摘要
氟化共价有机聚合物(F-COP)具有较大的比表面积和吸附容量,对丁香酚类化合物具有特异性吸附。该文以2,3,5,6-四氟对二苯甲醛(TFA)和1,3,5-三(4-氨苯基)苯(TAPB)为单体,三氟甲磺酸钪(Sc(OTf)3)为催化剂在室温下快速合成F-COP,并将其作为固相微萃取(SPME)吸附剂,结合高效液相色谱-紫外检测法(HPLC-UV),建立了测定水产品中丁香酚、乙酸丁香酚酯和甲基丁香酚麻醉剂的分析方法。通过傅里叶红外光谱、X射线衍射、N2吸附-解吸等温线和扫描电子显微镜等手段对F-COP材料进行表征。考察了萃取时间、搅拌速度、解吸溶剂及解吸时间对丁香酚类麻醉剂萃取量的影响,在萃取时间为30 min、搅拌速度为700 r/min、解吸溶剂为乙腈、解吸时间为10 min时,丁香酚类麻醉剂获得了最佳的萃取效果。在Diamonsil Plus C18-B色谱柱(250 mm×4.6 mm,5μm)上,以甲醇-水(60∶40,v/v)为流动相,流速0.800 mL/min,进样量20.0μL,紫外检测波长280 nm,柱温30℃条件下,丁香酚和乙酸丁香酚酯在10~1000μg/L,甲基丁香酚在10~1500μg/L范围内呈现出良好的线性关系,相关系数(r2)大于0.9961,方法检出限为2.9~4.5μg/kg(S/N=3),精密度小于8.7%(n=5)。最后,将该分析方法用于罗非鱼和基围虾样品的3种麻醉剂残留分析中,得到了满意的回收率(76.7%~104%)。结果表明,F-COP-SPME-HPLC-UV可满足水产品中丁香酚类麻醉剂的分析检测。
Fluorinated covalent organic polymers(F-COPs)constitute a new class of porous materials with a topological structure,large surface area,and potential superiority over other types of polymers in sample preparation.In this study,a F-COP was rapidly synthesized by a simple Schiff-based reaction using 2,3,5,6-tetrafluoroterephthalaldehyde(TFA)and 1,3,5-tris(4-aminophenyl)benzene(TAPB)as monomers,and by adding scandium(Ⅲ)triflate(Sc(OTf)3)as the metal catalyst at room temperature.The prepared F-COP was applied as a coating adsorbent for solid phase microextraction(SPME)to enrich three kinds of eugenol anesthetics in aquatic products.The extraction performance of an enrichment medium is an important factor for practical application in real analytical projects.This F-COP adsorbent with richπ-stacking electrons contained abundant phenyl rings and imine(-C=N)groups throughout the molecular framework.The adsorption mechanism was explored and discussed based on theπ-πaffinity and hydrogen bonding interaction,which contributed to its strong recognition affinity to targets.The F-COP was characterized by Fourier transform infrared(FT-IR)spectroscopy,X-ray diffraction(XRD),nitrogen adsorption-desorption isotherms,and scanning electron microscopy(SEM).The results indicated that the novel F-COP-SPME bar exhibited a rough and porous surface structure,good preparation reproducibility,and high stability.High performance liquid chromatography(HPLC)was performed with an ultraviolet-visible(UV-vis)wavelength detector.A Diamonsil plus C18 column(250 mm×4.6 mm,5μm)was used as the analytical column.The mobile phase comprised 60%methanol and 40%ultrapure water,and was flowed at 0.800 mL/min.The injected volume of the sample was 20.0μL.The column temperature was maintained at 30℃and the detection wavelength was set to 280 nm.Further,the SPME conditions(including extraction time,stirring rate,desorption solvent,and desorption time)that influenced the extraction efficiencies of the eugenol anesthetics were investigated in detail.Thu
作者
王兴益
陈彦龙
李攻科
WANG Xingyi;CHEN Yanlong;LI Gongke(School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China;School of Biology and Chemistry, Xingyi Normal University for Nationalities, Xingyi 562400, China)
出处
《色谱》
CAS
CSCD
北大核心
2021年第9期1012-1020,共9页
Chinese Journal of Chromatography
基金
广东省重点领域研发计划食品重点专项(2019B020211001)
国家重点研发计划课题(2019YFC1606101)
国家自然科学基金项目(21976213)
贵州省教育厅青年科技人才成长项目(黔教合KY字[2020]216).
关键词
高效液相色谱
固相微萃取
丁香酚
水产品
氟化共价有机聚合物
high performance liquid chromatography(HPLC)
solid phase microextraction(SPME)
eugenol
aquatic products
fluorinated covalent organic polymer(F-COP)
