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This dissertation encompasses research focused on application of attenuated total internal reflection (ATR) infrared spectroscopy and imaging approaches in quantitative analysis of kidney stone components and pharmaceuticals. Chapter 1 provides a background on the attenuated total internal reflection (ATR) and other infrared microspectroscopic techniques including the factors affecting quantitative analysis using infrared microspectroscopy. It also describes the chemometric methods used for quantitative analysis. Chapter 2 presents chemical synthesis and characterization of some closely related components of kidney stones including calcium oxalate dihydrate COD, hydroxylapatite HAP, and octacalcium phosphate OCP. The described chemical synthesis methods in this chapter were simple, reproducible, and provided these components into pure form so that high quality spectra can be obtained. Chapter 3 describes the effect of sample preparation on infrared microspectroscopic analysis of renal stones The sample prepration methods in this work involve polishing the surface of cross-sectioned renal calculi using sanding discs and lapping films. This study demonstrated that polishing of kidney stones using lapping films result in greater increase in the reflectance intensity and improvement of photometric accuracy of reflectance microspectroscopy technique compared to sanding discs. Chapter 4 investigates the use of attenuated total internal reflection (ATR) with PCR models for quantitative analysis of mixed renal stones. The results of this study show that the constructed PCR models can be potentially used for quantitative analysis of stone components. Chapter 5 presents a study of the spatial resolution and detection limits of attenuated total internal reflection (ATR) infrared microspectroscopy using polymer laminates and polymeric microspheres. The results of this work prove that ATR microspectroscopy is capable of detection of structures with dimensions below the theoretical diffraction limit. It is also demonstrated that Principal component analysis (PCA) can enhance the image contrast allowing better visualization of these structures. Additionally, this chapter studies the feasibility of quantitative analysis using GRAMS/ AI and PCR models. Chapter 6 investigates the application of ATR imaging for quantitative analysis of pharmaceuticals in their dosage forms based on image analysis using PCA and Image J software. The results demonstrate the capability of ATR-FTIR imaging of obtaining information about the relative concentration of active ingredients in drug formulations. |
