Abstract
A simple, rapid, and sensitive method using in-tube solid-phase microextraction (in-tube SPME) based on poly(methacrylic acid–ethylene glycol dimethacrylate) (MAA–EGDMA) monolith coupled to HPLC with fluorescence and UV detection was developed for the determination of five fluoroquinolones (FQs). Ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENRO), and sarafloxacin (SARA) can be enriched and determined in the spiked eggs and albumins. CIP/ENRO in eggs and albumins of ENRO-treated hens were also studied using the proposed method. Only homogenization, dilution, and centrifugation were required before the sample was supplied to the in-tube microextraction, and no organic solvents were consumed in the procedures. Under the optimized extraction conditions, good extraction efficiency for the five FQs was obtained with no matrix interference in the process of extraction and the subsequent chromatographic separation. The detection limits (S/N=3) were found to be 0.1–2.6 ng g−1 and 0.2–2.4 ng g−1 in whole egg and egg albumin, respectively. Good linearity could be achieved over the range 2–500 ng mL−1 for the five FQs with regression coefficients above 0.9995 in both whole egg and albumin. The reproducibility of the method was evaluated at three concentration levels, with the resulting relative standard deviations (RSDs) less than 7%. The method was successfully applied to the analysis of ENRO and its primary metabolite CIP in the eggs and albumins of ENRO-treated hens.
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References
Linder JA, Huang ES, Steinman MA, Gonzales R, Stafford RS (2005) Am J Med 118:259–268
Pedersen K, Wedderkopp A (2003) J Appl Microbiol 94:111–119
Zhang LR, Wang YM, Chen BY, Cheng NN (2003) Acta Pharmacol Sin 24:605–609
European Agency for the Evaluation of Medicine Products. Committee for Veterinary Medicinal products, http://www.emea.eu.int/pdfs/vet/mrls/enrofloxacin.pdf
European Agency for the Evaluation of Medicine Products. Committee for Veterinary Medicinal products, http://www.emea.eu.int/pdfs/vet/mrls/sarafloxacin.pdf
Samanidou VF, Christodoulou EA, Papadoyannis IN (2005) J Sep Sci 28:325–331
Ovando HG, Gorla N, Weyers A, Ugnia L, Magnoli A (2004) Arch Med Vet 36:93–98
Garcia MA, Solans C, Calvo A, Hernandez E, Rey R, Bregante MA, Puig M (2005) Biomed Chromatogr 19:27–31
van Hoop N, de Wasch K, Okerman L, Reybroeck W, Poelmans S, Noppe H, de Brabander H (2005) Anal Chim Acta 529:265–272
Roybal JE, Walker CC, Pfenning AP, Turnipseed SB, Storey JM, Gonzales SA, Hurlbut JA (2002) J AOAC Int 85:1293–1301
Marazuela MD, Moreno–Bondi MC (2004) J Chromatogr A 1034:25–32
Idowu OR, Peggins JO (2004) J Pharm Biomed Anal 35:143–153
Cinquina AL, Roberti P, Giannetti L, Longo F, Draisci R, Fagiolo A, Brizioli NR (2003) J Chromatogr A 987:221–226
He P, Ackman RG (2000) Sci J Food Agr 80:10–16
Shim JH, Lee MH, Kim MR, Lee CJ, Kim IS (2003) Biosci Biotech Biochem 67:1342–1348
Donoghue DJ, Schneider MJ (2003) J AOAC Int 86:669–674
Liu Y, **e MX, Ding L (2004) Chin J Anal Chem 32:352–355
Chu PS, Donoghue DJ, Sheikh B (2000) J Agric Food Chem 48:6409–6411
Schneider MJ, Donoghue DJ (2003) Anal Chim Acta 483:39–49
Samanidou VF, Christodoulou EA, Papadoyannis IN (2005) J Sep Sci 28:555–565
Hernandez–Arteseros JA, Barbosa J, Compano R, Prat MD (2002) J Chromatogr A 945:1–24
Lolo M, Pedreira S, Fente C, Vazquez BI, Franco CM, Cepeda A (2003) Anal Chim Acta 480:123–130
Schneider MJ, Donoghue DJ (2000) J AOAC Int 83:1306–1312
Eisert R, Pawliszyn J (1997) Anal Chem 69:3140–3147
Kataoka H (2002) Anal Bioanal Chem 373:31–45
Mullett WM, Levsen K, Borlak J, Wu J, Pawliszyn J (2002) Anal Chem 74:1695–1701
Kataoka H, Narimatsu S, Lord HL, Pawliszyn J (1999) Anal Chem 71:4237–4244
Saito Y, Kawazoe M, Hayashida M, **no K (2000) Analyst 125:807–809
Fan Y, Feng YQ, Da SL, Shi ZG (2004) Anal Chim Acta 523:251–258
Fan Y, Feng YQ, Da SL, Gao XP (2004) Analyst 129:1065–1069
Wen Y, Fan Y, Zhang M, Feng YQ (2005) Anal Bioanal Chem 382:205–210
Fan Y, Feng YQ, Zhang JT, Da SL, Zhang M (2005) J Chromatogr A 1074:9–16
Nie J, Zhang M, Fan Y, Wen Y, **ang BR, Feng YQ (2005) J Chromatogr B 828:18–25
Wen Y, Zhang M, Zhao Q, Feng YQ (2005) J Agric Food Chem 53:8468–8473
Lina CE, Denga YJ, Liaoa WS, Sunb SW, Lina WY, Chena CC (2004) J Chromatogr A 1051:283–290
Kan CA, Petz M (2000) J Agric Food Chem 48:6397–6403
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The authors gratefully acknowledge the National Nature Science Foundation of China (Grant: 20275029), the Excellent Young Teachers Program of MOE, China.
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Huang, JF., Lin, B., Yu, QW. et al. Determination of fluoroquinolones in eggs using in-tube solid-phase microextraction coupled to high-performance liquid chromatography. Anal Bioanal Chem 384, 1228–1235 (2006). https://doi.org/10.1007/s00216-005-0270-8
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DOI: https://doi.org/10.1007/s00216-005-0270-8