Abstract
A confirmatory analytical method for simultaneous determination of nine regulated quinolones (Council Regulation 2377/90/ECC) in six matrices of animal origin is proposed. The sample pretreatment involves double step liquid extraction with acetonitrile and purification by solid-phase extraction on Oasis HLB cartridges. The quinolones were separated by liquid chromatography on C18 Zorbax column with gradient elution program. Aqueous formic acid, methanol, and acetonitrile were used as a mobile phase. A multi-wavelength excitation/emission program was used for sensitive fluorescence detection of quinolones. The proposed sample pretreatment protocol was applied to each of the six studied matrices without any modification. The method was validated according to Commission Decision 2002/657 EC. Residues were quantified down to 15 μg kg−1 with limits of detection and quantification ranging from 3 to 50 μg kg−1 and from 7.5 to 100 μg kg−1, respectively. The recoveries at the maximum residual limits (MRLs) were between 77 and 120 % with RSD values lower than 30 %. For quinolones without established MRL or maximum required performance limit, the accuracy and precision of the method were estimated at concentration levels corresponding to the lowest linear calibration point and recoveries between 70 and 130 % were achieved. Decision limits, detection capability, and linear range in eggs, milk, fish, ovine muscle, chicken muscle, and porcine kidney are also reported.
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs12161-012-9488-1/MediaObjects/12161_2012_9488_Fig1_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs12161-012-9488-1/MediaObjects/12161_2012_9488_Fig2_HTML.gif)
![](http://media.springernature.com/m312/springer-static/image/art%3A10.1007%2Fs12161-012-9488-1/MediaObjects/12161_2012_9488_Fig3_HTML.gif)
Similar content being viewed by others
References
Aguilera-Luiz MM, Vidal JLM, Romero-González R, Frenich AG (2008) J Chromatogr A 1205:10
Aguilera-Luiz MM, Vidal JLM, Romero-González R, Frenich AG (2012) Food Chem 132:2171
Andreu V, Blasco C, Pico Y (2007) Trends Anal Chem 26:534
Bailac S, Ballesteros O, Jimenez-Lozano E, Barron D, Sanz-Nebot V, Navalon A, Vilchez JL, Barbosa J (2004) J Chromatogr A 1029:145
Bohm DA, Stachel CS, Gowik P (2009) J Chromatogr A 1216:8217
Chang C-S, Wang W-H, Tsai C-E (2010) J Food Drug Anal 18:87
Choi J-H, Mamun MIR, Abd El-Aty AM, Park J-H, Shin E-H, Park JY, Cho S-K, Shin SC, Lee KB, Shim J-H (2011) Food Chem 127:1878
Christodoulou EA, Samanidou VF, Papadoyannis IN (2007) J Chromatogr B 859:246
Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results, Official Journal of the European Communities L221/8/17.8.2002
Frenich AG, Aguilera-Luiz MM, Vidal JLM, Romero-González R (2010) Anal Chim Acta 661:150
Galarini R, Fioroni L, Angelucci F, Tovo G, Cristofani E (2009) J Chromatogr A 1216:8158
Hassouan MK, Ballesteros O, Zafra A, Vilchez JL, Navalon A (2007a) J Chromatogr B 859:282
Hassouan M, Ballesteros O, Taoufiki J, Vilchez J, Cabrera-Aguilera M, Navalon A (2007b) J Chromatogr B 852:625
He H-B, Lv X-X, Yu Q-W, Feng Y-Q (2010) Talanta 82:1562
