基于共价有机骨架-MSPE-HPLC-UV法测定多环芳烃

Determination of polycyclic aromatic hydrocarbons by MSPE-HPLC-UV-based on covalent organic frameworks

通过一种简易的方法制备磁性共价有机骨架材料(Fe3O4@COF-SCU1),用于磁性固相萃取(MSPE)大红袍茶汤中8种多环芳烃,并结合高效液相色谱-紫外(HPLC-UV)法对其进行定性定量分析。采用电子扫描显微镜、电子透射显微镜、X射线衍射、氮气等温吸附脱附、傅立叶变换红外光谱对Fe3O4@COF-SCU1进行表征。试验系统优化了Fe3O4@COF-SCU1组成、MSPE的吸附及洗脱条件,并建立多环芳烃的定性定量分析方法。在最佳操作条件下,8种多环芳烃均得到良好的线性关系,相关系数≥0.998 7。方法的检出限(LODs,S/N=3)和定量限(LOQs,S/N=10)分别为0.10~0.40,0.33~1.34ng/mL。用该方法对大红袍茶汤进行分析,加标回收率为74%~106%,相对标准偏差RSD为1.20%~8.50%。结果表明,Fe3O4@COF-SCU1可以简便快速地萃取分离痕量水平的多环芳烃。

A novel magnetic covalent organic framework(Fe3O4@COF-SCU1)was prepared via a facile method,and was used for the magnetic solid phase extraction(MSPE)of eight polycyclic aromatic hydrocarbons(PAHs)from dahongpao tea soup,which were analyzed by high performance liquid chromatographyUV(HPLC-UV).Fe3O4@COF-SCU1 was characterized by electron scanning microscope,electron transmission microscope,X-ray diffraction,nitrogen isothermal adsorption and desorption,and Fourier transform infrared.In this experiment,the composition of Fe3O4@COF-SCU1,the adsorption and elution conditions of MSPE were systematically optimized,and the qualitative and quantitative analysis method of PAHs was established.Under the optimal conditions,all the 8 PAHs obtained a good linear relationship,and the correlation coefficients were larger than0.998 7.The detection limit(LODs,S/N =3)and quantitative limit(LOQs,S/N=10)were in the range of 0.10~0.40 ng/mL and 0.33~1.34 ng/mL,respectively.The proposed method for analysis of PAHs was successfully applied to the analysis of dahongpao tea soup.The standard recovery and relative standard deviation were in the range of 74%~106% and 1.20%~8.50%,respectively.The results showed that Fe3O4@COF-SCU1 could be used for easily and rapidly extraction of trace PAHs.