Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 408, Issue 6, Pages 1701-1713Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-015-9284-z
Keywords
Antibiotics; Dispersive liquid-liquid microextraction; Solid-phase extraction; Ultra-high performance liquid chromatography-tandem mass spectrometry; Water samples
Funding
- 123 Project of China Environment Protection Foundation [CEPF2013-123-2-8]
- Large Instrument Sharing Service Construction Special of Shenyang Science and Technology Innovation Fund [F14-195-4-00]
- National Natural Science Foundation of China [81503029]
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A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16 % to 99.80 % with relative standard deviations between 0.7 and 8.4 %. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.
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