Food Analytical Methods

, Volume 9, Issue 8, pp 2223–2230 | Cite as

Application of Air-Assisted Liquid-Liquid Microextraction for Determination of Some Fluoroquinolones in Milk Powder and Egg Samples: Comparison with Conventional Dispersive Liquid-Liquid Microextraction

  • Li WangEmail author
  • Ting Huang
  • Hai Xia Cao
  • Qiu Xiang Yuan
  • Zhong Ping Liang
  • Guo Xi LiangEmail author


Herein, an air-assisted liquid-liquid microextraction (AALLME) has been described and compared to conventional dispersive liquid-liquid microextraction (DLLME) for the extraction/preconcentration of six fluoroquinolone compounds in milk powder and egg samples prior to high-performance liquid chromatography-UV detection (HPLC-UV). In order to compare the novel AALLME technique to the conventional DLLME technique, several parameters that influence the extraction efficiency were studied and optimized. Both methods have been validated for milk powder and egg analysis, obtaining limits of quantification lower than those usually permitted by legislation in food matrices, with precisions expressed as coefficients of variation lower than 8 % and recoveries between 72 and 115 % which were acceptable recoveries and repeatability. An AALLME method needs less organic solvent and shorter centrifugation time; therefore, it is more environmentally friendly and efficiently compared to DLLME.


Air-assisted liquid-liquid microextraction Fluoroquinolones Milk Egg 



This work was financially supported by the Nature Science Foundation of China (No. 21005033), Nature Science Foundation of Jiangsu Province (Nos. BK2011242 and BK20140577), College Education Nature Science Foundation of Jiangsu (No. 10KJD350001), and Advanced Talents Science Foundation of Jiangsu University (No. 10JDG052).

Compliance with Ethical Standards

Conflict of Interest

Li Wang declares that she has no conflict of interest. Ting Huang declares that she has no conflict of interest. Hai Xia Cao declares that she has no conflict of interest. Qiu Xiang Yuan declares that she has no conflict of interest. Zhong Ping Liang declares that she has no conflict of interest. Guo Xi Liang declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Informed consent is not applicable.


