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J Agric Food Chem. 2016 Nov 16;64(45):8684-8693. Epub 2016 Nov 4.

Sensitive Monitoring of Fluoroquinolones in Milk and Honey Using Multiple Monolithic Fiber Solid-Phase Microextraction Coupled to Liquid Chromatography Tandem Mass Spectrometry.

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State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University , Xiamen 361005, China.


In the present study, a new multiple monolithic fiber solid-phase microextraction (MMF-SPME) based on poly(apronal-co-divinylbenzene/ethylenedimethacrylate) monolith (APDE) was synthesized. The effect of the preparation parameters of APED on extraction efficiency was studied thoroughly. The combination of APDE/MMF-SPME with high-performance liquid chromatography tandem mass spectrometry detection (HPLC/MS-MS) was developed for sensitive monitoring of ultratrace fluoroquinolones (FQs) in foodstuffs, including milk and honey samples. Under the optimized experimental conditions, the limits of detection (S/N = 3) for the targeted FQs ranged from 0.0019 to 0.018 μg/kg in milk and 0.0010 to 0.0028 μg/kg in honey. The relative standard deviations (RSDs) for method reproducibility were less than 9% in all samples. The established method was successfully applied for the monitoring of FQs residues in milk and honey samples with the recoveries between 74.5% and 116% (RSDs were in the range 0.9-9.5%). In comparison to previous methods, the developed APDE/MMF-SPME-HPLC/MS-MS showed some merits, including satisfactory sensitivity, simplicity, high cost-effectiveness, and low consumption of organic solvent.


adsorbent; fluoroquinolones; honey; milk; multiple monolithic fiber solid-phase microextraction

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