Key Laboratory for Analytical Science of Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian, 350116, China.
Key Laboratory for Analytical Science of Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian, 350116, China; Testing Center, The Sport Science Research Center, Fuzhou University, Fuzhou, Fujian, 350116, China.
J Chromatogr A. 2018 Jun 29;1556:37-46. doi: 10.1016/j.chroma.2018.04.066. Epub 2018 Apr 30.
Volatile polycyclic aromatic hydrocarbons (PAHs) in water and soil are associated with status in the human body. Development of simple, efficient detection method is challenging due to the coating could be attacked by the abundance of water in the direct-immersion solid-phase microextraction. The stability of coating is essential to the analysis results. In this paper, a stable Ni-Zn MOF/g-CN (MG NFs) nanoflowers with cavity traps structure was firstly reported and acted as solid-phase microextraction (SPME) adsorbent for PAHs. Markedly enhanced moisture and acid stability of the MG NFs was obtained through the doping the hydrophobic graphitic carbon nitride (g-CN) and metal ions into metal organic frameworks (MOFs). The aperture environment and ambient environment of MG NFs were changed by the doping of the Ni and the g-CN respectively. The moisture and acid stability of MG NFs were prominently increased under the dual protection. Compared to commonly used commercial coatings, the MG NFs own large surface area, unique nanoflowers structure and numerous open metal sites on the nanosheets, which demonstrated significant extraction superiority for PAHs. The MG NFs coated fiber was used for the SPME preconcentration of PAHs and couped with GC-MS for detecting PAHs. It presented low detection limits (0.1-3.0 ng L), wide linearity (0.3-5000.0 ng L) and good linearity (the correlation coefficient >0.9951). The inter-day and intra-day relative standard deviation (RSD) (n = 3) for three replicate extractions using one fiber was 3.8%-9.1%, and 3.5%-9.2%, respectively. The fiber-to-fiber reproducibility (n = 3) was 4.2-11.8%. The coupling method was successfully applied in the analysis of real water and soil samples with satisfactory recoveries of 82.9-109.2%, 84.2-106.4%, and the corresponding RSDs were 2.4-11.3%, 3.6-10.8%, respectively. The results indicated the effectiveness of NG NFs coated fiber in further practical application.
水中和土壤中的挥发性多环芳烃(PAHs)与人体状况有关。由于直接浸入式固相微萃取中存在大量的水,涂层可能会受到攻击,因此开发简单、高效的检测方法具有挑战性。涂层的稳定性对分析结果至关重要。本文首次报道了一种具有空腔陷阱结构的稳定 Ni-Zn MOF/g-CN(MG NFs)纳米花,并将其用作 PAHs 的固相微萃取(SPME)吸附剂。通过将疏水性石墨相氮化碳(g-CN)和金属离子掺杂到金属有机骨架(MOFs)中,显著提高了 MG NFs 的耐湿性和耐酸性。通过掺杂 Ni 和 g-CN,分别改变了 MG NFs 的孔径环境和环境。在双重保护下,MG NFs 的耐湿性和耐酸性明显增强。与常用的商业涂层相比,MG NFs 具有大的表面积、独特的纳米花结构和纳米片上大量的开放金属位,对 PAHs 表现出显著的萃取优势。MG NFs 涂层纤维用于 PAHs 的 SPME 预浓缩,并与 GC-MS 耦合检测 PAHs。它具有较低的检测限(0.1-3.0ngL)、较宽的线性范围(0.3-5000.0ngL)和良好的线性度(相关系数>0.9951)。使用一根纤维进行三次重复萃取的日间和日内相对标准偏差(RSD)(n=3)分别为 3.8%-9.1%和 3.5%-9.2%。纤维间的重现性(n=3)为 4.2-11.8%。该耦合方法成功应用于实际水样和土壤样品的分析,回收率为 82.9-109.2%、84.2-106.4%,相应的 RSD 为 2.4-11.3%、3.6-10.8%。结果表明,NG NFs 涂层纤维在进一步的实际应用中是有效的。