Production and certification of BOTS-1: bovine muscle–certified reference material for incurred veterinary drug residues

• Published in: Analytical and bioanalytical chemistry 2024, Vol.416 (3), p.759-771
• Main Authors: McRae, Garnet, Leek, Donald M., Meija, Juris, Shurmer, Bryn, Lehotay, Steven J., Polzer, Joachim, Melanson, Jeremy E., Mester, Zoltan
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Animals; Biochemistry; Canada; Cattle; Certification; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chlorpromazine; Chromatography, Liquid - methods; Ciprofloxacin; Clenbuterol; Consumer protection; Dexamethasone; Dilution; Drug Residues; Drugs; Enrofloxacin; Food inspection; Food Safety Analysis 2.0; Food Science; Fractions; Inhomogeneity; Isotopes; Laboratory Medicine; Liquid chromatography; Mass spectrometry; Mass spectroscopy; Meloxicam; Monitoring/Environmental Analysis; Muscles; NMR; Nuclear magnetic resonance; Reference materials; Reference Standards; Research Paper; Residues; Stable isotopes; Sulfadiazine; Tandem Mass Spectrometry - methods; Veterinary Drugs; Veterinary medicine
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-023-04794-5

A freeze-dried bovine muscle–certified reference material (CRM), known as BOTS-1 (DOI: https://doi.org/10.4224/crm.2018.bots-1 ), containing incurred residues of commonly used veterinary drugs was produced and certified for the mass fraction of eight veterinary drug residues. Value assignment was carried out using liquid chromatography tandem mass spectrometry (LC–MS/MS) methods in conjunction with isotope dilution and standard addition approaches involving stable isotope internal standards. Data from the National Research Council of Canada (NRC), Canadian Food Inspection Agency (CFIA), United States Department of Agriculture (USDA), and the Federal Office of Consumer Protection and Food Safety in Germany (BVL) were used for value assignment. Results for two drug residues were also obtained through an international inter-laboratory comparison CCQM-K141/P178 organized under the auspices of the International Bureau of Weights and Measures (BIPM). Quantitative NMR ( 1 H-qNMR) was used to characterize primary standards of all veterinary drugs certified. The certified mass fractions of the veterinary drug residues were 490 ± 100 µg/kg for chlorpromazine, 44 ± 4.4 µg/kg for ciprofloxacin, 3.3 ± 1.4 µg/kg for clenbuterol, 9.5 ± 0.8 µg/kg for dexamethasone, 57 ± 4.8 µg/kg for enrofloxacin, 3.0 ± 0.4 µg/kg for meloxicam, 12.4 ± 1.2 µg/kg for ractopamine, and 2290 ± 120 µg/kg for sulfadiazine with expanded uncertainties quoted (95% confidence) which include the effects due to between-bottle inhomogeneity, instability during long-term storage and transportation, and characterization.