管内填充磁性碳纳米管固相萃取-气相色谱/质谱法测定环境样品中多环芳烃

Solid-phase extraction based in tube filled-magnetic carbon nanotubes coupled with GC-MS for analysis of polycyclic aromatic hydrocarbons in environmental samples

采用原位反应法在碳纳米管(CNTs)的管内合成CoFe2O4纳米颗粒,制备了管内填充磁性碳纳米管(IF-MCNTs),建立了管内填充磁性碳纳米管/磁性固相萃取-气相色谱/质谱法(IF-MCNTs/MSPEGC/M S)测定土壤和水藻样品中7种多环芳烃(PAHs)的分析方法。通过透射电镜(TEM)、X射线衍射仪(XRD)、傅立叶变换红外光谱(FT-IR)等研究了IF-MCNTs的结构性能。考察了萃取条件对萃取性能的影响。研究表明,在最佳实验条件下,IF-MCNTs能够有效富集萘(NAP)、苊(ANE)、芴(FLU)、菲(PHE)、荧蒽(FLA)、芘(PYR)和苯并荧蒽(B(b)FL),对应饱和萃取容量分别为197.2,247.8,293.5,387.1,488.5,504.2和43.6 ng/mg。方法线性范围为5.0~500 ng/L,检出限在1.7~3.1 ng/L之间,相对标准偏差(RSD)小于6.8%。将所建方法应用于分析实际环境样品中7种PAHs,加标回收率在73.5%~97.2%之间,RSDs为3.4%~9.5%。方法可用于环境样品中多环芳烃的检测。

The in tube filled-magnetic carbon nanotubes(IF-MCNTs)were prepared by in-situ method.A method based on the magnetic solid-phase extraction(MSPE)coupled with gas chromatography-mass spectrometry(GC-MS)was developed for the analysis of polycyclic aromatic hydrocarbons(PAHs)from environmental soils and algae samples.Transmission electron microscopy(TEM),X-ray diffraction(XRD)and Fourier-transform infrared(FT-IR)spectroscopy were used to characterized the IF-MCNTs.The effects of extraction solvent,desorption solvent,extraction time and desorption time on extraction performance were investigated.Under optimized conditions,IF-MCNTs showed high adsorption capacity towards naphthalene(NAP),acenaphthene(ANE),fluorine(FLU),phenanthrene(PHE),fluoranthene(FLA),pyrene(PYR)and benzo(b)fluoranthene(B(b)FL).The corresponding saturated extraction amounts of IF-MCNTs were197.2,247.8,293.5,387.1,488.5,504.2 and 43.6 ng/mg,respectively.The calibration curves for seven polycyclic aromatic hydrocarbons(PAHs)all showed good linear relationships in the range of 5.0-500 ng/L.The detection limits were in the range of 1.7-3.1 ng/L,with the relative standard deviations(RSDs)less than6.8%.This method was successfully applied in the determination of PAHs in environmental soil and algae samples with the recoveries of 73.5%-97.2%and the RSDs of 3.4%-9.5%.This method showed a great potential in the determination of PAHs in complex environmental samples.