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在镀镍金属表面制备氧化石墨烯/镍配合物新涂层用于某些多环芳烃的直接浸入式固相微萃取

Preparation of a new coating of graphene oxide/nickel complex on a nickelized metal surface for direct immersion solid phase microextraction of some polycyclic aromatic hydrocarbons.

作者信息

Pasandideh Yalda, Razmi Habib

机构信息

Department of Chemistry, Faculty of Basic Sciences, Azarbaijan Shahid Madani University, P.O. Box: 53714-161, Tabriz, Iran.

出版信息

BMC Chem. 2021 Oct 16;15(1):56. doi: 10.1186/s13065-021-00783-w.

Abstract

BACKGROUND

Solid-phase microextraction (SPME) is a versatile sampling and sample preparation technology that possess a significant application in the extraction and pre-concentration of a broad range of micro-pollutants from different kind of matrices. Selection and preparation of an appropriate fiber substrate and coating materials have always been the main challenges of the SPME procedure. This paper introduces a high-efficiency metal-based SPME fiber with a new chemical coating of nickel/graphene oxide/nickel tetraazamacrocyclic complex (Ni/GO/NiTAM).

RESULT

The Ni/GO/NiTAM sorbent was electroless deposited onto the surface of an aluchrom (Alu) wire, and then the prepared fiber was employed for the extraction and pre-concentration of some PAHs before their HPLC-UV analysis. The prepared fiber characterization data were assessed using FE-SEM, EDX, XRD, FT-IR, and BET techniques. The method validation parameters, including the linearity range (LRs: 0.10 to 200.0 µg L), the limit of detection (LODs: 0.03‒0.30 µg L), and the limit of quantification (LOQs: 0.10-1.00 µg L), under optimal conditions. The relative standard deviations (RSDs) of intra-day, inter-day, and single fiber repeatability (for the samples spiked at 25 µg L) were in the range of 0.32-2.94, 1.20-4.09, and 1.42‒4.39%, respectively. In addition, the technique recoveries (RR %) and enrichment factors (EF) were in the range of 83.10‒107.80% and 83-164, respectively.

CONCLUSION

The fiber fabrication was simple, and the applied materials were also economical and easily accessible. Alu metal has high physicochemical and mechanical stability and thus can be a good alternative for the substrate of the fragile commercial SPME fibers. High rigidity and durability, long service life, and high extraction capability are some of the other advantages of the offered fiber.

摘要

背景

固相微萃取(SPME)是一种多功能的采样和样品制备技术,在从不同类型基质中萃取和预浓缩多种微污染物方面具有重要应用。选择和制备合适的纤维基材及涂层材料一直是SPME程序的主要挑战。本文介绍了一种具有新型镍/氧化石墨烯/四氮杂大环镍配合物(Ni/GO/NiTAM)化学涂层的高效金属基SPME纤维。

结果

将Ni/GO/NiTAM吸附剂化学沉积在铝铬(Alu)丝表面,然后将制备好的纤维用于一些多环芳烃的萃取和预浓缩,之后进行高效液相色谱-紫外分析。使用场发射扫描电子显微镜(FE-SEM)、能量散射X射线光谱仪(EDX)、X射线衍射仪(XRD)、傅里叶变换红外光谱仪(FT-IR)和比表面积分析仪(BET)技术对制备好的纤维进行表征数据评估。在最佳条件下,该方法的验证参数包括线性范围(LRs:0.10至200.0 μg/L)、检测限(LODs:0.03‒0.30 μg/L)和定量限(LOQs:0.10 - 1.00 μg/L)。日内、日间和单纤维重复性(对于加标浓度为25 μg/L的样品)的相对标准偏差(RSDs)分别在0.32 - 2.94%、1.20 - 4.09%和1.42‒4.39%范围内。此外,该技术的回收率(RR %)和富集因子(EF)分别在83.10‒107.80%和83 - 164范围内。

结论

纤维制备简单,所用材料经济且易于获取。铝铬金属具有高的物理化学和机械稳定性,因此可以成为易碎的商用SPME纤维基材的良好替代品。所提供的纤维还具有高刚性和耐久性、长使用寿命以及高萃取能力等其他优点。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5660/8520613/fae7d83d723a/13065_2021_783_Fig1_HTML.jpg

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