Abstract
Immunoaffinity chromatography (IAC) for simultaneous determination of four fluoroquinolone antibiotics, e.g., norfloxacin (NOR), pefloxacin (PEF), lomefloxacin (LOM), and enrofloxacin (ENRO) from swine and chicken meat samples, was developed. The IAC column was constructed by covalently coupling polyclonal antibody (pAb) against NOR to cyanogen bromide (CNBr)-activated Sepharose 4B and packed into a common solid-phase extraction (SPE) cartridge. It was found that IAC column was able to separately capture NOR, PEF, LOM, and ENRO with a maximum capacity of 200, 336, 352, and 421 ng, respectively. The extraction conditions including loading, washing, and eluting solutions were carefully optimized. Under optimal conditions, the extraction recoveries of the IAC column for NOR, PEF, LOM, and ENRO at two different contents were within 85.8–105.9 %. The IAC column was also applied to real sample extraction. Swine and chicken meat samples were collected and spiked with NOR, PEF, LOM, and ENRO at the content of 20 and 35 ng g−1, respectively. The spiked and unspiked samples were extracted by IAC column and measured by high-performance liquid chromatography (HPLC). It was found that there was no detectable NOR, PEF, LOM, and ENRO in the blank samples, and the extraction recoveries of the IAC for NOR, PEF, LOM, and ENRO from the spiked samples were within 75.3–99.8 % with the relative standard deviation (RSD) of 4.3–12.1 %. The stability of the column was also tested. It was showed that after 30 times repeated usage, 65 % of the maximum capacity was still remained, indicating high reusability of the IAC column. The proposed IAC was proven to be an effectively selective extraction method for NOR, PEF, LOM, and ENRO from swine and chicken meat samples with the properties of high maximum capacity, extraction efficiency, and stability.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Adrian J, Gratacos-Cubarsi M, Sanchez-Baeza F, Regueiro JAG, Castellari M, Marco MP (2009) Traceability of sulfonamide antibiotic treatment by immunochemical analysis of farm animal hair samples. Anal Bioanal Chem 395:1009–1016
Andreu V, Blasco C, Pico Y (2007) Analytical strategies to determine quinolone residues in food and the environment. TrAC Trend Anal Chem 26:534–556
Baggiani C, Baravalle P, Giraudi G, Tozzi C (2007) Molecularly imprinted solid-phase extraction method for the high-performance liquid chromatographic analysis of fungicide pyrimethanil in wine. J Chromatogr A 1141:158–164
Bulletin of the Ministry of Agriculture of the People’s Republic of China, No. 235 (2002) The maxim residue levels (MRLs) of the veterinary drugs in foods of animal origin
Cao BY, He GZ, Yang H, Chang HF, Li SQ, Deng AP (2013a) Development of a highly sensitive and specific enzyme-linked immunosorbent assay (ELISA) for the detection of phenylethanolamine A in tissue and feed samples and confirmed by liquid chromatography tandem mass spectrometry (LC-MS/MS). Talanta 115:624–630
Cao BY, Yang H, Song J, Chang HF, Li SQ, Deng AP (2013b) Sensitivity and specificity enhanced enzyme-linked immunosorbent assay by rational hapten modification and heterogeneous antibody/coating antigen combinations for the detection of melamine in milk, milk powder and feed samples. Talanta 116:173–180
Chen HX, Deng QP, Zhang LW, Zhang XX (2009) Quantification of testosterone and epitestosterone in biological samples by capillary electrophoresis with immunoaffinity extraction. Talanta 78:464–470
Chiffoleau A, Nowoczyn M, Jacob C, Mathieu O, Hillaire-Buy D, Jolliet P (2007) Fluoroquinolone psychiatric adverse effects: review of French Pharmacovigilance data base. Fundam Clin Pharmacol 21:61
Ding T, Shen DX, Xu JZ, Wu B, Chen HL, Shen CY, Shen WJ, Zhao ZY, Liao HZ (2009) Simultaneous determination of 19 quinolone residues in honey using high performance liquid chromatography-tandem mass spectrometry. Chin J Chromatogr 27:34–38
Dufresne G, Fouquet A, Forsyth D, Tittlemier SA (2007) Multiresidue determination of quinolone and fluoroquinolone antibiotics in fish and shrimp by liquid chromatography/tandem mass spectrometry. J AOAC Int 90:604–612
EC/470/2009 (2009) Regulation (EC) No 470/2009 laying down Community procedures for the establishment of residue limits of pharmacologically active substances in foodstuffs of animal origin, repealing Council Regulation (EEC) No 2377/90 and amending Directive 2001/82/EC of the European Parliament and of the Council and Regulation (EC) No 726/2004 of the European Parliament and of the Council. J Eur Union L152:111–122
ECC/2377/90 (1990) Council Regulation (ECC) No. 2377/90 laying down a community procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin. Off J Eur Union L224:221–228
