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| Determination of Four Sulfonamides in Honey by Ultra-high Performance Liquid Chromatography with Polymer Monolithic Column Microextraction |
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| DOI： |
| KeyWord:polymer monolithic column microextraction ultra-high performance liquid chromatography sulfonamides honey |
| Author | Institution |
| CHENG Xiao-dan，FAN Zhe-feng |
College of Chemistry and Materials Science，Shanxi Normal University，Linfen ，China |
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| Abstract: |
| In this paper，an analytical method of ultra-high performance liquid chromatography with a polymer monolithic column microextraction（PMME/UPLC） was established for the extraction and separation of sulfadiazine（SDZ），sulfamethazine（SMZ），sulfapyridine（SPD）and sulfathiazole（STZ） in honey．The polymer monolithic column was prepared by the thermally initiated in-situ polymerization in pretreated glass capillaries，using 4-vinylbenzoic acid（VBA）and 4-vinylphenylboric acid（VPBA） as mixed functional monomers， methanol and toluene as the porogenic solvent and azobisisobutyronitrile（AIBN）as the initiator to copolymerize with divinylbenzene（DVB）. The poly（VBA-DVB-VPBA）monolithic column was used to extract sulfonamides（SAs） in honey in micro-extraction，and the target components were separated on a ZORBAX Eclipse Plus C18 column（2.1 mm × 50 mm i.d.，1.8 μm），then detected by diode array detection（DAD）．The extraction performance of the monolithic column was evaluated by peak area of chromatography．The properties of the monolithic column were characterized by infrared spectroscopy（IR），scanning electron microscopy（SEM） and energy dispersive spectroscopy（EDX）. With rich functional groups，uniform porosity，good permeability and stability，the column could adsorb sulfonamides by ion exchange，hydrophobic interaction，hydrogen bonding and B－N coordination，etc．The extraction conditions were optimized as follows：sample volume：3 mL，pH value：4，NaCl concentration：60 g/L，and elution volume：200 μL．The method was used for the extraction and separation of SDZ，SMZ，SPD and STZ in the actual samples. Under the optimized conditions，there were good linear relationships for the four target substances in corresponding mass concentration ranges，i.e. 40－200 ng/mL for SDZ，and 60－200 ng/mL for SPD，SMZ and STZ，with their correlation coefficients（r2） higher than 0.99．The enrichment factor of the monolithic column was between 10.97 and 12.82，while its extraction rate for four SAs ranged from 73.1% to 85.5%．The limits of detection and the limits of quantitation were in the ranges of 8.32－16.2 ng/mL and 27.5－53.9 ng/mL，respectively．The method was applied to the analysis of four SAs drugs in honey，and no target was detected in the actual samples．The average recoveries for those compounds at two spiked levels of 60.0 ng/mL and 100 ng/mL ranged from 89.8% to 105%，with relative standard deviations（RSD） of 2.0%－7.2%．With the advantages of low reagent consumption，short time and simple operation，the method could meet the requirements for extraction and separation of SAs in honey，and provide a simple and reliable approach for the actual monitoring of low-concentration antibiotics in food． |
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