College of Chemistry, Zhengzhou University, Kexue Avenue 100, Zhengzhou, Henan 450001, PR China.
Department of Epidemiology and Biostatistics, College of Public Health, Zhengzhou University, Zhengzhou, Henan 450001, PR China.
J Hazard Mater. 2023 Jun 15;452:131228. doi: 10.1016/j.jhazmat.2023.131228. Epub 2023 Mar 17.
Herein, a quinoline-linked ultrastable 2D covalent organic framework (COF-CN) coated fiber was successfully prepared and used for highly-sensitive headspace solid-phase microextraction (HS-SPME) of organochlorine pesticides (OCPs) in environmental water. The extraction efficiency of the COF-CN coating for all 14 OCPs was higher than that of four commercial SPME fiber coatings and most of the published works, with enrichment factors ranging from 540 to 5065. In combination with gas chromatography-tandem mass spectrometry (GC-MS/MS), a wide linear range (0.05-200 ng/L), low detection limits (LODs, 0.0010-13.54 ng/L) and satisfactory reproducibility and repeatability were obtained under optimal conditions. Compared with the published works, the LODs of the developed technique were improved 2-5.9 times, and the enrichment factors (EFs) of the developed method were enhanced at least 2 times. The COF-CN coated fiber can be easily recycled and reused at least 70 times without any washing step. The adsorption mechanism was first characterized by density functional theory calculations and X-ray photoelectron spectroscopy analysis. Besides, the established method was successfully applied to the analysis of the distribution of trace OCPs in real water samples from Henan Province. All these results proved the promising application of the developed HS-SPME-GC-MS/MS method for organic pollutants analysis in water samples.
在此,成功制备了一种喹啉连接的超稳定二维共价有机骨架(COF-CN)涂层纤维,并将其用于环境水样中有机氯农药(OCPs)的高灵敏度顶空固相微萃取(HS-SPME)。与四种商业 SPME 纤维涂层和大多数已发表的工作相比,COF-CN 涂层对所有 14 种 OCPs 的萃取效率都更高,富集因子范围为 540 至 5065。在最佳条件下,结合气相色谱-串联质谱(GC-MS/MS),获得了较宽的线性范围(0.05-200ng/L)、较低的检测限(LOD,0.0010-13.54ng/L)和令人满意的重现性和重复性。与已发表的工作相比,所开发技术的 LOD 提高了 2-5.9 倍,且开发方法的富集因子(EF)至少提高了 2 倍。COF-CN 涂层纤维无需任何洗涤步骤,可至少重复使用 70 次。通过密度泛函理论计算和 X 射线光电子能谱分析,首次对吸附机理进行了表征。此外,所建立的方法成功应用于分析来自河南省的实际水样中痕量 OCPs 的分布。所有这些结果均证明了所开发的 HS-SPME-GC-MS/MS 方法在水样中有机污染物分析中的应用前景广阔。