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Certified Reference Materials for Reliable Measurements of Oxytetracycline in Milk
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Oxytetracycline (OTC) is a broad-spectrum antibiotic highly effective against many bacteria. It is approved for use in a variety of food-producing animals, and widely used in lactating and non-lactating dairy cattle for treatment of bacterial infections such as enteritis, pneumonia, and diphtheria. A maximum residue limit (MRL) of 100 μg OTC/kg milk has been stipulated in the legislation to protect consumers from possible adverse side effects.
Effective consumer protection however relies on accurate measurements, and certified reference materials
(CRMs) are highly valuable tools for laboratories for the validation, and performance verification of their methods. IRMM produced a set of two certified reference material, consisting of ERM-BB492 - oxytetracycline in partially skimmed milk, and ERM-BB493 - partially skimmed milk blank material.
As matrix format, spray-dried milk powder was chosen, as it best meets the requirements of suitable stability while assuring good reconstituteability. Homogeneity and stability of the material was assessed by measurements with liquid chromatography tandem mass spectrometry (LC-MS/MS). The relative standard uncertainty due to possible heterogeneity was found to be 3.0 %, and no significant instability was detected during storage at -20 ºC for a shelf life of two years. The certified values were established in an inter-comparison with 12 expert laboratories using different sample preparation procedures with subsequent LC-UV or LC-MS/MS methods for analysis.
The certified value for ERM-BB492 amounts to 101 ± 11 μg/kg (mean ± expanded uncertainty). For ERM-BB493, the certified value was established as "below 5 μg/kg with a 95% level of confidence", and corresponds to the LOQ of the most sensitive method in the intercomparison. Both values are traceable to the International System of Units (SI). The materials shall be used for validation (trueness determination) and method performance verification of screening and confirmatory methods.
European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, 2440 Geel, Belgium
This poster was presented at HPLC 2011, 19 - 23 June in Budapest, Hungary.
Please click here to read the poster as a PDF
Contact
Reinhard Zeleny
European Commission • Joint Research Centre
Institute for Reference Materials and Measurements
Tel.: +32 14 571615 • Fax +32 14 571548
reinhard.zeleny@ec.europa.eu
http://www.erm-crm.org/
http://irmm.jrc.ec.europa.eu/
Authors:
Reinhard Zeleny
Heinz Schimmel
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Keywords : certified reference material CRM European Commission Food Food Quality Heinz Schimmel HPLC 2011 Poster Poster HPLC Reinhard Zeleny Standard
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