Determination of chloramphenicol in milk powder using liquid-liquid cartridge extraction (Chem Elut) and liquid chromatography-tandem mass spectrometry

• Autorzy: Zawadzka I. , Rodziewicz L.
• Języki publikacji: EN

Abstrakty

EN

Background. The European Union prohibits the use of chloramphenicol (CAP) as a veterinary drug in food-producing animals. Nevertheless, CAP have been detected in milk products (liquid milk and milk powder). Therefore, it is necessary to develop sensitive methods for determining CAP residues in milk powder. Objective. The aim of this study was to develop and validate a confirmatory method for determination of CAP in milk powder. Material and methods. Chloramphenicol was determined in milk powder using LC-ESI-MS/MS in negative mode. After fat removing milk powder sample was extracted/cleaned-up with a Chem Elut extraction cartridge. Separation was achieved on a Phenomenex Luna C-18 column with acetonitrile-water as a mobile phase. The mass spectrometer was operated in multiple reaction monitoring mode (MRM). Four transitions were monitored m/z 321→152, 321→194, 321→257 (CAP) and 326→157 (IS CAP-d5). Results. Linearity, accuracy, precision, decision limit (CCa), detection capability (CCb) and ruggedness were determined for m/z 321→152. The mean relative recoveries (inter standard-corrected) of CAP from whole milk powder spiked at levels 0.1, 0.2, 0.3 and 0.6 mg/kg were in the range 95 - 103%. Relative standard deviation (RSD%) of recoveries at all spiked levels were less than 14%. RSDs within-laboratory reproducibility calculated at fortification of 0.3 mg/kg was less than 16%. CCa and CCb were below 0.1 mg/kg. Conclusions. The developed LC-MS/MS method allows the determination of CAP in milk powder. The method was validated according to the Commission Decision No. 2002/657/EC requirements. This method can be applied to determination CAP in whole and skim milk powder.

PL

Wprowadzenie. Unia Europejska zabroniła stosowania chloramfenikolu (CAP) jako leku weterynaryjnego u zwierząt, których produkty są przeznaczone do spożycia. Pomimo tego, CAP jest wykrywany w produktach mleczarskich (mleko i mleko w proszku). Cel. Celem badań było opracowanie i zwalidowanie metody pozwalającej na oznaczanie CAP w mleku w proszku. Materiał i metoda. CAP był oznaczany w mleku w proszku metodą LC-ESI-MS/MS w trybie jonizacji ujemnej. Po usunięciu tłuszczu próbka była ekstrahowana/oczyszczana za pomocą ekstrakcyjnych kolumienek Chem Elut. Do rozdziału CAP stosowano kolumnę chromatograficzną Phenomenex Luna C-18. Fazę ruchomą stanowił acetonitryl/woda. Spektrometr masowy pracował w trybie monitorowania wybranych reakcji (MRM). Cztery przejścia były monitorowane m/z 321→152, 321→194, 321→257 (CAP) i 326→157 (IS CAP-d5). Wyniki. Liniowość, odzysk, precyzja, limit decyzyjny (CCa), zdolność wykrywania (CCb) i odporność metody zostały wyznaczone dla 321→152. Średni względny odzysk CAP z mleka pełnego był wyznaczony dla próbek wzbogaconych na poziomach odpowiadających 0.1, 0.2, 0.3 i 0.6 mg/kg i mieściły on się w zakresie 95 - 103%. Względne odchylenie stadardowe (RSD%) dla wszystkich poziomów było mniejsze niż 14%. Powtarzalność wewnątrzlaboratoryjna (RSDs) obliczona dla poziomu wzbogacenia 0.3 mg/kg była mniejsza niż 16%. CCa and CCb były poniżej 0.1 mg/kg. Wnioski. Opracowana metoda LC-ESI-Ms/MS pozwala oznaczyć CAP w mleku w proszku. Metoda została zwalidowana zgodnie z wymaganiami decyzji Komisji nr 2002/657/WE. Metoda może być stosowana do mleka pełnego i odtłuszczonego.

Słowa kluczowe

EN

chloramphenicol; determination; milk powder; liquid-liquid extraction; liquid chromatography-tandem mass spectrometry; veterinary drug residue

• Wydawca: -
• Czasopismo: Roczniki Państwowego Zakładu Higieny
• Rocznik: 2014
• Tom: 65
• Numer: 3
• Opis fizyczny: p.185-191,fig.,ref.

Twórcy

autor

Zawadzka I.

