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Updated: Mar 24, 2026

A Package of Established Analytical Tools to Investigate the Solid-State Alteration of Lipid-Based Excipients
Published on: August 9, 2022
Semi-quantitative prediction of a multiple API solid dosage form with a combination of vibrational spectroscopy
A Hertrampf1, R M Sousa2, J C Menezes3
1Quality Operations, Laboratory for Liquid Products, Merck Serono, Darmstadt, Germany; Institute for Biotechnology and Biosciences, Instituto Superior Técnico, Universidade de Lisboa, Portugal.
Near-infrared (NIR) and Raman spectroscopy effectively identify and quantify pharmaceutical dosages. Combining these techniques offers enhanced accuracy for quality control, improving drug safety and efficacy.
Area of Science:
- Pharmaceutical analysis
- Spectroscopic techniques
- Chemometrics
Background:
- Pharmaceutical quality control (QC) is vital for ensuring drug safety, efficacy, and quality.
- Vibrational spectroscopy, including Near-Infrared Spectroscopy (NIRS) and Raman spectroscopy, offers rapid analysis for raw materials and final products.
- Accurate identification and quantification of active pharmaceutical ingredients (APIs) are critical QC functions.
Purpose of the Study:
- To evaluate Near-Infrared Spectroscopy (NIRS) and Raman spectroscopy for identifying and quantifying different dosages of pharmaceutical tablets.
- To develop multivariate models for discriminating between dosages and predicting API content.
- To investigate the synergistic benefits of combining NIRS and Raman spectroscopy for pharmaceutical analysis.
Main Methods:
- Analysis of pharmaceutical tablets containing bisoprolol and hydrochlorothiazide using NIRS and Raman spectroscopy.
- Development of multivariate calibration models using Partial Least Squares (PLS) regression.
- Application of multiblock PLS (MB-PLS) and sequential-orthogonalised PLS (SO-PLS) for combined spectroscopic data analysis.
Main Results:
- NIRS demonstrated superior performance over Raman spectroscopy for both identification and semi-quantitative prediction of drug dosages.
- Multiblock analysis revealed that NIRS and Raman spectroscopy provide complementary information, enhancing analytical capabilities.
- Combined spectroscopic approaches using MB-PLS and SO-PLS showed potential for improved accuracy in identification and quantification.
Conclusions:
- Both NIRS and Raman spectroscopy are valuable tools for pharmaceutical QC, with NIRS showing higher efficacy in this study.
- Combining NIRS and Raman spectroscopy offers significant advantages, leveraging unique information from each technique for more robust analysis.
- Multivariate chemometric methods, particularly multiblock approaches, are effective for integrating data from multiple spectroscopic sources for enhanced pharmaceutical analysis.
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