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CERTIFICATION REPORT

Certification of mass fractions of nitromidazoles in pork meat

Certified Reference Materials ERM-BB124

EU

R 23574

EN

-2008

The mission of the IRMM is to promote a common and reliable European measurement system in support of EU policies. European Commission Joint Research Centre Institute for Reference Materials and Measurements Contact information Reference materials sales Retieseweg 111 B-2440 Geel, Belgium E-mail: jrc-irmm-rm-sales@ec.europa.eu Tel.: +32 (0)14 571 705 Fax: +32 (0)14 590 406 http://irmm.jrc.ec.europa.eu/ http://www.jrc.ec.europa.eu/ Legal Notice Neither the European Commission nor any person acting on behalf of the Commission is responsible for the use which might be made of this publication.

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A great deal of additional information on the European Union is available on the Internet. It can be accessed through the Europa server http://europa.eu/ EUR 23574 EN ISBN 978-92-79-10654-5 ISSN 1018-5593 DOI 10.2787/94270 Luxembourg: Office for Official Publications of the European Communities European Communities, 2008 Reproduction is authorised provided the source is acknowledged Printed in Belgium

CERTIFICATION REPORT

Certification of mass fractions of nitroimidazoles in pork meat

Certified Reference Materials ERM-BB124

R. Zeleny, H. Schimmel, F. Ulberth, H. Emons

European Commission, Joint Research Centre Institute for Reference Materials and Measurements

Geel, Belgium

Disclaimer

Certain commercial equipment, instruments, and materials are identified in this report to specify adequately the experimental procedure. In no case does such identification imply recommendation or endorsement by the European Commission, nor does it imply that the material or

equipment is necessarily the best available for the purpose.

1

Summary This report describes the preparation of the pork meat matrix reference material ERM-BB124 and the certification of the content (mass fraction) of six nitroimidazole parent drugs and hydroxy metabolites. The preparation and processing of the material, homogeneity and stability studies, and the characterisation are described hereafter and the results are discussed. Uncertainties were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) [1] and include uncertainties due to possible heterogeneity, instability, characterisation, and calibrant uncertainty. The certified values and their uncertainties are listed below:

Nitroimidazole in the reconstituted material

Certified value 1) [g/kg]

Uncertainty 2) [g/kg]

Number of accepted sets of results

Ronidazole (RNZ) 2.09 0.25 11

Metronidazole (MNZ) 1.93 0.15 12

2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI) 0.69 0.09 11

Hydroxymetronidazole (MNZOH) 6.2 0.9 11

Hydroxyipronidazole (IPZOH) 1.67 0.12 11 1) These values are the mass fractions based on the unweighted mean of accepted results. 2) The uncertainties are the expanded uncertainties (k = 2) of the values defined in 1). Additionally, the following certified value has been assigned:

Nitroimidazole in the reconstituted material

Certified value 1) [g/kg]

Dimetridazole (DMZ)

2

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Table of contents Summary ..................................................................................................................................1 Table of contents......................................................................................................................3 1 Glossary ..........................................................................................................................5 2 Introduction......................................................................................................................7

2.1 Background ....................................................................................................................7 2.2 Choice of the material ....................................................................................................7 2.3 Definition of analytes and chemical structures ...............................................................8

3 Participants......................................................................................................................9 4 Processing of the material .............................................................................................10 5 Material characterisation measurements.......................................................................10

5.1 Water content ...............................................................................................................10 5.2 Sieve analysis and particle size measurements...........................................................10

6 Homogeneity study........................................................................................................12 6.1 Minimum sample intake................................................................................................13

7 Stability studies..............................................................................................................14 7.1 Short-term stability study..............................................................................................14 7.2 Long-term stability study ..............................................................................................14

8 Characterisation ............................................................................................................16 8.1 Design of the study.......................................................................................................16 8.2 Results and technical evaluation..................................................................................17

9 Certified values and uncertainties .......................................................................................23 10 Metrological traceability .................................................................................................24 11 Instructions for use ........................................................................................................25

11.1 Safety precautions..................................................................................................25 11.2 Reconstitution of the material .................................................................................25 11.3 Intended use...........................................................................................................25 11.4 Storage conditions..................................................................................................25

12 Acknowledgements .......................................................................................................26 13 References ....................................................................................................................27 Annex A. Homogeneity data...................................................................................................29 Annex B. Short-term stability data..........................................................................................32 Annex C. Long-term stability data ..........................................................................................38

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1 Glossary ANOVA............................Analysis of variances APCI ................................Atmospheric pressure chemical ionisation C18 ...................................Octadecyl silica C8 ....................................Octyl silica CAS.................................Chemical Abstracts Services CC .................................Decision limit CRM ................................Certified reference material d3- ....................................Tri-deuterated compound DAD.................................Diode-array detector DMZ.................................Dimetridazole ERM ................................European Reference Material ESI...................................Electrospray ionisation GC...................................Gas chromatography GC-MS ............................Gas chromatography-mass spectrometry GUM................................Guide to the Expression of Uncertainty in Measurement HMMNI ............................2-hydroxymethyl-1-methyl-5-nitroimidazole HPLC...............................High-performance liquid chromatography IPZ................................... Ipronidazole IPZOH .............................Hydroxy ipronidazole IRMM............................... Institute for Reference Materials and Measurements IUPAC ............................. International Union for Pure and Applied Chemistry LC....................................Liquid chromatography LC-MS/MS.......................Liquid chromatography-tandem mass spectrometry LLE..................................Liquid liquid extraction LOD.................................Limit of detection LOQ.................................Limit of quantification m/m .................................Mass-to-mass MNZ.................................Metronidazole MNZOH ...........................Hydroxy metronidazole MRM................................Multiple reaction monitoring MS...................................Mass spectrometry MSbetween ..........................Mean of squares between groups (ANOV

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