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Biomedical subjects

Brian M Patterson

Publications and source records attributed to Brian M Patterson.

5 recordsLinked to original sources

Integrating X-ray fluorescence and infrared imaging microspectroscopies for comprehensive characterization of an acetaminophen model pharmaceutical.

The integration of full spectral images using the complementary microspectroscopic imaging techniques X-ray fluorescence and Fourier transform infrared is demonstrated. This effort surpasses previous work in that a single chemometric software package is used to elicit chemical information from the integrated spectroscopic images. Integrating these two complementary spectroscopic methods provides both elemental and molecular spatial distribution within a specimen. The critical aspect in this work is using full spectral maps from each pixel within the image and subsequent processing with chemometric tools to provide integrated chemical information. This integration enables a powerful approach to more comprehensive materials characterization. Issues addressed include sample registration and beam penetration depth and how each affects post-processing. An inorganic salt and an acetaminophen pharmaceutical model mixture demonstrate the power of integrating these techniques with chemometric software.

Acetaminophen↗

Elemental and molecular characterization of aged polydimethylsiloxane foams.

The application and integration of micro X-ray fluorescence (MXRF) and Fourier transform infrared (FT-IR) imaging to polydimethylsiloxane (PDMS) foam aging issues have been applied to cross-sectional images. Previous work has shown the tin in the stannous 2-ethylhexanoate catalyst to be highly mobile and it typically migrates to the PDMS foam upper surface. The current paper discusses a method for the integration of full spectral MXRF and FT-IR imaging of aged foams. Solvent extractions have also been performed on both fresh and aged foams to further examine aged foam properties. Combining elemental and molecular imaging techniques and applying them to PDMS aging provides synergistic information that aids in understanding the sample composition and distribution of components. Application of chemometric analysis to the full spectral elemental and molecular maps demonstrates correlations within the foams of the residual tin, organo-tin functional group moieties, and the presence of nitroplasticizer from an exogenous source.

Combinatorial Chemistry Techniques↗

Attenuated total internal reflection infrared microspectroscopic imaging using a large-radius germanium internal reflection element and a linear array detector.

The number of techniques and instruments available for Fourier transform infrared (FT-IR) microspectroscopic imaging has grown significantly over the past few years. Attenuated total internal reflectance (ATR) FT-IR microspectroscopy reduces sample preparation time and has simplified the analysis of many difficult samples. FT-IR imaging has become a powerful analytical tool using either a focal plane array or a linear array detector, especially when coupled with a chemometric analysis package. The field of view of the ATR-IR microspectroscopic imaging area can be greatly increased from 300 x 300 microm to 2500 x 2500 microm using a larger internal reflection element of 12.5 mm radius instead of the typical 1.5 mm radius. This gives an area increase of 70x before aberrant effects become too great. Parameters evaluated include the change in penetration depth as a function of beam displacement, measurements of the active area, magnification factor, and change in spatial resolution over the imaging area. Drawbacks such as large file size will also be discussed. This technique has been successfully applied to the FT-IR imaging of polydimethylsiloxane foam cross-sections, latent human fingerprints, and a model inorganic mixture, which demonstrates the usefulness of the method for pharmaceuticals.

Dermatoglyphics↗

Attenuated total internal reflectance infrared microspectroscopy as a detection technique for capillary electrophoresis.

A novel detector for capillary electrophoresis (CE) using single-bounce attenuated total internal reflectance (ATR) Fourier transform infrared (FT-IR) microspectroscopy is presented. The terminus of the CE capillary is placed approximately 1 microm from the internal reflectance crystal at the focus of an ATR infrared microscope. Using pressure driven flow injection, concentration and volume detection limits have been determined for 25- and 10-microm-i.d. silica capillaries. Upon injection of 820 pL of succinylcholine chloride in a 10-microm capillary, a concentration detection limit of approximately 0.5 parts per thousand (ppt), or 410 pg, is found. The injection volume detection limit using a 108 ppt solution is 2.0 pL (216 pg). Sample separations using a programmed series of pressure, voltage, and again pressure on 25-, 50-, and 75-microm-i.d. capillaries are shown. CE separations of citrate and nitrate, as well as succinylcholine chloride with sodium salicylate using acetone as a neutral marker, are demonstrated. Several advantages of this CE-FT-IR technique include: (1) minimization of postcolumn broadening as a result of a small detector volume; (2) the ability to signal average spectra of the same aliquot, thereby improving the signal-to-noise in a stopped-flow environment; and (3) simplicity of design.

Electrophoresis, Capillary↗

Attenuated total internal reflectance infrared microspectroscopy as a detection technique for high-performance liquid chromatography.

The use of single reflection attenuated total internal reflection infrared microspectroscopy as a detector for high-performance liquid chromatography (HPLC) is demonstrated. The terminus of the HPLC column is placed at the focus of an ATR infrared microscope, allowing several advantages over other detection techniques. These include the following: (1) the reduction or elimination, or both, of detection cell dead volume, (2) the ability to interrogate a nearly pure aliquot of analyte, and (3) the ability to signal average spectra of the same aliquot (depending on its size) thereby improving the signal-to-noise ratio of the measurement and, concomitantly, the analytical characteristics of the method. Static measurements of succinylcholine chloride in water have shown a detection limit of 0.7 parts per thousand (ppt). Two-microliter injections of succinylcholine chloride in a 5-cm x 1-mm C-18 column with a flow rate of 60 microL/min have shown a detection limit of 1.9 ppt. This analytical concentration corresponds to a mass of 3.8 microg in the injection loop and a mass of 350 fg in the sampling volume. The potential of this detector for HPLC is demonstrated, and future improvements are also discussed.

Journal Article↗