Sample preparation combined with electroanalysis to improve simultaneous determination of antibiotics in animal derived food samples

Abstract

A procedure based on liquid-liquid extraction (LLE) and phase separation using magnetically stirred salt-induced high-temperature liquid-liquid extraction (PS-MSSI-HT-LLE) was developed to extract and pre-concentrate ciprofloxacin (CIPRO) and enrofloxacin (ENRO) from animal food samples before electroanalysis. Firstly, simple LLE was used to extract the fluoroquinolones (FQs) from animal food samples, in which dilution was performed to reduce interference effects to below a tolerable threshold. Then, adapted PS-MSSI-HT-LLE protocols allowed re-extraction and further pre-concentration of target analytes in the diluted acid samples for simultaneous electrochemical quantification at low concentration levels. To improve the peak separation, in simultaneous detection, a baseline-corrected second-order derivative approach was processed. These approaches allowed quantification of target FQs from animal food samples spiked at levels of 0.80 to 2.00 µmol L in chicken meat, with recovery values always higher than 80.5%, as well as in milk samples spiked at 4.00 µmol L, with recovery values close to 70.0%.

Rapid Quantitative Detection of Voriconazole in Human Plasma Using Surface-Enhanced Raman Scattering

“…However, after the addition of salt, the mixture of water and acetonitrile tends to undergo liquid–liquid phase separation into a water-rich phase and an acetonitrile-rich phase . This phenomenon, known as salting-out-assisted liquid–liquid extraction (SALLE), has great potential in sample preparation. , The addition of salt increases the partitioning of the analyte in the organic phase by reducing the solubility of hydrophilic compounds in the aqueous phase through the salting-out effect . Both high concentrations of salts and organic solvents in the SALLE system can effectively precipitate proteins prior to phase separation, and most salts, matrix components, and particulate residues remain in the aqueous phase during phase separation .…”

“…It is known that water and acetonitrile are miscible under normal temperature and pressure conditions. 27 However, after the addition of salt, the mixture of water and acetonitrile tends to undergo liquid–liquid phase separation into a water-rich phase and an acetonitrile-rich phase. 28 This phenomenon, known as salting-out-assisted liquid–liquid extraction (SALLE), has great potential in sample preparation.…”

“… 29 Both high concentrations of salts and organic solvents in the SALLE system can effectively precipitate proteins prior to phase separation, and most salts, matrix components, and particulate residues remain in the aqueous phase during phase separation. 30 This technology has been initially studied in the detection of food 27 and personal care products. 29 Compared to traditional liquid–liquid extraction and solid-phase extraction, SALLE has the advantage of being more efficient and environmentally friendly, showing great potential for applications in biological fluid sample preparation.…”

Establishment and Validation of a GC–MS/MS Method for the Quantification of Penicillin G Residues in Poultry Eggs

“…To remove interfering substances in matrices, a simple and efficient sample preparation procedure was developed. Commonly, classical sample pretreatment techniques for the majority of edible tissues consists of extraction, purification, concentration and reconstitution [8,9]. The derivatization process is also included in the pretreatment in terms of physicochemical properties of hardly volatile penicillin G. To date, traditional liquid-liquid extraction (LLE) has been gradually substituted by the modern technique of accelerated solvent extraction (ASE) because of the relatively high complexity and low extraction efficiency of LLE [10].…”

Determination of Fluoroquinolones in Milk by Ionic Liquid-Mediated two phase extraction followed by Capillary Electrophoresis Analysis

“…However, FQs have drawn ongoing concerns owing to the possible toxic effects, allergic reactions, and development of resistant strains of bacteria. Therefore, the maximum residue limits (MRLs) for FQ residues in animalderived foods have been set by the European Union and other countries and regions [2-3] and methods for quick and accurate determination of FQs in animal-derived foods are highly needed [4].…”