Department of Chemistry and Biochemistry, College of Natural Sciences and Mathematics, University of Toledo, Toledo, OH, 43606, United States; School of Green Chemistry and Engineering, University of Toledo, Toledo, OH, 43606, United States.
Department of Chemistry and Biochemistry, College of Natural Sciences and Mathematics, University of Toledo, Toledo, OH, 43606, United States; School of Green Chemistry and Engineering, University of Toledo, Toledo, OH, 43606, United States.
J Chromatogr A. 2018 Jul 27;1560:1-9. doi: 10.1016/j.chroma.2018.04.027. Epub 2018 Apr 13.
A novel sorbent material, gold-polypyrrole (Au-PPy) nanocomposite-coated silica, is described for the efficient solid-phase extraction (SPE) of six common microcystins (MCs) well below the recommended United States EPA and World Health Organization (WHO) guidelines. With the optimized SPE protocol, samples spiked with MCs were determined at ng/L concentrations by liquid chromatography-mass spectrometry (LC-MS) in different aqueous sample matrices, including HPLC-grade, tap, and lake water. The average recoveries for all MCs tested in the three water matrices ranged from 94.1-103.2% with relative standard deviations (RSDs) of 1.6-5.4%, which indicated excellent extraction efficiency and reproducibility. Limits of detection (LODs) and limits of quantification (LOQs) for all MCs in both tap and lake water samples were determined to be ≤1.5 ng/L and 5.0 ng/L, respectively. The Au-PPy nanocomposite-coated sorbent material was reusable for at least three independent MC extractions with a single SPE cartridge in the concentration range of 10-500 ng/L. Importantly, off-column selective separation at the sample preparation and preconcentration stage between more hydrophilic and more hydrophobic MCs was achieved by sequential elution through changes in the solvent composition and SPE bed size. Therefore, the Au-PPy nanocomposite-coated silica sorbent is a promising new material for the quantification of MC variants in water samples.
一种新型的吸附材料，金-聚吡咯（Au-PPy）纳米复合材料涂层二氧化硅，用于高效固相萃取（SPE）六种常见微囊藻毒素（MCs），浓度远低于美国环保署和世界卫生组织（WHO）推荐的水平。通过优化的 SPE 方案，在不同的水样基质中，包括 HPLC 级、自来水和湖水，用液相色谱-质谱（LC-MS）在 ng/L 浓度下测定加标样品中的 MCs。在三种水样基质中，所有测试的 MCs 的平均回收率在 94.1-103.2%之间，相对标准偏差（RSD）在 1.6-5.4%之间，表明萃取效率和重现性都非常好。自来水中所有 MCs 的检测限（LOD）和定量限（LOQ）分别为≤1.5ng/L 和 5.0ng/L。Au-PPy 纳米复合材料涂层的吸附材料在 10-500ng/L 的浓度范围内，至少可以进行三次独立的 MC 萃取，每个 SPE 小柱重复使用。重要的是，通过改变溶剂组成和 SPE 床层尺寸，在样品制备和预浓缩阶段，在柱外实现了更亲水和更疏水的 MC 之间的选择性分离。因此，Au-PPy 纳米复合材料涂层的二氧化硅吸附剂是一种很有前途的新型材料，可用于水样中 MC 变体的定量分析。
