The self-association of fluoroquinolones (FQ) in water would play a relevant role in their translocations across lipid membranes. Triplet excited states of these drugs have been shown as reporters of FQ self-association using laser flash photolysis technique. A study using low-temperature phosphorescence technique was performed with quinolone derivatives such as enoxacin (ENX), norfloxacin (NFX), pefloxacin (PFX), ciprofloxacin (CPX, ofloxacin (OFX), nalidixic acid (NLA), pipemidic acid (PPA) and piromidic acid (PRA) to explore emission changes associated with self-associations and to shed some light on the triplet excited state energy (E_T) discrepancies described in the literature for most of these drugs. The emissions obtained at 77 K in buffered aqueous medium revealed that the amphoteric nature of the quinolones CPX, NFX, PFX, ENX, OFX and PPA must generate their self-associations because a redshift of their phosphorescence maxima is produced by FQ concentrations increases. Hence, this effect was not observed for NLA and PRA or when all quinolones were analysed using ethanol or ethylene glycol aqueous mixtures as glassed solvents. Interestingly, the presence of these organic mixtures produced a blue-shift in the phosphorescence emission maximum of each FQ. Additionally, laser flash photolysis experiments with PRA and the amphoteric quinolone PPA, compounds with the same skeleton but different peripheral substituent, confirm the expected correlations between the amphoteric nature of compounds and their self-associations in aqueous media because the excimer generation was only detected for PPA. Now, the discrepancies described in the literature for the E_T of FQs can be understood considering that changes of medium polarity or proticity as well as the temperature can considerably modify their E_T values. Thereby, low-temperature phosphorescence technique, is an effective way to detect molecular self-associations and surrounding changes in quinolones that opens the possibility to evaluate these effects in other drug families.

03 Jun 2018·Food Additives & Contaminants: Part AQ3 · AGRICULTURAL & FORESTRY SCIENCE

Determination of quinolone residues in raw cow milk. Application of polar stir-bars and ultra-high performance liquid chromatography–tandem mass spectrometry

Q3 · AGRICULTURAL & FORESTRY SCIENCE

Article

Author: Zafra-Gómez, Alberto ; García-Córcoles, María Teresa ; Çipa, Morsina ; Barrón, Dolores ; Rodríguez-Gómez, Rocío ; Navalón, Alberto

Seventeen quinolone antibiotics were determined in cows' milk. A method of high sensitivity, selectivity and accuracy was developed. Accuracy (trueness and precision), linearity, sensitivity, selectivity, decision limit and detection capability were established following the recommendations of the Commission Decision 2002/657/EC and the Food and Drug Administration (FDA) guideline. The use of polar stir-bar sorptive extraction (SBSE) prior to UHPLC-MS/MS analysis is proposed. The variables that affect SBSE were optimised using multivariate optimisation strategies. The ionic strength, the extraction time and the sample volume were studied. pH and stir-bar coating (polydimethylsiloxane, PDMS, and polyethyleneglycol modified silicone, PEG) were studied. PEG showed the best extraction yield at pH 6. For validation, a matrix-matched calibration and a recovery assay were carried out. Limits of quantification from 0.5 μg kg^-1 for nalidixic acid, flumequine and piromidic acid, to 4.0 μg kg^-1 for sarafloxacin were calculated. The precision (%, RSD) was lower than 15% for all antibiotics. Recoveries in fortified samples were between 88 and 114%.

30 Dec 2012·Rapid Communications in Mass SpectrometryQ3 · CHEMISTRY

Laser diode thermal desorption mass spectrometry for the analysis of quinolone antibiotic residues in aquacultured seafood

Q3 · CHEMISTRY

Article

Author: Madson, Mark R. ; Lohne, Jack J. ; Clark, Susan B. ; Turnipseed, Sherri B. ; Andersen, Wendy C.

RATIONALEVeterinary drug residue analysis of meat and seafood products is an important part of national regulatory agency food safety programs to ensure that consumers are not exposed to potentially dangerous substances. Complex tissue matrices often require lengthy extraction and analysis procedures to identify improper animal drug treatment. Direct and rapid analysis mass spectrometry techniques have the potential to increase regulatory sample analysis speed by eliminating liquid chromatographic separation.METHODSFlumequine, oxolinic acid, and nalidixic acid were extracted from catfish, shrimp, and salmon using acidified acetonitrile. Extracts were concentrated, dried onto metal sample wells, then rapidly desorbed (6 s) with an infrared diode laser for analysis by laser diode thermal desorption atmospheric pressure chemical ionization with tandem mass spectrometry (LDTD‐MS/MS). Analysis was conducted in selected reaction monitoring mode using piromidic acid as internal standard.RESULTSSix‐point calibration curves for each compound in extracted matrix were linear with r2 correlation greater than 0.99. The method was validated by analyzing 23 negative samples and 116 fortified samples at concentrations of 10, 20, 50, 100, and 600 ng/g. Average recoveries of fortified samples were greater than 77% with method detection levels ranging from 2 to 7 ng/g. Three product ion transitions were acquired per analyte to identify each residue.CONCLUSIONSA rapid method for quinolone analysis in fish muscle was developed using LDTD‐MS/MS. The total analysis time was less than 30 s per sample; quinolone residues were detected below 10 ng/g and in most cases residue identity was confirmed. This represents the first application of LDTD to tissue extract analysis. Published 2012. This article is a US Government work and is in the public domain in the USA.

100 Deals associated with Piromidic Acid

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D01431	Piromidic Acid	J01MB03	DB13744

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