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Kantiani L.,CSIC - Institute of Environmental Assessment And Water Research | Farre M.,CSIC - Institute of Environmental Assessment And Water Research | Grases I Freixiedas J.M.,Laboratori Agroalimentari Of Catalonia | Barcelo D.,CSIC - Institute of Environmental Assessment And Water Research | Barcelo D.,Catalan Institute for Water Research
Analytical and Bioanalytical Chemistry | Year: 2010

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 μg kg-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 μg kg-1, decision limits (CCα) and detection capabilities (CCβ) in the range 10-174 μg kg-1 and 22-182 μg kg -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 mg kg-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 μg kg-1 compared with 0.12-3.94 μg kg-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. © 2010 Springer-Verlag.

Kantiani L.,CSIC - Institute of Environmental Assessment And Water Research | Farre M.,CSIC - Institute of Environmental Assessment And Water Research | Freixiedas J.M.G.I.,Laboratori Agroalimentari Of Catalonia | Barcelo D.,CSIC - Institute of Environmental Assessment And Water Research | Barcelo D.,King Saud University
Journal of Chromatography A | Year: 2010

This study presents the development and validation of a sensitive and fast (30. min extraction time and 10. min chromatographic run) method for the detection of penicillins, cephalosporins and sulfonamides in animal feed using pressurised liquid extraction and solid phase extraction as extraction and pre-concentration procedures, followed by liquid chromatography-quadrupole-linear ion-trap mass spectrometry. The developed method was validated showing limits of detection ranging from 0.12 (ampicillin) to 3.94. ng/g (amoxicillin), instrumental and analytical linearity coefficients above 0.99 in both standard and matrix-based solutions as well as relative recoveries ranging from 71% (cefoperazone) to 115% (cefazolin). Repeatability of the method was in the range of 1-9% (RSD %), whereas reproducibility ranged from 3% to 13% (RSD %). The developed and validated method was finally applied to the analysis of real feed samples. The results showed 10 out of 18 analytes to be present in at least one sample and all 14 samples to contain at least one analyte. Penicillin V, oxacillin, ceftiofur, cefoperazone, cefalexin, cefazolin, sulfamethoxypyridazine and sulfapyridine were not detected in any of the samples analysed. Considering the ban of antibacterials as growth promoters added in animal feed, this method is capable of detecting the low concentrations that could result from failure to comply with the regulations or on-site contamination. © 2010 Elsevier B.V.

Borras S.,University of Barcelona | Companyo R.,University of Barcelona | Guiteras J.,University of Barcelona | Bosch J.,Laboratori Agroalimentari Of Catalonia | And 2 more authors.
Analytical and Bioanalytical Chemistry | Year: 2013

A rapid multiclass method that covers 50 antimicrobials from 13 different families in animal feeds was developed. Samples were extracted using a mixture of methanol, acetonitrile and a McIlvaine buffer combined with sonication. Feed extracts were simply diluted prior to injection, since the clean-up strategies that were tested, based on either solid-phase extraction or dispersive solid-phase extraction, were ineffective at minimizing matrix-related signal suppression/enhancement. Analysis was carried out by liquid chromatography coupled to tandem mass spectrometry using an electrospray ionization source operating in positive and negative modes. For the quantification, matrix-fortified standard calibration curves were used to compensate for matrix effects and losses in sample preparation. The method was validated in-house in pig, poultry and cattle feed matrices and showed satisfactory performance characteristics. Thus, the proposed approach was suitable for application in a routine high-throughput laboratory for the official control of feeds. [Figure not available: see fulltext.] © 2013 Springer-Verlag Berlin Heidelberg.

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