Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry
A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μgkg−1. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of the extract with C18HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS). Chromatographic separation was achieved within 10 min by use of a C12 Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1% formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μgkg−1, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μgkg−1 and 22– 182 μgkg−1, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at least one antimicrobial at concentrations between 0.006 and 1.526 mgkg−1.
| Main Authors: | , , , |
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| Format: | artículo biblioteca |
| Language: | English |
| Published: |
Springer
2010
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| Subjects: | β-lactams, Penicillins, Cephalosporins, Sulfonamides, Online SPE, LC–ESI-MS–MS, Animal feed, |
| Online Access: | http://hdl.handle.net/10261/44219 |
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| Summary: | A fully automated method has been developed for
analysis of eighteen antibacterial compounds, including
penicillins, cephalosporins and sulfonamides, in animal feed
with limits of quantification in the range 0.25–5.79 μgkg−1.
The method is based on pressurized liquid extraction of 3 g
homogenized feed with water and online clean-up of 500 μL
of the extract with C18HD cartridges. The purified sample
was directly analysed by liquid chromatography–electrospray
tandem mass spectrometry (SPE–LC–ESI-MS–MS). Chromatographic
separation was achieved within 10 min by use of
a C12 Phenomenex Hydro-RP reversed-phase analytical
column and a mobile phase gradient (water + 0.1% formic
acid–methanol + 0.1% formic acid). The method was
validated, revealing capability for detection of concentrations
as low as 0.09 μgkg−1, decision limits (CCα) and detection
capabilities (CCβ) in the range 10–174 μgkg−1 and 22–
182 μgkg−1, respectively, and inter-day precision ranging
from 0.7 to 8.3%. Recovery, with internal standard correction,
was in the range 93–134% for all analytes. The method was
then applied to analysis of fifteen feed samples, nine of which
contained at least one antimicrobial at concentrations between
0.006 and 1.526 mgkg−1. |
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