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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Sputtered silicon solid phase microextraction fibers with a polydimethylsiloxane stationary phase with negligible carry-over and phase bleed
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Sputtered silicon solid phase microextraction fibers with a polydimethylsiloxane stationary phase with negligible carry-over and phase bleed

机译：溅射的硅固相微萃取纤维，具有多二甲基硅氧烷固定相，随便的携带和相渗

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We report the preparation of high performance, sputtered, polydimethylsiloxane (PDMS)-coated solid phase microextraction (SPME) fibers that show negligible carry-over and phase bleed. This process involves sputtering silicon onto silica fibers and functionalizing the resulting porous nanostructures with ultrathin films of vapor-deposited PDMS. Different thicknesses of silicon (0.25, 0.8, and 1.8 mu m) and PDMS (8, 16, and 36 nm) were produced and their extraction efficiencies evaluated. The deposition of PDMS was confirmed by time-of-fight secondary ion mass spectrometry (ToF-SIMS), X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and contact angle goniometry on model, planar silicon substrates. These fibers were investigated using direct immersion SPME coupled with gas chromatography-mass spectrometry (GC-MS) analysis of a series of polycyclic aromatic hydrocarbons (PAHs), which are carcinogenic pollutants. The 1.8 mu m thick silicon coating with 16 nm of PDMS (Si (1.8 mu m)/PDMS (16 nm)) produced the best response among the combinations tested. Conditions for the extraction of PAHs with this fiber were optimized and its extraction performance was compared to that of a commercial 7 mu m PDMS fiber. The linearity (1-110 mu gL(-1)), repeatability (RSD%, n = 3) (17% ave.), and minimum detection limits (0.6-1.5 mu gL(-1)) of the sputtered fibers were determined and found to be superior to the commercial 7 mu m PDMS fiber in many respects. Carry-over and phase bleed from commercial PDMS-based SPME fibers are two of their major drawbacks, which decrease their lifetimes and usefulness. Minimal carry-over and phase bleed were observed for our sputtered PDMS-coated fibers. In particular, our fiber only shows 12% of the phase bleed of the comparable commercial fiber. In addition, it shows no carry-over for analytes with retention times greater than pyrene, and only 5% of the carry-over of the other analytes. Our fibers could be used for at least 300 injections without any significant loss of performance. (C) 2020 Elsevier B.V. All rights reserved.
机译：我们报告了高性能，溅射，聚二甲基硅氧烷（PDMS）固相微萃取（SPME）纤维的制备，其显示可忽略的携带和相渗流。该方法涉及将硅溅射到二氧化硅纤维上，并用蒸汽沉积的PDMS的超薄薄膜官能化的多孔纳米结构。产生不同厚度的硅（0.25,0.8和1.8μm）和PDMS（8,16和36nm），并评估其提取效率。通过对抗二次离子质谱（TOF-SIMS），X射线光电子能谱（XPS），光谱椭圆形（SE），光谱椭圆形（SE），光谱椭圆形（SE），以及在模型，平面硅基板上的接触角焦管术来确认PDMS的沉积。使用与气相色谱 - 质谱（GC-MS）分析偶联的直接浸没SPME对一系列多环芳烃（PAH）进行研究，研究了这些纤维，这是致癌污染物。 1.8微米与PDMS的16nm的硅烷（Si（1.8微米）/ PDMS（16 nm）的）厚的硅涂层产生测试的组合中的最佳响应。优化了用该纤维提取PAHS的条件，并将其提取性能与商业7μMPDMS纤维的萃取性进行了比较。线性度（1-110μG1）），可重复性（RSD％，N = 3）（17％AVE）和溅射纤维的最小检测限（0.6-1.5μGL（-1））是确定并发现在许多方面上优于商业7μMPDMS纤维。来自基于商业PDMS的SPME纤维的随身携带和相渗出是它们的两个主要缺点，这降低了它们的寿命和有用性。对于我们的溅射的PDMS涂覆的纤维，观察到最小的携带和相排放。特别是，我们的纤维仅显示了可比较的商业纤维的12％的相渗流。此外，它表明对具有比芘的保留时间大的分析物没有携带，并且只有其他分析物的携带的5％。我们的纤维可用于至少300个注射，而无需任何显着的性能损失。 （c）2020 Elsevier B.v.保留所有权利。

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