Combination of microwave-assisted micellar extraction with liquid chromatography tandem mass spectrometry for the determination of fluoroquinolone antibiotics in coastal marine sediments and sewage sludges samples

• Published in: Biomedical chromatography Vol. 26; no. 1; pp. 33 - 40
• Main Authors: Montesdeoca-Esponda, Sarah, Sosa-Ferrera, Zoraida, Santana-Rodríguez, José Juan
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01-01-2012
• Subjects: Anti-Bacterial Agents - analysis; Chemical Fractionation - methods; Chromatography, Liquid - methods; fluoroquinolones; Fluoroquinolones - analysis; Geologic Sediments - chemistry; Limit of Detection; liquid chromatography; mass spectrometry; micellar media; Micelles; microwave-assisted extraction; Microwaves; Reproducibility of Results; Sewage - chemistry; Tandem Mass Spectrometry - methods; Water Pollutants, Chemical - analysis
• ISSN: 0269-3879; 1099-0801
• DOI: 10.1002/bmc.1621

ABSTRACT
In this work, a method for the analysis of fluoroquinolone antibiotics using microwave‐assisted micellar extraction combined with liquid chromatography–mass spectrometry detection has been developed. Different surfactants were tested for use as extractants in the isolation of the analytes from solid samples, and several experimental designs were evaluated for the determination and optimization of the variables that affect recovery from the matrix. Under optimal conditions, we obtained recoveries greater than 73% with relative standard deviations below 8%. Compounds were detected by liquid chromatography–electrospray ionization tandem mass spectrometry with detection limits between 0.15 and 0.55 ng g−1 and quantification limits between 0.49 and 1.85 ng g−1. Finally, the optimized method was applied in the determination of antibiotics in real solid samples. Four fluoroquinolones (levofloxacin, norfloxacin, ciprofloxacin and enrofloxacin) were found in coastal marine sediments taken close to a marine outfall and in sewage sludge samples from a wastewater treatment plant. Concentrations ranged between 0.81 and 34.3 ng g−1 in the sediments and 3.43 and 206.1 ng g−1 in the sludge. Copyright © 2011 John Wiley & Sons, Ltd.