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.
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Format: | artículo biblioteca |
Language: | English |
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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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dig-idaea-es-10261-442192012-01-18T23:00:00Z Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry Kantiani, Lina Farré, Marinella Grases Freixiedas, Josep Manuel Barceló, Damià β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed 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. The performance data and results from the method were compared with those from a previous method developed by our group, using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved sensitivity, with LODs of 0.09–2.12 μgkg−1 compared with 0.12– 3.94 μgkg−1 by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes) and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results. Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of food control and safety. This work was supported by the Spanish Ministry of Science and Innovation, through project CEMAGUA (CGL2007-64551/HID). Waters is acknowledged for providing the SPE cartridges. Lina Kantiani acknowledges the Generalitat de Catalunya (2009FI_B 00660) and the Alexander S. Onassis foundation (F-ZD 029/2007-2008). Peer reviewed 2012-01-13T09:10:28Z 2012-01-13T09:10:28Z 2010 artículo http://purl.org/coar/resource_type/c_6501 Analytical and Bioanalytical Chemistry 1618-2642 http://hdl.handle.net/10261/44219 10.1007/s00216-010-4005-0 1618-2650 en http://dx.doi.org/10.1007/s00216-010-4005-0 none Springer |
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β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed |
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β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed Kantiani, Lina Farré, Marinella Grases Freixiedas, Josep Manuel Barceló, Damià Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
description |
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. |
format |
artículo |
topic_facet |
β-lactams Penicillins Cephalosporins Sulfonamides Online SPE LC–ESI-MS–MS Animal feed |
author |
Kantiani, Lina Farré, Marinella Grases Freixiedas, Josep Manuel Barceló, Damià |
author_facet |
Kantiani, Lina Farré, Marinella Grases Freixiedas, Josep Manuel Barceló, Damià |
author_sort |
Kantiani, Lina |
title |
Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
title_short |
Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
title_full |
Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
title_fullStr |
Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
title_full_unstemmed |
Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
title_sort |
determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry |
publisher |
Springer |
publishDate |
2010 |
url |
http://hdl.handle.net/10261/44219 |
work_keys_str_mv |
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_version_ |
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