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Quantitative analysis of solid samples using modified specular reflectance accessory.

Tomasz Czaja1, Sylwester Mazurek1, Roman Szostak1

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A modified specular reflectance (SR) accessory offers a cost-effective alternative to diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) for pharmaceutical analysis. This method accurately quantifies solid samples using infrared and near-infrared spectroscopy.

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Pharmaceutical Analysis

Background:

  • Diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) is a standard analytical technique.
  • DRIFTS is valued for its speed, reliability, and minimal sample preparation needs.
  • It is widely applied in pharmaceutical and food analysis for both qualitative and quantitative purposes.

Purpose of the Study:

  • To evaluate a simpler and more economical specular reflectance (SR) accessory operating in a DRIFTS-like mode (SR-DL) as an alternative to traditional DRIFTS.
  • To demonstrate the application of a modified SR accessory for the quantitative analysis of solid pharmaceutical samples.
  • To compare the performance of SR-DL with DRIFTS using infrared (IR) and near-infrared (NIR) spectroscopy.

Main Methods:

  • Utilized a modified SR accessory and a standard DRIFTS attachment for spectral acquisition.
  • Recorded IR and NIR spectra using Deuterated Triglycine Sulphate (DTGS) and Indium-Gallium Arsenide (InGaAs) detectors.
  • Constructed Partial Least Squares (PLS) models to quantify cinnarizine concentration in commercial tablets.
  • Calculated Relative Standard Errors of Prediction (RSEP) for calibration, validation, and analysis datasets.

Main Results:

  • The modified SR accessory achieved comparable quantification results to DRIFTS.
  • RSEP values for DRIFTS were 2.4-2.5% (calibration), 2.1-2.7% (validation), and 2.0-2.6% (analysis).
  • RSEP values for the modified SR accessory were 2.1-2.2% (calibration), 2.0-2.3% (validation), and 1.9-2.6% (analysis).

Conclusions:

  • The modified SR accessory (SR-DL) is a viable and cost-effective alternative to DRIFTS for quantitative analysis of solid pharmaceutical samples.
  • The SR-DL method demonstrates high accuracy and reliability in both mid- and near-infrared regions.
  • This advancement offers a more accessible approach for routine pharmaceutical quality control.