Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

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Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can ... continued below

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31 p.

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Freeze, R. October 8, 1997.

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This thesis or dissertation is part of the collection entitled: Office of Scientific & Technical Information Technical Reports and was provided by UNT Libraries Government Documents Department to Digital Library, a digital repository hosted by the UNT Libraries. More information about this document can be viewed below.

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  • Ames Laboratory
    Publisher Info: Ames Lab., IA (United States)
    Place of Publication: Iowa

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Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 {micro}l injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few {micro}l of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

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31 p.

Notes

OSTI as DE98004644

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  • Other Information: TH: Thesis (Ph.D.)

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  • Other: DE98004644
  • Report No.: IS-T--1818
  • Grant Number: W-7405-ENG-82
  • Office of Scientific & Technical Information Report Number: 587891
  • Archival Resource Key: ark:/67531/metadc690433

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Office of Scientific & Technical Information Technical Reports

Reports, articles and other documents harvested from the Office of Scientific and Technical Information.

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  • October 8, 1997

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  • Aug. 14, 2015, 8:43 a.m.

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  • Nov. 6, 2015, 8:46 p.m.

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Freeze, R. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography, thesis or dissertation, October 8, 1997; Iowa. (digital.library.unt.edu/ark:/67531/metadc690433/: accessed December 11, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.