Han D, Yu M, Knopp D, Niessner R, Wu M, Deng AP (2007) Development of a highly sensitive and specific enzyme-linked immunosorbent assay for detection of Sudan I in food samples. J Agric Food Chem 55:6424–6430
He L, Pu C, Yang H, Zhao D, Deng AP (2009) Development of a polyclonal indirect ELISA with sub-ng g(−1) sensitivity for the analysis of clenbuterol in milk, animal feed, and liver samples and a small survey of residues in retail animal products. Food Addit Contam Part A 26:1153–1161
Hernandez-Arteseros JA, Barbosa J, Compano R, Prat MD (2002) Analysis of quinolone residues in edible animal products. J Chromatogr A 945:1–24
Hou XL, Chen G, Zhu L, Yang T, Zhao J, Wang L, Wu YL (2014) Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk. J Chromatogr B 962:20–29
Lara FJ, Garcia-Campana AM, Ales-Barrero F, Bosque-Sendra JM, Garcia-Ayuso LE (2006) Multiresidue method for the determination of quinolone antibiotics in bovine raw milk by capillary electrophoresis-tandem mass spectrometry. Anal Chem 78:7665–7673
Li C et al (2008) Development of an immunoaffinity column method using broad-specificity monoclonal antibodies for simultaneous extraction and cleanup of quinolone and sulfonamide antibiotics in animal muscle tissues. J Chromatogr A 1209:1–9
Licata A, Randazzo C, Morreale I, Butera G, D’Alessandro N, Craxi A (2012) Fluoroquinolone-induced liver injury: three new cases and a review of the literature. Eur J Clin Pharmacol 68:525–532
Martinez M, McDermott P, Walker R (2006) Pharmacology of the fluoroquinolones: a perspective for the use in domestic animals. Vet J 172:10–28
Mi JB, Wang S, Ding XJ, Guo ZQ, Zhao MP, Chang WB (2006) Efficient purification and preconcentration of erythropoietin in human urine by reusable immunoaffinity column. J Chromatogr B 843:125–130
Mulgaonkar A, Venitz J, Sweet DH (2012) Fluoroquinolone disposition: identification of the contribution of renal secretory and reabsorptive drug transporters. Exp Opin Drug Metab 8:553–569
Senyuva HZ, Gilbert J (2010) Immunoaffinity column clean-up techniques in food analysis: a review. J Chromatogr B 878:115–132
Tsikas D (2010) Quantitative analysis of biomarkers, drugs and toxins in biological samples by immunoaffinity chromatography coupled to mass spectrometry or tandem mass spectrometry: a focused review of recent applications. J Chromatogr B 878:133–148
Wang J, MacNeil JD, Kay JF (2012) Chemical analysis of antibiotic residues in food. Wiley, Hoboken
Wang ZH, Zhang HY, Ni HJ, Zhang SX, Shen JZ (2014) Development of a highly sensitive and specific immunoassay for enrofloxacin based on heterologous coating haptens. Anal Chim Acta 820:152–158
Zeng ZL, Dong AG, Yang GX, Chen ZL, Huang XH (2005) Simultaneous determination of nine fluoroquinolones in egg white and egg yolk by liquid chromatography with fluorescence detection. J Chromatogr B 821:202–209
Zhang W, Wang HH, Wang JP, Li XW, Jiang HY, Shen JZ (2006) Multiresidue determination of zeranol and related compounds in bovine muscle by gas chromatography/mass spectrometry with immunoaffinity cleanup. J AOAC Int 89:1677–1681
Zhao MP, Liu Y, Li YZ, Zhang XX, Chang WB (2003) Development and characterization of an immunoaffinity column for the selective extraction of bisphenol A from serum samples. J Chromatogr B 783:401–410
Zhu QZ, DeGelmann P, Niessner R, Knopp D (2002) Selective trace analysis of sulfonylurea herbicides in water and soil samples based on solid-phase extraction using a molecularly imprinted polymer. Environ Sci Technol 36:5411–5420
Acknowledgments
The authors thank the National Natural Science Foundation of China (NSFC, contact nos. 20835003, 21075087, and 21175097) and a Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions for financial support of this study.
Conflict of Interest
Lulu Sun declares that she has no conflict of interest. Liyun Mei declares that she has no conflict of interest. Hong Yang declares that he has no conflict of interest. Kang Zhao declares that he has no conflict of interest. Jianguo Li declares that he has no conflict of interest. Danni Jiang declares that he has no conflict of interest. Mingxing Li declares that he has no conflict of interest. Mingxin Li declares that he has no conflict of interest. Anping Deng declares that he has no conflict of interest. All institutional and national guidelines for the care and use of laboratory animals were followed.
Author information
Authors and Affiliations
Corresponding authors
Rights and permissions
About this article
Cite this article
Sun, L., Mei, L., Yang, H. et al. Development and Application of Immunoaffinity Column for the Simultaneous Determination of Norfloxacin, Pefloxacin, Lomefloxacin, and Enrofloxacin in Swine and Chicken Meat Samples. Food Anal. Methods 9, 342–352 (2016). https://doi.org/10.1007/s12161-015-0192-9
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-015-0192-9