Advanced calibration strategy for in situ quantitative monitoring of phase transition processes in suspensions using FT-raman spectroscopy

Z.P. Chen, G. Fevotte, A. Caillet, D. Littlejohn, J. Morris

Research output: Contribution to journalArticle

37 Citations (Scopus)

Abstract

There is an increasing interest in using Raman spectroscopy to identify polymorphic forms and monitor phase changes in pharmaceutical products for quality control. Compared with other analytical techniques for the identification of polymorphs such as X-ray powder diffractometry and infrared spectroscopy, FT-Raman spectroscopy has the advantages of enabling fast, in situ, and nondestructive measurements of complex systems such as suspension samples. However, for suspension samples, Raman intensities depend on the analyte concentrations as well as the particle size, overall solid content, and homogeneity of the solid phase in the mixtures, which makes quantitative Raman analysis rather difficult. In this contribution, an advanced model has been derived to explicitly account for the confounding effects of a sample's physical properties on Raman intensities. On the basis of this model, a unique calibration strategy called multiplicative effects correction (MEC) was proposed to separate the Raman contributions due to changes in analyte concentration from those caused by the multiplicative confounding effects of the sample's physical properties. MEC has been applied to predict the anhydrate concentrations from in situ FT-Raman measurements made during the crystallization and phase transition processes of citric acid in water. The experimental results show that MEC can effectively correct for the confounding effects of the particle size and overall solid content of the solid phase on Raman intensities and, therefore, provide much more accurate in situ quantitative predictions of anhydrate concentration during crystallization and phase transition processes than traditional PLS calibration methods. (Abstract from: http://pubs.acs.org/doi/abs/10.1021/ac800987m)
LanguageEnglish
Pages6658-6665
Number of pages7
JournalAnalytical Chemistry
Volume80
Issue number17
Early online date30 Jul 2008
DOIs
Publication statusPublished - 1 Sep 2008

Fingerprint

Raman spectroscopy
Suspensions
Phase transitions
Calibration
Monitoring
Crystallization
Physical properties
Particle size
Polymorphism
Citric Acid
Powders
Quality control
Large scale systems
Infrared spectroscopy
X rays
Water
Pharmaceutical Preparations

Keywords

  • advanced calibration strategy
  • in situ quantitative monitoring
  • phase transition processes
  • suspensions
  • FT-Raman spectroscopy

Cite this

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Advanced calibration strategy for in situ quantitative monitoring of phase transition processes in suspensions using FT-raman spectroscopy. / Chen, Z.P.; Fevotte, G.; Caillet, A.; Littlejohn, D.; Morris, J.

In: Analytical Chemistry, Vol. 80, No. 17, 01.09.2008, p. 6658-6665.

Research output: Contribution to journalArticle

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