Simultaneous Determination of Danofloxacin and Flumequine in Milk Based on Fluorescence Spectroscopy and Chemometrics To
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Simultaneous Determination of Danofloxacin and Flumequine in Milk Based on Fluorescence Spectroscopy and Chemometrics Tools Xiaoming Liu & Shiyun Feng & Peng Zhou & Yongquan Chen & Hao Zhang & Wei Chen
Received: 22 June 2013 / Accepted: 13 August 2013 / Published online: 25 August 2013 # Springer Science+Business Media New York 2013
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.
X. Liu : W. Chen State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214122, People’s Republic of China X. Liu : S. Feng : P. Zhou : Y. Chen : H. Zhang : W. Chen (*) School of Food Science and Technology, Jiangnan University, Wuxi 214122, People’s Republic of China e-mail: [email protected]
Keywords Danofloxacin . Flumequine . Milk . Fluorescence spectroscopy . PLS . PLS-DA 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 R2 Coefficient of determination RMSECV Root mean square error of cross-validation RMSEP Root mean square error of prediction LV Number of latent variables
Introduction Danofloxacin (DANO) and flumequine (FLU) belong to the quinolone and fluoroquinolone family, which features broadspectrum antibacterial activity based on the inhibition of bacteria DNA (Shojaee Aliabadi and Lees 2003; Garcia-Segura et al. 2012; Lombardo-Agüí et al. 2010). These drugs are widely used on food-producing animals to treat and prevent diseases and as feed additives to increase animal mass (Commission of the European Communities 2000; Oka et a
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