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| Detection of Seven Quinolones in Honey by High Performance Liquid Chromatography with Effervescent Assisted Liquid Phase Microextraction |
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| DOI： |
| KeyWord:high performance liquid chromatography switchable hydrophilic solvent effervescent assisted liquid phase microextraction honey quinolones |
| Author | Institution |
| WANG Yi-xia，YANG Lin-yan，HUANG Di，LI Liu-an，LI Na，ZHANG Wei，GUO Yong-ze，LI Cun |
1. Tianjin Key Laboratory of Agricultural Animal Breeding and Healthy Husbandry，College of Animal Science and Veterinary Medicine，Tianjin Agricultural University，Tianjin ，China; 2. Institute of Agricultural Quality Standards and Testing Technology，Tianjin Academy of Agricultural Sciences，Tianjin ，China |
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| Abstract: |
| A high performance liquid chromatography－fluorescence detection（HPLC－FLD） method combined with an effervescent assisted liquid phase microextraction（EA－LPME） was established for the determination of seven quinolones（QNs） in honey，based on a switchable hydrophilic solvent（SHS），nonanoic acid with switchability and density lower than water．In the proposed method，the pH value of the solution was adjusted by adding Na2CO3 and H2SO4 separately to make nonanoic acid complete the conversion from hydrophobicity to hydrophilicity and then to hydrophobicity．Meanwhile，the CO2 bubbles generated in-situ increased the contact area，and consequently promoting the extraction of analytes．Unlike traditional liquid phase microextraction（LPME）performed in a centrifuge tube，this method with simultaneous extraction and enrichment was completed in the syringe to realize the phase separation without centrifugation．In order to improve the extraction efficiency，the type and volume of extractant，the type and volume of pH regulator and the extraction time were optimized．The optimum extraction conditions were as follows：extraction solvent：nonanoic acid（200 μL），pH regulators：2.0 mol/L Na2CO3（400 μL） and 2.0 mol/L H2SO4（300 μL），and extraction time：1.5 min．There were linear ranges of 2.0－100 μg/L for norfloxacin and ciprofloxacin，and 2.0－200 μg/L for the other five drugs，with correlation coefficients（r2） of 0.999 5－0.999 9．The recoveries at three spiked levels of 10，100 and 500 ng/g for analytes ranged from 62.8% to 117%，with intra-day relative standard deviation（RSDs， n = 3） and inter-day（n = 6） RSDs not more than 6.2%．The limits of detection and the limits of quantitation were 3.0 ng/g and 10 ng/g，respectively. To evaluate the practicability of the present metnod，three kinds of honey samples spiked with 100 ng/g QNs were examined under the optimized conditions for the extraction（n = 3），the recoveries for seven analytes ranged from 78.8% to 120%，with RSDs less than 5.1%．The results demonstrated that the developed method is simple，accurate，effective and environmentally friendly，which could be used for the determination of quinolones in honey samples． |
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