Molecular spectroscopy is a widely recognized technique for the characterization of solid-state materials. Numerous advantages exist with molecular spectroscopy, namely qualitative and quantitative analysis, real-time monitoring of transient species, the ability to study API or drug product, and more recently, process analytical technology (PAT) application. Due to these advantages, SSCI utilizes molecular spectroscopy for standard compendial methodology, but also for high-end research applications. Because of the wide range of spectroscopic instrumentation at SSCI, we can apply the appropriate technology to our customers needs.

Infrared and Raman Spectroscopy

SSCI performs solid-state analyses with state-of-the-art infrared (IR), near IR (NIR) and Raman spectrometers. Each of these techniques can provide both qualitative characterization of different solid forms and a means to quantitate the solid form composition within the drug substance or product.

  • Infrared Spectroscopy
    Diffuse Reflectance
    Alkyl Halide Pellet
    Mineral Oil Mull
    Variable Temperature Diffuse Reflectance
    Variable Humidity Diffuse Reflectance
    Attenuated Total Reflectance
    Grazing Angle
    Chemical Mapping
  • NIR Spectroscopy Imaging
  • Raman Spectroscopy
    Dispersive and FT-Raman Spectrometers
    Chemical Mapping
    Variable Temperature

UV/Visible Spectroscopy

As an industry standard, ultraviolet/visible absorption spectroscopy is used by SSCI in support of dissolution, stability, and solubility studies.

NMR Spectroscopy

NMR spectroscopy is a powerful analytical technique that can be used on a wide variety of solid and liquid materials. Specific NMR active nuclei within a sample can be observed, which confers a unique level of selectivity for NMR spectroscopy. SSCI routinely uses both solid-state and liquid-state NMR spectroscopy to characterize a wide variety of materials from inorganic compounds to large biological molecules.

Solid-state NMR

Solid-state NMR spectroscopy is useful for analyzing polymorphs, solvates, salts, cocrystals, amorphous solids, and formulations. SSCI can perform high resolution solid-state NMR spectroscopy at 400 MHz (1H) for most of the NMR active nuclei on the periodic table. However, the most frequently observed nuclei in solid pharmaceutical compounds are 13C, 31P, 19F, and 15N. Variable temperature experiments can be performed from –75°C to 100°C. Available SSNMR techniques include standard direct excitation or enhancement via ramped amplitude cross polarization, modulated high power proton decoupling, very high speed spinning (up to 18 kHz), spectral editing, and spinning sideband suppression. Solid-state NMR experiments require approximately 50 mg of material with the potential to use as little as 10 mg.

Liquid-state NMR

Liquid-state NMR spectroscopy is a common technique for determining molecular structure and conformation or to analyze specific components in a mixture either qualitatively or quantitatively. Solution NMR spectroscopy provides a sensitive method to quantify impurities, reaction products, or residual solvents including water. A large variety of methods for NMR spectroscopy of liquid solutions are available at 400 MHz (1H). Variable temperature experiments are also available for liquids NMR analyses. Some of the most common analyses include 1D NMR of 1H, 13C, 19F, and 31P NMR. More advanced 2D NMR analyses such as COSY, NOESY, TOCSY, HMQC, HSQC, and HMBC are also routinely performed. These techniques can be used to determine the assignments of specific resonances for a molecule, which can provide the necessary information to the obtain a molecular conformation in solution. Most liquid-state NMR experiments require only a few milligrams of material.