Multiresidue LC–MS/MS analysis of cephalosporins and quinolones in milk following ultrasound‐assisted matrix solid‐phase dispersive extraction combined with the quick, easy, cheap, effective, rugged, and safe methodology

Abstract

A sensitive and selective confirmatory method for milk-residue analysis of ten quinolones and eight cephalosporins by LC-MS/MS has been developed herein. For the chromatographic separation of target analytes, a Perfectsil ODS-2 (250 × 4 mm, 5 μm) analytical column was used and gradient elution was applied, using a mobile phase of 0.1% w/w TFA in water and 0.1% w/w TFA in ACN. Ultrasound-assisted matrix solid-phase dispersion procedure was applied for the extraction and clean-up procedure of antimicrobials agents from milk matrix using a mixture of Bond Elut Plexa sorbent and QuEChERS. The method was validated meeting the European Legislation determining selectivity, linearity response, trueness, precision (repeatability and between-day reproducibility), decision limit, detection capability, and ruggedness following the Youden approach. Recoveries of all antibiotics ranged from 81.7 to 117.9%, while RSD values were lower than 13.7%. Limits of quantification for all examined compounds ranged from 2.4 to 15.0 μg/kg, substantially lower than the maximum residue limits established by the European Union (30-100 μg/kg).

Materials for Solid-Phase Extraction of Organic Compounds

“…A composite of Fe 3 O 4 @SiO 2 @GO was further modified with ionic liquid (IL) and successfully applied in the preconcentration of a group of polar and non-polar chlorophenols from the tap, well, and river water prior to their determination by LC-MS/MS [91]. 1 BTEX: benzene, toluene, ethylbenzene, and xylene; 2 MALDI-TOF: matrix-assisted laser desorption-time-of-flight; 3 SWCNTs: single-walled carbon nanotubes; 4 MWCNTs: multiwalled carbon nanotubes; 5 G: graphene; 6 GO: graphene oxide; 7 1,4-PDBA: 1,4-phenyldiboric acid.…”

“…EDCs: endocrine disrupting compounds; 2 NVIm-DVB: N-vinylimidazole-divinylbenzene;3 MAA-EDMA: methacrylic acid-ethyldimethacrylate;4 HXLPP: hyper-crosslinked sorbent prepared by precipitation polymerization; 5 HXLPP (HEMA): HXLPP including hydroxyethylene dimethacrylate;6 PAHs: polycyclic aromatic compounds;7 NSAIDs: non-steroidal anti-inflammatory drugs; 8 PCBs: polychlorinated bisphenyls; 9 PBDEs: polybrominated diphenyl ethers; 10 TOF: time-of-flight;11 PFCAs: polyfluorinated carboxylic acids;12 DEAEMA: 2-(diethylamino)ethyl methacrylate;13 GMA: glycidyl methacrylate.…”

Multiwalled‐carbon‐nanotubes‐based matrix solid‐phase dispersion extraction coupled with high‐performance liquid chromatography for the determination of honokiol and magnolol in Magnoliae Cortex

“…Because of its unique properties, MSPD has attracted increasing interest and is used more and more as attractive alternative to wide range of drugs, pesticides, microcontaminants, and other compounds from a variety of complex matrices [25][26][27] and the applications of MSPD on TCM materials increase obviously [28][29][30][31][32][33][34][35]. However, to the best of our knowledge, the simultaneous extraction of major active compounds in the Magnoliae Cortex by the MSPD has not been reported.…”

Determination of fluoroquinolones in environmental water and milk samples treated with stir cake sorptive extraction based on a boron‐rich monolith

“…So far, a variety of analytical methods have been developed for the determination of FQs in different samples including environmental waters and milk samples . Because of simplicity and convenience, HPLC coupled with detectors such as UV , MS/MS and fluorescence detector (FD) has been widely accepted for the monitoring of FQs in various samples. However, due to the very low concentration of FQs in real samples and the complexity of sample matrices, suitable sample preparation steps are necessary before HPLC analysis.…”