Skip to main content
Log in

Simultaneous Determination of Danofloxacin and Flumequine in Milk Based on Fluorescence Spectroscopy and Chemometrics Tools

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

The aim of this paper was to develop a rapid screening method to determine danofloxacin (DANO) and flumequine (FLU) in milk by fluorescence spectroscopy combined with three different chemometric tools. In this study, 2-D fluorescence data and multivariate calibration based on a partial least squares discriminant analysis (PLS-DA) regression were combined to simultaneously qualify and quantify DANO and FLU concentrations in commercial ultra-high-temperature (UHT) sterilized and pasteurized milk. Calibration sets based on the UHT whole milk from brand A were built and performed using a partial least squares (PLS) regression after deproteinization. Prediction sets based on 13 types of milk were analyzed using principal component analysis (PCA), principal PLS-DA, and PLS regression models. The multivariate calibration models were better able to determine the DANO and FLU concentrations than the univariate models, and these models could be applied to other types of milk. In contrast to the PLS-DA, which had good sensitivity and specificity, the PCA yielded less satisfactory results. In the quantitative analysis, the recoveries of the two analytes were reasonable and the root mean square error of prediction was within the acceptable range. The relative standard deviations of the predicted DANO and FLU concentrations on the various testing days were 9.2 and 6.2 %, respectively, demonstrating that the analytical method had a good reproducibility.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

Abbreviations

DANO:

Danofloxacin

FLU:

Flumequine

UHT:

Ultra-high-temperature sterilization

PCA:

Principal component analysis

PLS:

Partial least squares

PLS-DA:

Partial least squares discriminant analysis

TCA:

Trichloroacetic acid

R 2 :

Coefficient of determination

RMSECV:

Root mean square error of cross-validation

RMSEP:

Root mean square error of prediction

LV:

Number of latent variables

References

  • Andersen CM, Vishart M, Holm VK (2005) Application of fluorescence spectroscopy in the evaluation of light-induced oxidation in cheese. J Agric Food Chem 53(26):9985–9992

    Article  CAS  Google Scholar 

  • Birlouez-Aragon I, Sabat P, Gouti N (2002) A new method for discriminating milk heat treatment. Int Dairy J 12(1):59–67

    Article  CAS  Google Scholar 

  • Cañada-Cañada F, Espinosa-Mansilla A, de la Peña AM, Girón AJ, González-Gómez D (2009) Determination of danofloxacin in milk combining second-order calibration and standard addition method using excitation–emission fluorescence data. Food Chem 113(4):1260–1265

    Article  Google Scholar 

  • Chu XL (2011) Molecular spectroscopy analytical technology combined with chemometrics and its application. Chemical Industry Press, Beijing, pp 75–78

    Google Scholar 

  • Commission of the European Communities (2000) White paper on food safety. European Commission, Brussels

    Google Scholar 

  • Commission Regulation (EU) No. 37/2010 of 22 December 2009, on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Off. J. L. 2010, 20.1

  • Durante C, Cocchi M, Grandi M, Marchetti A, Bro R (2006) Application of N-PLS to gas chromatographic and sensory data of traditional balsamic vinegars of Modena. Chemometrics Intell Lab Syst 83(1):54–65

    Article  CAS  Google Scholar 

  • European Decision (EC) No. 2002/657/EC of 12 August 2002, implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off. J. L. 2002, 221

  • Garcia-Segura S, Garrido JA, Rodríguez RM, Cabot PL, Centellas F, Arias C, Brillas E (2012) Mineralization of flumequine in acidic medium by electro-Fenton and photoelectro-Fenton processes. Water Res 46(7):2067–2076

    Article  CAS  Google Scholar 

  • Hammami M, Rouissi H, Salah N, Selmi H, Al-Otaibi M, Blecker C, Karoui R (2010) Fluorescence spectroscopy coupled with factorial discriminant analysis technique to identify sheep milk from different feeding systems. Food Chem 122(4):1344–1350

    Article  CAS  Google Scholar 

  • Hooper DC, Wolfson JS (1993) Quinolone antimicrobial agents, 2nd edn. ASM, Washington, DC

    Google Scholar 

  • Jolliffe IT (1986) Principal component analysis. Springer, New York, 271 pp

    Book  Google Scholar 

  • Karoui R, De Baerdemaeker J (2007) A review of the analytical methods coupled with chemometric tools for the determination of the quality and identity of dairy products. Food Chem 102(3):621–640

    Article  CAS  Google Scholar 

  • Karoui R, Martin B, Dufour E (2005) Potentiality of front-face fluorescence spectroscopy to determine the geographic origin of milks from the Haute-Loire department. Lait 85(3):223–236

