磁固相萃取结合化学计量学分析水样中多环芳烃

Determination of PAHs in Water by Magnetic Solid Phase Extraction Coupled with Chemometrics

利用萘基的稠环结构和π-π相互作用,运用异氰酸萘酯和羟基反应特性,将萘基引入包硅的Fe_3O_4磁纳米粒子表面,制备了萘基功能化的核-壳结构磁性吸附材料Fe_3O_4@SiO_2@Nap,并研究其对多环芳烃的萃取性能。采用化学计量学对多环芳烃的GC-MS质谱图进行分辨,结合质谱库相似度匹配对各组分进行定性。从35个色谱峰中获得了22种化学成分,其中多环芳烃12种,其余10种为含有苯基或双键官能团化合物。实验证明Fe_3O_4@SiO_2@Nap纳米粒子具有选择性、稳定性、疏水性、快速富集与分离、萃取过程简单等优点,不仅能富集多环芳烃,也能富集含有π键结构的化合物。结合化学计量学分析方法,不仅降低了对色谱柱的要求,而且能快速、全面检测环境水样中的复杂未知多环芳烃。

This paper elaborates on the synthesis of Fe304@SiO2@Nap, a kind of naphthalene functionalized core-shell magnetic adsorbent, which was prepared by means of the interaction between naphthyl condensed ring structure and Л-Л, and of introducing naphthalene group into the surface of Fe304 magnetic nanoparticle that contained silicon. Meanwhile, the extraction properties of PAHs （polycyclic aromatic hydrocarbons） were studied. Chemometric resolution method was used to identify PAHs based on the GC-MS spectrum, and the components were characterized by similarity matching of mass spectra library. Consequently, 22 chemical constituents were discriminated from 35 chromatographic peaks, of which were 12 polycy- clic aromatic hydrocarbons （PAHs）, and the others containing phenyl or double bond functional groups. The experimental re- sults showed that characterized with selectivity, stability and hydrophobicity, Fe304@SiO2@Nap nanoparticles have the advantages of rapid enrichment and separation, as well as a simplified extraction process. Not only can those nanoparticles enrich PAHs but also can enrich the w-bond-containing compounds. With the chemomelliC analytical method, requirements for the chromatographic column were lessened, and detection of unknown complex polycyclic aromatic hydrocarbons in environmental water samples can be done quickly and comprehensively.