  1. Farajzadeh MA, Mogaddam MRA (2012) Air-assisted liquid–liquid microextraction method as a novel microextraction technique; application in extraction and preconcentration of phthalate esters in aqueous sample followed by gas chromatography–flame ionization detection. Anal Chim Acta 728:31–38CrossRefGoogle Scholar
  2. Farajzadeh MA, Mogaddam MR, Aghdam AA (2013) Comparison of air-agitated liquid–liquid microextraction technique and conventional dispersive liquid–liquid micro-extraction for determination of triazole pesticides in aqueous samples by gas chromatography with flame ionization detection. J Chromatogr A 1300:70–78CrossRefGoogle Scholar
  3. Farajzadeh MA, Feriduni B, Mogaddam MR (2015) Determination of triazole pesticide residues in edible oils using air-assisted liquid–liquid microextraction followed by gas chromatography with flame ionization detection. J Sep Sci 38(6):1002–1009CrossRefGoogle Scholar
  4. Herrera-Herrera AV, Hernández-Borges J, Borges-Miquel TM, Rodríguez-Delgado MÁ (2010) Dispersive liquid–liquid microextraction combined with nonaqueous capillary electrophoresis for the determination of fluoroquinolone antibiotics in waters. Electrophoresis 31(20):3457–3465CrossRefGoogle Scholar
  5. Herrera-Herrera AV, Hernández-Borges J, Borges-Miquel TM, Rodríguez-Delgado MÁ (2013) Dispersive liquid–liquid microextraction combined with ultra-high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples. J Pharm Biomed Anal 75:130–137CrossRefGoogle Scholar
  6. Juan-García A, Mañes J, Font G, Picó Y (2004) Evaluation of solid-phase extraction and stir-bar sorptive extraction for the determination of fungicide residues at low-microg kg(−1) levels in grapes by liquid chromatography-mass spectrometry. J Chromatogr A 1050(2):119–127CrossRefGoogle Scholar
  7. Juan-García A, Font G, Yolanda P (2007) Simultaneous determination of different classes of antibiotics in fish and livestock by CE-MS. Electrophoresis 28(22):4180–4191CrossRefGoogle Scholar
  8. Leong MI, Fuh MR, Huang SD (2014) Beyond dispersive liquid–liquid microextraction. J Chromatogr A 1335:2–14CrossRefGoogle Scholar
  9. Meng Z, Shi Z, Liang S, Dong X, Li H, Sun H (2015) Residues investigation of fluoroquinolones and sulphonamides and their metabolites in bovine milk by quantification and confirmation using ultra-performance liquid chromatography–tandem mass spectrometry. Food Chem 174:597–605CrossRefGoogle Scholar
  10. Minovski N, Vračko M, Šolmajer T (2011) Quantitative structure–activity relationship study of antitubercular fluoroquinolones. Mol Divers 15(2):417–426CrossRefGoogle Scholar
  11. Moema D, Nindi MM, Dube S (2012) Development of a dispersive liquid–liquid microextraction method for the determination of fluoroquinolones in chicken liver by high performance liquid chromatography. Anal Chim Acta 730:80–86CrossRefGoogle Scholar
  12. Picó Y, Andreu V (2007) Fluoroquinolones in soil—risks and challenges. Anal Bioanal Chem 387(4):1287–1299CrossRefGoogle Scholar
  13. Rezaee M, Assadi Y, Milani Hosseini MR, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid–liquid microextraction. J Chromatogr A 1116:1–9CrossRefGoogle Scholar
  14. Rusu A, Hancu G, Uivaroşi V (2015) Fluoroquinolone pollution of food, water and soil, and bacterial resistance. Environ Chem Lett 13(1):21–36CrossRefGoogle Scholar
  15. Saleh A, Yamini Y, Faraji M, Rezaee M, Ghambarian M (2009) Ultrasound-assisted emulsification microextraction method based on applying low density organic solvents followed by gas chromatography analysis for the determination of polycyclic aromatic hydrocarbons in water samples. J Chromatogr A 1216(39):6673–6679CrossRefGoogle Scholar
  16. Saraji M, Bidgoli AA (2010) Dispersive liquid–liquid microextraction using a surfactant as disperser agent. Anal Bioanal Chem 397(7):3107–3115CrossRefGoogle Scholar
  17. Saraji M, Boroujeni MK (2014) Recent developments in dispersive liquid–liquid microextraction. Anal Bioanal Chem 406(8):2027–2066CrossRefGoogle Scholar
  18. Sharafi K, Fattahi N, Mahvi AH, Pirsaheb M, Azizzadeh N, Noori M (2015) Trace analysis of some organophosphorus pesticides in rice samples using ultrasound-assisted dispersive liquid–liquid microextraction and high-performance liquid chromatography. J Sep Sci 38(6):1010–1016CrossRefGoogle Scholar
  19. Speltini A, Sturini M, Maraschi F, Consoli L, Zeffiro A, Profumo A (2015) Graphene-derivatized silica as an efficient solid-phase extraction sorbent for pre-concentration of fluoroquinolones from water followed by liquid-chromatography fluorescence detection. J Chromatogr A 1379:9–15CrossRefGoogle Scholar
  20. Viñas P, Campillo N, López-García I, Hernández-Córdoba M (2014) Dispersive liquid–liquid microextraction in food analysis. A critical review. Anal Bioanal Chem 406(8):2067–2099CrossRefGoogle Scholar
  21. Wang L, Yuan Q, Liang G, Shi L, Zhan Q (2015) Magnetic mixed hemimicelles solid-phase extraction coupled with high-performance liquid chromatography for the extraction and rapid determination of six fluoroquinolones in environmental water samples. J Sep Sci 38(6):996–1001CrossRefGoogle Scholar
  22. Wu C, Liu N, Wu Q, Wang C, Wang Z (2010) Application of ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of some organophosphorus pesticides in water samples. Anal Chim Acta 679(1–2):56–62CrossRefGoogle Scholar
  23. Xiao Q, Hu B, Yu C, Xia L, Jiang Z (2006) Optimization of a single-drop microextraction procedure for the determination of organophosphorus pesticides in water and fruit juice with gas chromatography-flame photometric detection. Talanta 69(4):848–855CrossRefGoogle Scholar
  24. You X, Xing Z, Liu F, Jiang N (2013) Air-assisted liquid–liquid microextraction used for the rapid determination of organophosphorus pesticides in juice samples. J Chromatogr A 1311:41–47CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  1. 1.Department of Pharmaceutics, School of PharmacyJiangsu UniversityZhenjiangChina
  2. 2.Department of Environment Science, School of the Environment and Safety EngineeringJiangsu UniversityZhenjiangChina

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