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http://dx.doi.org/10.13103/JFHS.2018.33.1.58

Analytical Method for Determination of Cephalexin in Bovine Edible Tissues using Liquid Chromatography Coupled to Tandem Mass Spectrometry  

Chae, Won-Seok (Department of Chemistry, Daejin University)
Lee, Sung Joong (Department of Chemistry and Research Institute of Live Science, Gyeongsang National University)
Son, Song-Ee (Institute of Animal Medicine and College of Veterinary Medicine, Gyeongsang National University)
Kim, Suk (Institute of Animal Medicine and College of Veterinary Medicine, Gyeongsang National University)
Lee, Hu-Jang (Institute of Animal Medicine and College of Veterinary Medicine, Gyeongsang National University)
Publication Information
Journal of Food Hygiene and Safety / v.33, no.1, 2018 , pp. 58-64 More about this Journal
Abstract
An analytical method for the determination of cephalexin (CEX) in bovine tissues (muscle, liver, kidney and fat tissues) was developed and validated using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Tissue samples were extracted by the liquid-liquid extraction based on 5% trichloroacetic acid (TCA). The chromatographic separation was achieved on a reverse phase $C_{18}$ column with gradient elution using a mobile phase of 20 mM hexafluroacetylacetone (HFAC)/50% acetonitrile (40:60). The procedure was validated according to the Ministry of Food and Drug Safety guideline determining accuracy, precision, and limit of detection. Mean recoveries of CEX from spiked edible tissues ($6{\sim}1,500{\mu}g/kg$) were 83.9~106.8%, and the relative standard deviation was between 2.3 and 14.8%. Linearities were obtained with the correlation coefficient ($r^2$) of > 0.999. Limit of detection and limit of quantification for the investigated CEX were 2~10 and $6{\sim}30{\mu}g/kg$, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of CEX residues in bovine edible tissues.
Keywords
Cephalexin; Bovine edible tissues; LC-MS/MS;
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1 Ministry of Agriculture, Food and Rural Affairs (MAFRA), Animal and Plant Quarantine Agency (APQA) and National Institute of Food and Drug Safety Evaluation (NIFDS).: National antimicrobial usage and resistance monitoring in 2015 - livestock and animal products. MAFRA, Sejong, Korea, pp. 9-10 (2016).
2 Heo, J.H., Cho, M.H., Lee, K.C., Park, M.N., Cho, E.J., Choi, M.S., Kim, C.H., Kang, J.B., Kim, E. and Kim, J.S.: An epidemiological study on the calves with clinical diarrhea in southern Gyeongnam. Korean J. Vet. Serv. 31, 305-313 (2008).
3 Son, B., Kim, J., An, C., Lee, S. and Kim, B., Chung, D.: Simultaneous analysis of ${\beta}$-lactam antibiotics and ${\beta}$-blockers by LC-MS/MS. Anal. Sci. Technol. 29, 179-185 (2016).   DOI
4 Carretero, V., Blasco, C. and Pico, Y.: Multi-class determination of antimicrobials in meat by pressurized liquid extraction and liquid chromatography-tandem mass spectrometry. J. Chromatogr. A. 1209, 162-173 (2008).   DOI
5 The European Agency for the Evaluation of Medical Products (EMEA).: Cefalexin - summary report. Committee for veterinary medicinal products. Veterinary Medicines Evaluation Unit (EMEA/MRL/627/99) (1999).
6 Codex guidelines for the establishment of a regulatory programme for control of veterinary drug residues in foods (CAC/GL 16) (1993).
7 Validation guidelines, Codex committee on residues of veterinary drugs in foods, 11th session (1998).
8 Mainero Rocca, L., Gentili, A., Perez-Fernandez, V. and Tomai, P.: Veterinary drugs residues: a review of the latest analytical research on sample preparation and LC-MS based methods. Food Addit. Contam. Part A Chem. Anal. Control Expo. Risk Assess. 34, 766-784 (2017).
9 Farouk, F., Azzazy, H.M. and Niessen, W.M.: Challenges in the determination of aminoglycoside antibiotics, a review. Anal. Chim. Acta. 890, 21-43 (2015).   DOI
10 Moreno-Bondi, M.C., Marazuela, M.D., Herranz, S. and Rodriguez, E.: An overview of sample preparation procedures for LC-MS multiclass antibiotic determination in environmental and food samples. Anal. Bioanal. Chem. 395, 921-943 (2009).
