Simultaneous quantification of several classes of antibiotics in water, sediments, and fish muscles by liquid chromatography–tandem mass spectrometry

doi:10.1007/s11783-013-0580-6

Front.Environ.Sci.Eng.

2014, Vol. 8

Issue (3) : 357-371 https://doi.org/10.1007/s11783-013-0580-6

RESEARCH ARTICLE

Simultaneous quantification of several classes of antibiotics in water, sediments, and fish muscles by liquid chromatography–tandem mass spectrometry

WEI Yimei^1,²,ZHANG Yuan²,XU Jian^2,(

),GUO Changsheng²,LI Lei²,FAN Wenhong³

College of Environment, Liaoning University, Shenyang 110036, China
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China
Department of Environmental Science and Engineering, School of Chemistry and Environment, Beihang University, Beijing 100191, China

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Abstract

Precise and sensitive methods for the simultaneous determination of different classes of antibiotics, including sulphonamides, fluoroquinolones, macrolides, tetracyclines, and trimethoprim in surface water, sediments, and fish muscles were developed. In water samples, drugs were extracted with solid-phase extraction (SPE) by passing 1000 mL of water through hydrophilic lipophilic balanced (HLB) SPE cartridges. Sediment samples were solvent-extracted, followed by tandem SPE (strong anion exchange (SAX) + HLB) clean-ups. Fish muscles were extracted by a mixture of acetonitrile and citric buffer (80:20, v/v) solution, and cleaned by SPE. Liquid chromatography–tandem mass spectrometry (LC-MS/MS) with multiple reaction monitoring (MRM) detection was employed to quantify all compounds. The recoveries for the antibiotics in the spiked water, sediment, and fish samples were 60.2%–95.8%, 48.1%–105.3%, and 59.8%–103.4%, respectively. The methods were applied to samples taken from Dianchi Lake, China. It showed that concentrations of the detected antibiotics ranged from limits of quantification (LOQ) to 713.6 ng·L^-1 (ofloxacin) in surface water and from less than LOQ to 344.8 μg·kg^-1 (sulphamethoxazole) in sediments. The number of detected antibiotics and the overall antibiotic concentrations were higher in the urban area than the rural area, indicating the probable role of livestock and human activities as important sources of antibiotic contamination. In fish muscles, the concentration of norfloxacin was the highest (up to 38.5 μg·kg^-1), but tetracyclines and macrolides were relatively low. Results showed that the methods were rapid and sensitive, and capable of determining several classes of antibiotics from each of the water, sediment, and fish matrices in a single run.

Keywords antibiotics liquid chromatography–tandem mass spectrometry (LC-MS/MS) water sediment fish muscle

Corresponding Author(s): XU Jian

Issue Date: 19 May 2014

Cite this article:

WEI Yimei,ZHANG Yuan,XU Jian, et al. Simultaneous quantification of several classes of antibiotics in water, sediments, and fish muscles by liquid chromatography–tandem mass spectrometry[J]. Front.Environ.Sci.Eng., 2014, 8(3): 357-371.

URL:

https://academic.hep.com.cn/fese/EN/10.1007/s11783-013-0580-6
https://academic.hep.com.cn/fese/EN/Y2014/V8/I3/357

Tab.1

Fig.1 Sampling locations in Dianchi Lake, China

Tab.2

Fig.2 Total ion chromatogram (TIC) of the antibiotic extract of a spiked sediment (100 μg·kg^-1 each) from Miyun Reservoir (1: SCT, 2: ¹³C₃-caffeine, 3: STZ, 4: TMP, 5: NOR, 6: OFL, 7: OTC, 8: CIP, 9: TC, 10: ENR, 11: SMZ, 12: CTC, 13: SCP, 14: ERM, 15: SMX, 16: SIA, 17: ROM, 18: SDX)

Fig.3 Extracted ion chromatograms (XIC) of the multiple reaction monitoring (MRM) chromatograms of the antibiotics (100 μg·kg^-1 each in sediment)

Tab.3

Fig.4 (a) Extraction recoveries of the antibiotics in sediment using methanol and citric buffer with different pH values; (b) Extraction recoveries of the antibiotics in sediment using different extraction solvents. A: methanol; B: citric buffer; C: methanol+ citric buffer (50:50 v/v); D: methanol+ citric buffer (20:80 v/v); E: methanol+ citric buffer (80:20 v/v)

Tab.4

Fig.5 Recoveries of antibiotics from fish tissues under different conditions: (a) pH effects and (b) extractant volumes

Fig.6 Spatial distribution of antibiotics detected in different sites in (a) surface water and (b) sediment from Dianchi Lake

Tab.5

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