Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics

Area of Science:

• Analytical Chemistry
• Pharmaceutical Analysis
• Chemometrics

Background:

• Accurate quantification of active pharmaceutical ingredients (APIs) and excipients in complex mixtures is crucial for quality control.
• Traditional methods may struggle with simultaneous determination of multiple components in pharmaceutical powders.

Purpose of the Study:

• To develop and validate a chemometric approach for simultaneous determination of multiple components in pharmaceutical mixed powders.
• To evaluate the performance of powder X-ray diffraction (PXRD) coupled with chemometrics for quantitative analysis.

Main Methods:

• Samples of caffeine anhydrate, acetaminophen, and lactose monohydrate were prepared in various ratios.
• Powder X-ray diffraction (PXRD) data were collected in specific angular ranges (2θ=5.00-30.0 and 35.0-45.0 degrees).
• Diffractograms were analyzed using conventional peak intensity, multi curve resolution-alternating least squares (MCR-ALS), and partial least squares (PLS) methods.

Main Results:

• Partial least squares (PLS) models demonstrated the highest accuracy in predicting component concentrations compared to other methods.
• Regression vectors in PLS models showed correlation with both the target compound and coexisting components.
• The combined PXRD and PLS approach proved effective for analyzing multi-component pharmaceutical formulations.

Conclusions:

• The combination of powder X-ray diffraction (PXRD) and partial least squares (PLS) is a powerful and accurate method for simultaneous quantitative analysis of multiple components in pharmaceutical powders.
• This approach offers a robust solution for quality control and formulation analysis in the pharmaceutical industry.