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

Abstract

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.

Development of an icELISA and immunochromatographic strip for detection of norfloxacin and its analogs in milk

“…Currently, the methods of monitoring NOR focus on instrumental analytical methods and immunoassays (Annunziata et al, 2016;Bucknall, Silverlight, Coldham, Thorne, & Jackman, 2003;Chierentin & Salgado, 2016;Huang et al, 2016;Jiang et al, 2013;Liu et al, 2015;Mannemala & Kannappan, 2016;Mendes et al, 2015;Tong, Liu, Xie, & Li, 2016;Zhao et al, 2014). The most commonly used instrumental analytical methods including high-performance liquid chromatography and liquid chromatography-mass spectrometry are able to detect multiple fluoroquinolones, including NOR, simultaneously to give both quantitative and qualitative results, but the requirements for expensive apparatus and complicated sample preparation limit their application when monitoring samples in bulk (Tao et al, 2013).…”

A rapid and reliable assay to determine flumequine, marbofloxacin, difloxacin, and sarafloxacin in commonly consumed meat by micellar liquid chromatography

“…In general, they require careful multistep sample preparation . First, the antimicrobials must be extracted by leaching using a solvent (aqueous or hydroorganic, by simple mixing, vortexing, shaking, which may be ultrasound assisted or microwave assisted), eventually followed by centrifugation . Sometimes, several successive extraction steps may be required.…”

“…19 First, the antimicrobials must be extracted by leaching using a solvent (aqueous [20][21][22] or hydroorganic, 11,[23][24][25][26][27][28] by simple mixing, 20 vortexing, 11,21,22 shaking, [23][24][25][26]28,29 which may be ultrasound assisted 23,28 or microwave assisted 24 ), eventually followed by centrifugation. 11,[20][21][22][23][24][25][26]28,29 Sometimes, several successive extraction steps may be required. Afterwards, the supernatant is often purified before injection to avoid the introduction of particles, proteins, macromolecules, or other small endogenous compounds, which may be harmful for the column and/or overlap with the analytes, by solid phase extraction using a C18, 20,21 hydrophilic-lipophilic 23,29 or hydroxylated polystyrene-divinylbenzene, 24,25 immunoaffinity 22 or metalchelate affinity 27 coating, liquid/liquid extraction 11,28 or Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure 26 extraction.…”

“…11,[20][21][22][23][24][25][26]28,29 Sometimes, several successive extraction steps may be required. Afterwards, the supernatant is often purified before injection to avoid the introduction of particles, proteins, macromolecules, or other small endogenous compounds, which may be harmful for the column and/or overlap with the analytes, by solid phase extraction using a C18, 20,21 hydrophilic-lipophilic 23,29 or hydroxylated polystyrene-divinylbenzene, 24,25 immunoaffinity 22 or metalchelate affinity 27 coating, liquid/liquid extraction 11,28 or Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure 26 extraction. These procedures increase the time, effort, economic, and laboratory resources, and amount of toxic chemicals required for the analysis.…”

“…They also provide oscillating recoveries and increase the sources of variance in the method. Chromatographic separation has been carried out using polystyrenedivinylbenzene, 28 C8 25 or C18 11,[20][21][22][23][24]26,29 columns, a mobile phase with a high concentration of organic solvent (up to 100%), usually programmed as a gradient, 11,[20][21][22][23][24][25][26]28,29 and detected by mass spectrometry, [20][21][22][23]25,26 and UV-visible absorbance 24,25 or fluorescence. 11,21,22,[27][28][29] The latter is preferred because of its higher analytical performance per cost ratio.…”