Improved determination of quinolones in milk at their MRL levels using LC–UV, LC–FD, LC–MS and LC–MS/MS and validation in line with regulation 2002/657/EC

Hermo, M.P.; Nemutlu, Emirhan; Kır, Sedef; Barrón, D.; Barbosa, J.

doi:10.1016/j.aca.2008.02.045

Cited by 126 publications

(76 citation statements)

References 25 publications

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“…This method was previously applied to test quinolones [11]. The extraction procedure consisted of adding 2 mL of Milli-Q water to fortified milk samples and subsequent application of solid phase extraction on a Strata X cartridge.…”

Section: Methodsmentioning

confidence: 99%

“…There are several papers on antibiotic analysis in milk in the literature, but most focus on only few compounds or one class of antibiotics [10][11][12][13][14][15]. Although it is also possible to find multi-class published methods [8,[16][17][18][19][20][21][22][23][24], some are not quantitative or do not determine the quality parameters necessary for validating the method according to European legislation [25].…”

Section: Introductionmentioning

confidence: 99%

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Comparative study of the LC–MS/MS and UPLC–MS/MS for the multi-residue analysis of quinolones, penicillins and cephalosporins in cow milk, and validation according to the regulation 2002/657/EC

Junza

Amatya

Barrón

et al. 2011

Journal of Chromatography B

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The aim of this study was to develop and validate an analytical method to simultaneously determine European Union-regulated ȕ-lactams (penicillins and cephalosporins) and quinolones in cow milk. The procedure involves a new solid phase extraction (SPE) to clean-up and pre-concentrate the three series of antibiotics before analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). LC-MS/MS and UPLC-MS

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Comparative study of the LC–MS/MS and UPLC–MS/MS for the multi-residue analysis of quinolones, penicillins and cephalosporins in cow milk, and validation according to the regulation 2002/657/EC

Junza

Amatya

Barrón

et al. 2011

Journal of Chromatography B

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“…They have also important effects in the treatment of intestinal, respiratory, and urinary tract infections in humans and food-producing animals such as cattle, turkey, pig, and poultry. In the last years, the significant progressive increase of their use caused inevitable residues in food that represent a potential health hazard for consumers (Hermo et al 2008). There are many adverse effects commonly associated with quinolones including gastrointestinal, hepatic, and central nervous system toxicity, disrupted glucose metabolism, phototoxicity, hypersensitivity, and skin disorders (Liu 2010).…”

Section: Introductionmentioning

confidence: 99%

Development and Validation of a Method for the Determination of Quinolones in Muscle and Eggs by Liquid Chromatography-Tandem Mass Spectrometry

et al. 2016

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In this study, the development and validation of a multiresidue method for the detection of 11 quinolones (marbofloxacin, norfloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine) in muscle and eggs were reported. The method involved an extraction with a methanol/metaphosphoric acid mixture and a clean up by Oasis hydrophilic-lipophilic balance (HLB) cartridge. The validation was performed according to the Commission Decision 2002/657/EC. Linearity, specificity, decision limit (CCα), detection capability (CCβ), recovery, precision (repeatability and within-laboratory reproducibility), and ruggedness were determined. Depending on the analytes, CCα and CCβ ranged from 113 to 234 μg/kg and from 126 to 282 μg/kg in muscle samples, whereas in eggs, these parameters were between 5.6 and 7.4 μg/kg and between 6.1 and 9.8 μg/kg, respectively. In both the examined matrices, the recovery values were always higher than 90 % and precision, calculated as relative standard deviation, was equal to or lower than 16 % for repeatability and 23 % for within-laboratory reproducibility. The described method can be considered adequate for the simultaneous determination and quantification of quinolones in the tested food matrices.

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“…Several pre-treatment methods, including solid-phase extraction (SPE) (Hermo, Nemutlu, Kir, Barron, & Barbosa, 2008), liquid-liquid extraction (LLE) (Chu et al, 2002), stir bar sorption extraction (SBSE) (Huang, Yuan, & Lin, 2011), microwave-assisted extraction (MAE) (Hermo, Barron, & Barbosa, 2005), cloud point extraction (CPE) (Wu, Zhao, & Du, 2010) and supercritical fluid extraction (SFE) (Shim, Lee, Kim, Lee, & Kim, 2003) have been developed. Major limitations of these methods include timeconsuming extraction procedures, low enrichment factor, tedious operation and creation of a large amount of hazardous organic solvent waste.…”

Section: Introductionmentioning

confidence: 99%

Optimization of a phase separation based magnetic-stirring salt-induced liquid–liquid microextraction method for determination of fluoroquinolones in food

Gao

Wang

et al. 2015

Food Chemistry

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a b s t r a c tHerein, we developed a novel integrated apparatus to perform phase separation based on magneticstirring, salt-induced, liquid-liquid microextraction for determination of five fluoroquinolones in animal-based foods by HPLC analysis. The novel integrated apparatus consisted of three simple HDPE (high density polyethylene) parts that were used to separate the solvent from the aqueous solution prior to retrieving the extractant. The extraction parameters were optimized using the response surface method based on central composite design: 791 lL of acetone solvent, 2.5 g of Na 2 SO 4 , pH 1.7, 3.0 min of stir time, and 5.5 min centrifugation. The limits of detection were 0.07-0.53 lg kg À1 and recoveries were 91.6-105.0% for the five fluoroquinolones from milk, eggs and honey. This method is easily constructed from inexpensive materials, extraction efficiency is high, and the approach is compatible with HPLC analysis. Thus, it has excellent prospects for sample pre-treatment and analysis of fluoroquinolones in animal-based foods.

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Improved determination of quinolones in milk at their MRL levels using LC–UV, LC–FD, LC–MS and LC–MS/MS and validation in line with regulation 2002/657/EC

Cited by 126 publications

References 25 publications

Comparative study of the LC–MS/MS and UPLC–MS/MS for the multi-residue analysis of quinolones, penicillins and cephalosporins in cow milk, and validation according to the regulation 2002/657/EC

Comparative study of the LC–MS/MS and UPLC–MS/MS for the multi-residue analysis of quinolones, penicillins and cephalosporins in cow milk, and validation according to the regulation 2002/657/EC

Development and Validation of a Method for the Determination of Quinolones in Muscle and Eggs by Liquid Chromatography-Tandem Mass Spectrometry

Optimization of a phase separation based magnetic-stirring salt-induced liquid–liquid microextraction method for determination of fluoroquinolones in food

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