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Related Concept Videos

Raman Spectroscopy Instrumentation: Overview01:26

Raman Spectroscopy Instrumentation: Overview

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A conventional Raman spectrophotometer includes a laser source, a sample holding system, a wavelength selector, and a detector.
The monochromatic laser source, typically using visible or near-infrared radiation, generates a highly focused beam of light. This light interacts with the molecules of the sample, scattering some of the light. Liquid and gaseous samples are usually tested in ordinary glass capillaries, while solids can be analyzed as powders packed in capillaries or as potassium...
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Raman Spectroscopy: Overview01:20

Raman Spectroscopy: Overview

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The underlying principle of Raman spectroscopy is based on the interaction between light and matter, specifically molecules' inelastic scattering of photons. When a monochromatic beam of light, typically from a laser source, interacts with a sample, most scattered light has the same frequency as the incident light. This is known as Rayleigh scattering.
However, a small fraction of the scattered light exhibits a frequency shift due to the exchange of energy between the incident photons and...
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Volatilization01:10

Volatilization

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Volatilization gravimetry is an analytical technique that measures the mass lost due to the volatilization of the substance. This technique is used to estimate the amount of volatile material in a sample. To perform this method, heat a known amount of the sample to a high temperature in a crucible or other suitable vessel. The volatile substance in the sample evaporates, and the vapor is completely expelled from the crucible either by heating the sample or bubbling a stream of inert gas through...
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Related Experiment Video

Updated: Jan 13, 2026

O-cresol Concentration Online Measurement Based On Near Infrared Spectroscopy Via Partial Least Square Regression
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Quantitative analysis of granules moisture content within a fluidized bed drying process using simultaneously

Chuan-Chuan Li1, Wei-Ping Zhu1

  • 1Shanghai Key Laboratory of Chemical Biology, School of Pharmacy, East China University of Science and Technology, Shanghai 200237, PR China.

International Journal of Pharmaceutics
|January 8, 2026
PubMed
Summary

Near-infrared (NIR) spectroscopy with Partial Least Squares (PLS) models offers superior accuracy for monitoring granule moisture content during fluidized bed drying (FBD) compared to Raman spectroscopy, enabling precise endpoint determination.

Keywords:
A. Fluid-bed dryingB. Granule moistureC. Near-infrared spectroscopyD. Raman spectroscopyE. ChemometricsF. Process monitoring

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Area of Science:

  • Pharmaceutical Manufacturing
  • Process Analytical Technology (PAT)
  • Spectroscopy

Background:

  • Effective monitoring of granule moisture content (MC) is critical for quality control in fluidized bed drying (FBD).
  • Accurate determination of the drying endpoint ensures product quality and process efficiency in pharmaceutical manufacturing.
  • Traditional methods can be time-consuming, necessitating advanced techniques for real-time analysis.

Purpose of the Study:

  • To compare Near-infrared (NIR) and Raman spectroscopy for monitoring granule MC during hydroxychloroquine sulfate (HCQ) FBD.
  • To evaluate the performance of chemometric models (PLS, SVM) and spectral preprocessing techniques for MC determination.
  • To establish an integrated approach for real-time process understanding and drying endpoint detection.

Main Methods:

  • Comparative analysis of NIR and Raman spectral data acquired during large-scale HCQ manufacturing.
  • Development of calibration models using Partial Least Squares (PLS) and Support Vector Machine (SVM) regression.
  • Application of various spectral preprocessing techniques (SNV, MSC, SG, ND, derivatives, OSC) to enhance model accuracy.

Main Results:

  • NIR spectroscopy combined with PLS demonstrated superior predictive performance (R²p=0.9990, RMSEP=0.105) for MC monitoring.
  • Raman spectroscopy with SVM showed good performance (R²p=0.9600, RMSEP=0.474) but was less accurate than NIR.
  • At-line Raman spectra provided external verification for NIR results, enhancing confidence in MC analysis.

Conclusions:

  • Online NIR spectroscopy, integrated with humidity/temperature data loggers, provides real-time process understanding in FBD.
  • This integrated approach enables accurate and rapid determination of the drying endpoint, typically between 1.5% and 2.5% MC.
  • The study validates the use of advanced spectroscopic techniques for robust quality control in pharmaceutical drying processes.