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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
초록

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
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Supelco
Hydrogen chloride – ethanol solution, ~1.25 M HCl, LiChropur
Sigma-Aldrich
Hydrochloric acid, meets analytical specification of Ph. Eur., BP, NF, fuming, 36.5-38%
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Hydrochloric acid, ACS reagent, 37%
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Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
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Sodium hydroxide, beads, 16-60 mesh, reagent grade, 97%
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Sodium hydroxide, anhydrous, free-flowing, Redi-Dri, reagent grade, ≥98%, pellets
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
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Hydrogen chloride solution, 1.0 M in acetic acid
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Hydrogen chloride solution, 1.0 M in diethyl ether
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Hydrogen chloride solution, 2.0 M in diethyl ether
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Hydrochloric acid, 37 wt. % in H2O, 99.999% trace metals basis
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