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Related Concept Videos

Preparation of Samples for Electron Microscopy01:20

Preparation of Samples for Electron Microscopy

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To be visualized by an electron microscope, either transmission or scanning, biological samples need to be fixed (stabilized) so the electron beam does not destroy them and dried thoroughly (desiccated/dehydrated) so the vacuum does not affect them. Fixation needs to be done as quickly as possible because the sample properties will start changing as soon as it is removed from its natural environment. For example, in a tissue sample, the oxygen levels begin decreasing, causing an altered...
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Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides
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Porous, High Capacity Coatings for Solid Phase Microextraction by Sputtering.

Anubhav Diwan1, Bhupinder Singh1, Tuhin Roychowdhury1

  • 1Department of Chemistry and Biochemistry, Brigham Young University , Provo, Utah 84602, United States.

Analytical Chemistry
|December 24, 2015
PubMed
Summary
This summary is machine-generated.

New porous silicon solid phase microextraction (SPME) fibers offer enhanced sensitivity and selectivity for analyzing complex mixtures. These durable SPME coatings provide superior extraction performance compared to commercial options.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Separation Science

Background:

  • Solid phase microextraction (SPME) is a widely used technique for sample preparation.
  • Current SPME coatings have limitations in sensitivity and selectivity for certain analytes.
  • Development of novel SPME materials is crucial for advancing analytical capabilities.

Purpose of the Study:

  • To develop and characterize a new method for preparing porous solid phase microextraction (SPME) coatings using sputtered silicon on silica fibers.
  • To evaluate the performance of these novel SPME fibers in terms of extraction efficiency, selectivity, and durability.
  • To compare the performance of sputtered silicon SPME fibers with commercial poly(dimethylsiloxane) (PDMS) fibers.

Main Methods:

  • Preparation of porous silicon coatings on silica fibers via sputtering.
  • Surface modification of silicon coatings using piranha solution and silanization with octadecyldimethylmethoxysilane.
  • Characterization of coating properties using X-ray photoelectron spectroscopy and contact angle goniometry.
  • Optimization of headspace extraction parameters (time and temperature).
  • Comparative analysis of sputtered silicon SPME fibers and commercial PDMS fibers using gas chromatography-mass spectrometry (GC-MS).

Main Results:

  • Sputtered silicon coatings exhibited strong adhesion and were successfully functionalized with hydrophobic ligands.
  • Optimized extraction conditions (5 min, 40 °C) were established for headspace analysis.
  • The 2.0 μm sputtered silicon fiber showed significantly higher signal intensities for alcohols, aldehydes, amines, and esters compared to a commercial 7 μm PDMS fiber.
  • Sputtered fibers detected low molecular weight analytes missed by commercial fibers and demonstrated selectivity for analytes with hydrophobic and hydrogen-bonding properties.
  • Fibers maintained performance over at least 300 extractions with excellent repeatability and reproducibility.

Conclusions:

  • The novel sputtered silicon SPME fibers represent a promising alternative to commercial SPME coatings, offering enhanced extraction performance.
  • These fibers demonstrate superior sensitivity and selectivity for a wide range of analytes, including those with both hydrophobic and hydrogen-bonding characteristics.
  • The durability and ease of preparation make these sputtered silicon SPME fibers suitable for routine analysis in complex samples, as evidenced by the identification of over 50 compounds in a botanical sample.