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V. G. Amelin, D. S. Bol’shakov
Simultaneous determination of chloramphenicol and chloramphenicol
palmytate residues in food products by liquid chromatography – mass
spectrometry
Abstract
A simple method of sample preparation, identification and determination
of chloramphenicol and chloramphenicol palmitate in food products using
ultra-high-performance liquid chromatography – a high-resolution quadrupole
time-of-flight mass spectrometry using the exact ion masses produced by
electrospray was proposed. The objects of analysis are meat (beef, pork,
poultry), aquaculture products (fish). The preparation consisted in the
extraction of the target components with acetonitrile and diluting the extract
with deionized water 2 times. Five parameters were used for identification: retention
times, the accuracy of the monoisotopic masses of the parent ions, the presence
and accuracy of the monoisotopic masses of the daughter ions, the mSigma
parameter (the theoretical isotopic distribution corresponds to the practical
one) and the monoisotopic masses of the adducts. The features of the
determination of chloramphenicol and chloramphenicol palmitate associated with
the appearance in the electrospray device of deprotonated molecules and adducts
with chloride, formate and trifluoroacetate ions in the detection of negative
ions, as well as the fact that chloramphenicol is eluted during the first
chromatography of the extract (tR = 4,0 min), are considered
and upon repeated chromatography of the acetonitrile-water mixture (1:1, by
volume), chloramphenicol palmitate is eluted (tR = 6,5 min).
A method for determining chloramphenicol and chloramphenicol palmitate by the
method of standard additives using the summation of the peak areas of all
registered ions is proposed. The ranges of the determined contents were 0,1–10
ng/g and 0,5–50 ng/g for chloramphenicol and chloramphenicol palmitate,
respectively. The relative standard deviation of the analysis results did not
exceed 0.15. The analysis time is 50–60 minutes.
Key words: chloramphenicol, chloramphenicol palmitate, ultra-high
performance liquid chromatography – quadrupole time-of-flight high-resolution
mass spectrometry, food analysis.
Copyright (C) Chemistry Dept., Moscow State University, 2002
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