Single‐step extraction followed by LC for determination of (fluoro)quinolone drug residues in muscle, eggs, and milk

Abstract

In this study, a simplified method for the extraction and determination of seven fluoroquinolone residues (danofloxacin, difloxacin, enrofloxacin, marbofloxacin, orbifloxacin, ofloxacin, and sarafloxacin) and three quinolones (oxolinic acid, flumequine, and nalidixic acid), in porcine muscle, table eggs, and commercial whole milk, which required no cleanup step, was devised. This procedure involves the extraction of analytes from the samples via liquid-phase extraction, and the subsequent quantitative determination was accomplished via LC-fluorescence detection. Analyte separation was successfully conducted on an XBridge-C(18) column, with a linear gradient mobile phase composed of acetonitrile and 0.01 M oxalic acid buffer at pH=3.5. The one-step liquid-liquid extraction method evidenced good selectivity, precision (RSDs=0.26-15.07%), and recovery of the extractable analytes, ranging from 61.12 to 115.93% in matrices. The LOQs ranged from 0.3 to 25 microg/kg. A survey of ten samples purchased from local markets was conducted, and none of the samples harbored fluoroquinolone residues. This method is an improvement over existing methodologies, since no additional cleanup was necessary.

Fluoroquinolone antibiotic determination in bovine milk using capillary liquid chromatography with diode array and mass spectrometry detection

“…Different procedures have been proposed to improve the cleanup and pre-concentration step of the antibiotics from milk samples. Thus, liquid-phase extraction (Cho et al, 2010), Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) methodology (Lombardo-Agü í et al, 2011), molecular imprinted-SPE (Lombardo-Agü í et al, 2011;Zhen et al, 2010), solid phase extraction (SPE) (Herrera-Herrera et al, 2009;Tang et al, 2009), and ionic liquid-based homogeneous liquid-liquid microextraction (Gao et al, 2011) were used. Moreover, some authors studied the improvement of the separation of Qns in milk from interfering matrix compounds using ionic liquids (HerreraHerrera et al, 2009) or surfactants (Rambla-Alegre et al, 2011) as mobile phase additives and in sample preparation.…”

Ionic liquid as hollow fibre membrane carrier for extraction of fluoroquinolone antibiotics in milk coupled with high-performance liquid chromatography quantification

“…For example, a limit of 100 mg kg À1 has been established by the European Union for the combined amount of enrofloxacin and ciprofloxacin in milk [5,6]. Several methods, such as capillary electrophoresis [7] and liquid chromatography [8][9][10][11][12][13], have been proposed for the analysis of these drugs in environmental water, biological samples and animal products. In previous research, the sample preparation techniques were based on either liquid-liquid extraction (LLE) [8][9][10][11] or solid-phase extraction (SPE) [12,13].…”

“…Several methods, such as capillary electrophoresis [7] and liquid chromatography [8][9][10][11][12][13], have been proposed for the analysis of these drugs in environmental water, biological samples and animal products. In previous research, the sample preparation techniques were based on either liquid-liquid extraction (LLE) [8][9][10][11] or solid-phase extraction (SPE) [12,13]. Although these techniques provided adequate analyte enrichment, high reproducibility and high sample capacity, a tedious process for LLE and a time consuming process for SPE were their disadvantages.…”

A Rapid and Effective Method for Simultaneous Determination of Residual Sulfonamides and Sarafloxacin in Pork and Chicken Muscle by High Performance Liquid Chromatography with Accelerated Solvent Extraction–Solid Phase Extraction Cleanup

“…A capillary electrophoresis-MS/MS method was presented for the determination of 12 SAs in pork meat with the LOQ of 46.5 μg.kg -1 [13]. Several LC methods were described for the determination of residual FQs in muscle, eggs, and milk with fluorescence detection with the LOQ of 5 μg.kg -1 for sarafloxacin [14], and in milk food or infant foods with MS/MS detection [15][16][17]. A LC method with programmable fluorescence-ultraviolet detection was described for the determination of sulfadiazine, sulfapyridine, sulfathiazole, sulfadimidine, and 7 FQs without sarafloxacin in chicken muscle with the limit of quantification of 15 μg.kg -1 for the SAs [18].…”

“…An ionic liquid aqueous two-phase system was developed for the separation of sulfadiazine and sulfamethoxazole in water samples and aquaculture products [8]. A simplified method with single-step extraction was developed for the extraction and determination of seven FQs residues and three quinolones in porcine muscle, table eggs, and commercial whole milk [14]. Recently, we reviewed the application of accelerated solvent extraction (ASE) in multiresidue analysis for food and feed [22].…”