3 in H2O (T)
Sigma-Aldrich
Sodium hydroxide-16O solution, 20 wt. % in H216O, 99.9 atom % 16O
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Chloramphenicol, VETRANAL®, analytical standard
Chloramphenicol, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Hexane, HPLC Plus, for HPLC, GC, and residue analysis, ≥95%
Sigma-Aldrich
Hexane, suitable for HPLC, ≥97.0% (GC)
Sigma-Aldrich
Hexane, suitable for HPLC, ≥95%
Sigma-Aldrich
Chloramphenicol, ≥98% (HPLC)
Sigma-Aldrich
Chloramphenicol, meets USP testing specifications
Sigma-Aldrich
Chloramphenicol, BioReagent, suitable for plant cell culture
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, powder
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, ≥98%, pellets (anhydrous)