• Laboratory of Chemical Examination in Foodstuffs, Department of Hygiene Veterinary, Voivodship Veterinary Inspectorate, Bialystok, Poland

autor

Rodziewicz L.

• Laboratory of Chemical Examination in Foodstuffs, Department of Hygiene Veterinary, Voivodship Veterinary Inspectorate, Bialystok, Poland

Bibliografia

• 1. Commission Decision 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and interpretation of results. Off J Eur Commun 2002;L221:8-36.
• 2. Commission Decision 2003/181/EC of 13 March 2003 amending Decision 2002/657/EC as regards the setting of minimum required performance limits (MRPLs) for certain residues in food of animal origin. Off J Eur Commun 2003; L71:17-18.
• 3. Guy P.A., Royer D., Mottier P., Gremaud E., Perisset, A.,Stadler R.H.: Quantitative determination of chloramphenicol in milk powders by isotope dilution liquid chromatography coupled to tandem mas spectrometry. J Chromatogr A 2004, 1054, 365–371.
• 4. Impens S., Reybroeck W., Vercammen J., Courtheyn D., Ooghe S., De Wasch K., Smedts W., De Brabander H.: Screening and conformation of chloramphenicol in shrimp tissue using ELISA in combination with GC-MS2 an LC-MS2. Anal Chim Acta 2002;483;153-169.
• 5. ISO 11843-2: Capability to Detection (Part I); Terms definitions (Part 2), Methodology in the linear calibration case. 2003.
• 6. Kaufmann A., Butcher P.: Quantitative liquid chromatography/ tandem mass spectrometry determination of chloramphenicol residues in food using sub-2 μm particulate high-performance liquid chromatography columns for sensitivity and speed. Rapid Commun Mass Spectrom 2005;19;3694-3700.
• 7. Mohamed R., Richoz-Payot J., Gremaud E., Mottier P., Yilmaz E., Tabet J., Guy P. A.: Advantages of molecularly imprinted polymers LC-ESI-MS/MS for the selective extraction and quantification of chloramphenicol in milk-based matrixes. Comparison with a classical sample preparation. Anal Chem 2007, 79, 9557–9565.
• 8. Nicolich R.S., Werneck-Barroso E., Sipoli Marques M.A.: Food safety evaluation: Detection and confirmation of chloramphenicol in milk by high performance liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta 2006, 565, 97-102.
• 9. Rezende D., Filho N., Rocha G.: Simultaneous determination of chloramphenicol and florfenicol in liquid milk, milk powder and bovine muscle by LC-MS/MS. Food Addit Contam 2012;29;559-570.
• 10. Rodziewicz L., Zawadzka I.: Rapid determination of chloramphenicol residues in milk powder by liquid chromatography–electrospray ionization tandem mass spectrometry. Talanta 2008, 75, 846–850.
• 11. Rodziewicz L., Zawadzka I.: Determination of chloramphenicol residues in animals tissues by LC-MS/MS method. Rocz Panstw Zakl Hig 2006, 57, 31-38 (in Polish).
• 12. Rodziewicz L., Zawadzka I.: Rapid determination of chloramphenicol residues in honey by liquid chromatography tandem mass spectrometry and the validation of method based on 2002/657/EC. Apiacta 2007, 42, 25-30.
• 13. Rodziewicz L., Zawadzka I.: Determination of chloramphenicol residues in milk powder using molecular imprinted polymers (MIP) by LC-MS/MS. Rocz Panstw Zakl Hig 2010, 3, 249-253 (in Polish).
• 14. Rodziewicz L., Zawadzka I.: Determination of chloramphenicol in animals urine by liquid chromatographytandem mass spectrometry. Bull Vet. Inst Pulawy 2008, 52, 431-434.
• 15. Rønning, H., Einarsen K.,, Asp T.: Determination of chloramphenicol residues in meat, seafood, honey, milk, plasma and urine with liquid chromatography-tandem mass spectrometry, and validation of the method based on 2003/657/EC. J Chromatogr A 2006;118 ; 226-233.
• 16. Sorensen L., Elbaek T.H., Hansen H.: Determination of chloramphenicol in bovine milk by liquid chromatography/tandem mass spectrometry. J AOAC Int 2003, 86, 703-706.
• 17. Zhang S., Zhang Z., Shi W., Eremin S.: Development of a chemiluminescent ELISA for determining chloramphenicol in chicken muscle. J Agric Food Chem 2006;54;5718-5722.