Hermo MP, Nemutlu E, Kir S, Barron D, Barbosa J (2008a) Anal Chim Acta 613:98
Hermo M, Barron D, Barbosa J (2008b) J Chromatogr A 1201:1
Hernandez-Arteseros JA, Barbosa J, Compano R, Prat MD (2002) J Chromatogr A 945:1
Herrera-Herrera AV, Hernandez-Borges J, Rodriguez-Delgado MA, Herrero M, Cifuentes A (2011) J Chromatogr A 1218:7608
Ho C, Sin D, Tang H, Chung L, Siu A (2004) J Chromatogr A 1061:123
Jimenez V, Companyo R, Guiteras J (2011a) Talanta 85:596
Jimenez V, Rubies A, Centrich F, Companyo R, Guiteras J (2011b) J Chromatogr A 1218:1443
Junza A, Amatya R, Barron D, Barbosa J (2011) J Chromatogr B 879:2601
Kantiani L, Farre M, Barcelo D (2011) J Chromatogr A 1218:9019
Lombardo-Agui M, Gamiz-Gracia L, Cruces-Blanco C, Garcia-Campana AM (2011) J Chromatogr A 1218:4966
Marazuela MD, Bogialli S (2009) Anal Chim Acta 645:5–17
Pecoreli I, Galarini R, Bibi R, Al F, Casciarri E, Floridi A (2003) Anal Chim Acta 483:81
Prat MD, Benito J, Compano R, Hernandez-Arteseros JA, Grandos M (2004) J Chromatogr A 1041:27
Prieto A, Schrader S, Bauer C, Moder M (2011) Anal Chim Acta 685:146
Rubies A, Vaquerizo R, Centrich F, Compano R, Granados M, Prat MD (2007) Talanta 72:269
Runnqvist H, Bak SA, Hansen M, Styrishave B, Halling-Sørensen B, Björklund E (2010) J Chromatogr A 1217:2447
Samanidou V, Evaggelopoulou E, Trotzmuller M, Guo X, Lankmayr E (2008) J Chromatogr A 1203:115
Scortichini G, Annunziata L, Girolamo V, Buratti R, Galarini R (2009) Anal Chim Acta 637:273
Seifrtova M, Novakova L, Lino C, Pena A, Solich P (2009) Anal Chim Acta 649:158
Si-Jun Z, Cun L, Hai-Yang J, Bing-Yu L, Jian-Zhong S (2007) Chin J Anal Chem 35:786
Stolker AAM, Brinkman UAT (2005) J Chromatogr A 1067:15
Stubbings G, Bigwood T (2009) Anal Chim Acta 637:68
Sun H, He P, Lv Y, Liang S (2011) J Chromatogr B 852:145
Tsai W-H, Chuang H-Y, Chen H-H, Huang J-J, Chen H-C, Cheng S-H, Huang T-C (2009) Anal Chim Acta 656:56
Verdon E, Couedor P, Roudaut B, Sanders P (2005) JAOAC Int 88:1179
Wang Y, Baeyens WRG, Huang C, Fei G, He L, Ouyang J (2009) Talanta 77:1667
Yan H, Wang H, Qin X, Liu B, Du J (2011) J Pharm Biomed Anal 54:53
Yu Y-J, Wu H-L, Shao S-Z, Kang C, Zhao J, Wang Y, Zhu S-H, Yu R-Q (2011) Talanta 85:1549
Zheng M-M, Ruan G-D, Feng Y-Q (2009) J Chromatogr A 1216:7510
Zheng M-M, Gong R, Zhao X, Feng Y-Q (2010) J Chromatogr A 1217:2075
Acknowledgments
Financial support within the project BG051PO001/3.3-05-001 “Science and Business,” “Human Resources Development” Operational Programme of the European Social Fund of the EU is gratefully acknowledged. The authors wish to thank to Dr. Eric Verdon ANSES—Laboratory of Fougeres, French Agency for Food, Environmental and Occupational Health Safety for his helpful comments and insightful review of this manuscript.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Stoilova, N.A., Surleva, A.R. & Stoev, G. Simultaneous Determination of Nine Quinolones in Food by Liquid Chromatography with Fluorescence Detection. Food Anal. Methods 6, 803–813 (2013). https://doi.org/10.1007/s12161-012-9488-1
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-012-9488-1