11 Sawant, A.A., Sordillo, L.M. and Jayarao, B.M.: A survey on antibiotic usage in dairy herds in pennsylvania. J. Dariy Sci. 88, 2991-2999 (2005).   DOI
12 Fisher, J.F., Meroueh, S.O. and Mobashery, S.: Bacterial resistance to beta-lactam antibiotics: compelling opportunism, compelling opportunity. Chem. Rev. 105, 395-424 (2005).   DOI
13 Drawz, S.M. and Bonomo, R.A.: Three decades of beta-lactamase inhibitors. Clin. Microbiol. Rev. 23, 160-201 (2010).   DOI
14 Ministry of Food and Drug Safety (MFDS).: Korean Food Standards Codex. Appendix 6: Maximum residue limits of veterinary drugs in food. MFDS, Cheongju, Korea, pp. 21 (2017).
15 The European Agency for the Evaluation of Medical Products.: Committee for veterinary medicinal products cephalexin summary report: EMEA/MRL/627/99-FINAL. Veterinary Medicines Evaluation Unit, London, U.K., pp. 8 (1999).
16 Panda, S.S., Ravi, K., Bera, V.V., Dash, R. and Mohanta, G.: Determination of cephalexin monohydrate in pharmaceutical dosage form by stability-indicating RP-UFLC and UV spectroscopic methods. Sci. Pharm. 81, 1029-1036 (2013).   DOI
17 Regina, V.O., Angela, C.D. and Quezia, B.C.: Quantification of cephalexin as residue levels in bovine milk by high-performance liquid chromatography with on-line sample cleanup. Talanta. 71, 1233-1238 (2007).   DOI
18 Jeswani, R.M., Sinha, P.K., Topagi, K.S., Damle, M.C.: A validated stability indicating HPTLC method for determination of cephalexin in bulk and pharmaceutical formulation. Int. J. Pharm. Tech. Res. 1, 527-536 (2009).
19 Edward, P.C. and Stanley, G.W.: Molecularly imprinted solid phase extraction for rapid screening of cephalexin in human plasma and serum. Anal. Chim. Acta. 481, 165-174 (2003).
20 Argekara, A.P., Raja, S.V. and Kapadiaa, S.U.: Simultaneous determination of cephalexin and carbocisteine from capsules by reverse phase high performance liquid chromatography (RP-HPLC). Anal. Lett. 30, 821-831 (1997).   DOI
21 Kim, M.R., Choi, Y.H., Choi, H., Kim, D.H., Kim, Y.S. and Lee, J.H.: Monitoring for cephalosporins residues in raw meat in Seoul. Korean J. Vet. Serv. 38, 259-264 (2015).
22 Li, W., Shen, H., Hong, Y., Zhang, Y., Yuan, F. and Zhang, F.: Simultaneous determination of 22 cephalosporins drug residues in pork muscle using liquid chromatography-tandem mass spectrometry. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 1022, 298-307 (2016).   DOI
23 Liu, X., Yu, Y., Zhao, M., Zhang, H., Li, Y. and Duan, G.: Solid phase extraction using magnetic core mesoporous shell microspheres with C18-modified interior pore-walls for residue analysis of cephalosporins in milk by LC-MS/MS. Food Chem. 150, 206-212 (2014).   DOI
24 Pecavar, A., Smidovnik, A., Milivojevic, D. and ProSek, M.: A reversed phase high-performance liquid chromatographic method for determination of cephalexin in human plasma. J. High Resol. Chrornatogr. 20, 674-678 (1997).
25 Perez-Burgos, R., Grzelak, E.M., Gokce, G., Saurina, J., Barbosa, J. and Barron, D.: Quechers methodologies as an alternative to solid phase extraction (SPE) for the determination and characterization of residues of cephalosporins in beef muscle using LC-MS/MS. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 899, 57-65. (2012).   DOI
26 Chen, H., Li, X. and Zhu, S.: Occurrence and distribution of selected pharmaceuticals and personal care products in aquatic environments: a comparative study of regions in China with different urbanization levels. Environ. Sci. Pollut. Res. Int. 19, 2381-2389 (2012).   DOI
27 Lee, Y.J. and Lee, H.S.: Simultaneous determination of cefoxitin, cefuroxime, cephalexin and cephaloridine in plasma using HPLC and a column-switching technique. Chromatographia. 30, 80-84 (1990).   DOI
28 Ministry of Food and Drug Safety (MFDS).: Korean Food Standards Codex. Chapter 7. General analytical method, 5. Monitoring of veterinary drug residues in foods. MFDS, Cheongju (2016).
29 Li, W., Shen, H., Hong, Y., Zhang, Y., Yuan, F. and Zhang, F.: Simultaneous determination of 22 cephalosporins drug residues in pork muscle using liquid chromatography-tandem mass spectrometry. J. Chromatogr. B. 1022, 298-307 (2016).   DOI
30 National Institute of Food and Drug Safety Evaluation (NIFDS).: Handbook of residue analytical methods for veterinary drugs in food. NIFDS, Cheongju, Korea, pp. 3-4 (2014).