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Evaluation of Fibrous Silica Particles for Chromatographic Applications and the Analysis of Human-Derived Biofluids by HPLC and Capillary Electrophoresis.

Record Type:	Language materials, manuscript : Monograph/item
Title/Author:	Evaluation of Fibrous Silica Particles for Chromatographic Applications and the Analysis of Human-Derived Biofluids by HPLC and Capillary Electrophoresis./
Author:	Lopez Dauphin, Nahyr Arelis.
Description:	1 online resource (206 pages)
Notes:	Source: Dissertations Abstracts International, Volume: 84-08, Section: B.
Contained By:	Dissertations Abstracts International84-08B.
Subject:	Analytical chemistry. -
Online resource:	click for full text (PQDT)
ISBN:	9798371976024

Evaluation of Fibrous Silica Particles for Chromatographic Applications and the Analysis of Human-Derived Biofluids by HPLC and Capillary Electrophoresis.
Lopez Dauphin, Nahyr Arelis.

Evaluation of Fibrous Silica Particles for Chromatographic Applications and the Analysis of Human-Derived Biofluids by HPLC and Capillary Electrophoresis. - 1 online resource (206 pages)

Source: Dissertations Abstracts International, Volume: 84-08, Section: B.

Thesis (Ph.D.)--State University of New York at Buffalo, 2023.

Includes bibliographical references

Advances in liquid chromatography (LC) are highly connected with the development of chromatographic column technology. Herein, fibrous silica particles (FSPs) with a diameter of 1.0 μm were investigated as a potential new support material for LC column technology. Their inherent high surface area may provide a means to increase sample loadability. FSPs were derivatized with n-octyltrimethoxy silane (C8-TMS) to evaluate their chromatographic characteristics under reversed-phase (RP) conditions. The particles were examined via FTIR spectroscopy, gas adsorption analysis, thermogravimetric analysis, and scanning electron microscopy before and after functionalization with C8-TMS. In addition, LC columns were packed with functionalized and bare FSPs to evaluate their chromatographic performance using high-performance liquid chromatography (HPLC). Columns packed with bare FSPs exhibited the behavior that is consistent with hydrophilic interaction liquid chromatography (HILIC), while the C8-TMS-functionalized FSPs showed RP characteristics. The separation of probe compounds in a column packed with FSPs deteriorated over time as it was exposed to high pressures. Morphological analysis of the packing material by scanning electron microscopy (SEM) after exposing the packed column to high pressures (up to 12,000 psi) showed the breakage of the particles, suggesting that the 1 μm diameter FSPs are not mechanical stable under the high-pressure condition used in HPLC. In a second study, the adsorptive characteristics of porous and fibrous silica particles functionalized with fluorophilic, and anion-exchange moieties were examined for the adsorption of per and polyfluoroalkyl substances (PFAS) to enhance detectability in LC mass spectrometry (MS) for potential application in the analysis of PFAS in the environment. Fibrous silica particles, as well as traditional porous silica particles, were reacted with different silanes such as aminopropyltriethoxysilane (APTES) and tridecafluoro-1,1,2,2 tetrahydrooctyl triethoxy silane (C8-TFT), resulting in surface coverages of 1.96 and 1.34 μmol/m2 for the porous silica, and 4.43 and 3.32 μmol/m2 respectively for the fibrous silica particles. Dispersive-solid phase extraction (D-SPE) experiments showed the adsorption of long and short-chain PFAS using the modified particles. Several studies, such as loading capacity, adsorption, preliminary elution, and partition coefficient experiments, were performed to understand the behavior and adsorbent capabilities. The loading capacity and adsorption experiments using 10 mg of the fibrous particles modified to contain both C8-TFT and APTES showed the adsorption of perfluorooctanoic acid (PFOA), perfluorooctane sulfonic acid (PFOS), heptafluorobutyric acid (HFBA), and hexafluoropropylene oxide-dimer acid (Gen-X) in the range of 10 to 25000 ng/L. Elution experiments revealed that PFOS was extracted completely with ACN. In contrast, the best elution solvent for PFOA, HFBA, and Gen-X was 75:25 acetonitrile/water. Lastly, preliminary studies have shown that a human-derived biofluid (i.e., ascites) has antibacterial activity against Acinetobacter baumannii. However, the compound(s) responsible for the antibacterial activity and the complete profile of this fluid remains unknown. An HPLC method was used to enhance the separation of highly polar components in an ascites biofluid. Previous work on the ascitic fluid had shown antibacterial activity of two isolated early eluting HPLC peaks.The separation method was modified by extending the column length, resulting in higher resolution, which allowed the separation of new species from the early eluting bands. These were fractionated into four different fractions, and their antibacterial activities against A. baumannii were tested; however, the separated species did not show antibacterial properties. In addition, analysis of the ascites fluid via capillary electrophoresis revealed the amount of acetate and formate present in the sample, 0.74 and 4.34 mM. Efforts continue to further separate and identify the different components in the ascitic fluid.

Electronic reproduction.
Ann Arbor, Mich. :
ProQuest,
2024

Mode of access: World Wide Web

ISBN: 9798371976024Subjects--Topical Terms:

1182118
Analytical chemistry.
Subjects--Index Terms:

ElectrophoresisIndex Terms--Genre/Form:

554714
Electronic books.

Evaluation of Fibrous Silica Particles for Chromatographic Applications and the Analysis of Human-Derived Biofluids by HPLC and Capillary Electrophoresis.
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504 $a Includes bibliographical references
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650 4 $a Environmental studies. $3 1180247
653 $a Electrophoresis
653 $a Polyfluoroalkyl substances
653 $a Silica
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