    Article  Google Scholar 

  • Karoui R, Dufour E, Schoonheydt R, De Baerdemaeker J (2007a) Characterisation of soft cheese by front face fluorescence spectroscopy coupled with chemometric tools: effect of the manufacturing process and sampling zone. Food Chem 100(2):632–642

    Article  CAS  Google Scholar 

  • Karoui R, Schoonheydt R, Decuypere E, Nicolai B, De Baerdemaeker J (2007b) Front face fluorescence spectroscopy as a tool for the assessment of egg freshness during storage at a temperature of 12.2 degrees C and 87 % relative humidity. Anal Chim Acta 582(1):83–91

    Article  CAS  Google Scholar 

  • Li H, Yin J, Liu Y, Shang J (2012) Effect of protein on the detection of fluoroquinolone residues in fish meat. J Agric Food Chem 60(7):1722–1727

    Article  CAS  Google Scholar 

  • Lombardo-Agüí M, García-Campaña AM, Gámiz-Gracia L, Cruces Blanco C (2010) Laser induced fluorescence coupled to capillary electrophoresis for the determination of fluoroquinolones in foods of animal origin using molecularly imprinted polymers. J Chromatogr A 1217(15):2237–2242

    Article  Google Scholar 

  • Lombardo-Agüí M, Gámiz-Gracia L, Cruces-Blanco C, García-Campaña AM (2011) Comparison of different sample treatments for the analysis of quinolones in milk by capillary-liquid chromatography with laser induced fluorescence detection. J Chromatogr A 1218(30):4966–4971

    Article  Google Scholar 

  • Oka H, Nakazawa H, Harada KI, MacNeil JD (1995) Chemical analysis for antibiotics used in agriculture. AOAC International, Gaithersburg

    Google Scholar 

  • Rodríguez N, Real BD, Cruz Ortiz M, Sarabia LA, Herrero A (2009) Usefulness of parallel factor analysis to handle the matrix effect in the fluorescence determination of tetracycline in whey milk. Anal Chim Acta 632(1):42–51

    Article  Google Scholar 

  • Rodríguez N, Ortiz MC, Sarabia LA, Herrero A (2010) A multivariate multianalyte screening method for sulfonamides in milk based on front-face fluorescence spectroscopy. Anal Chim Acta 657(2):136–146

    Article  Google Scholar 

  • Sahar A, Boubellouta T, Dufour E (2011) Synchronous front-face fluorescence spectroscopy as a promising tool for the rapid determination of spoilage bacteria on chicken breast fillet. Food Res Intl 44(1):471–480

    Article  CAS  Google Scholar 

  • Shojaee Aliabadi F, Lees P (2003) Pharmacokinetic–pharmacodynamic integration of danofloxacin in the calf. Res Vet Sci 74(3):247–259

    Article  CAS  Google Scholar 

  • Sousa J, Alves G, Fortuna A, Falcão A (2012) Analytical methods for determination of new fluoroquinolones in biological matrices and pharmaceutical formulations by liquid chromatography: a review. Anal Bioanal Chem 403(1):93–129

    Article  CAS  Google Scholar 

  • Takeda N, Gotoh M, Matsuoka T (2011) Rapid screening method for quinolone residues in livestock and fishery products using immobilised metal chelate affinity chromatographic clean-up and liquid chromatography-fluorescence detection. Food Addit Contam 28(9):1168–1174

    Article  CAS  Google Scholar 

  • Westerhuis JA, Hoefsloot HCJ, Smit S, Vis DJ, Smilde AK, Velzen EJJ, Duijnhoven JPM, Dorsten FA (2008) Assessment of PLSDA cross validation. Metabolomics 4(1):81–89

    Article  CAS  Google Scholar 

  • Yu H, Tao Y, Chen D, Pan Y, Liu Z, Wang Y, Huang L, Dai M, Peng D, Wang X, Yuan Z (2012) Simultaneous determination of fluoroquinolones in foods of animal origin by a high performance liquid chromatography and a liquid chromatography tandem mass spectrometry with accelerated solvent extraction. J Chromatogr B 885–886:150–159

    Article  Google Scholar 

Download references

Acknowledgments

Financial support for this study was provided by the Chinese National Natural Science Foundation of China (30901128).

Conflict of Interest

Xiaoming Liu declares that she has no conflict of interest. Shiyun Feng declares that she has no conflict of interest. Peng Zhou declares that he has no conflict of interest. Yongquan Chen declares that he has no conflict of interest. Hao Zhang declares that he has no conflict of interest. Wei Chen declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Wei Chen.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Liu, X., Feng, S., Zhou, P. et al. Simultaneous Determination of Danofloxacin and Flumequine in Milk Based on Fluorescence Spectroscopy and Chemometrics Tools. Food Anal. Methods 6, 1739–1749 (2013). https://doi.org/10.1007/s12161-013-9702-9

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-013-9702-9

Keywords

Navigation