XIV
h
International Conference on Molecular Spectroscopy, Białka Tatrzańska 2017
309
T6: P–17
Quantitative analysis of pharmaceutical suspensions by FT Raman
spectroscopy
Sylwester Mazurek
1
, and Roman Szostak
1
1
Department of Chemistry, University of Wrocław, 14 F. Joliot-Curie, 50-383 Wrocław, Poland,
e-mail: sylwester.mazurek@chem.uni.wroc.pl
Suspensions are among the most difficult forms of pharmaceutical products to analyze.
Presence of dispersed solid particles in the studied samples can adversely affect reproducibility
of measurements. This makes quantitative analysis of suspensions problematic and challenging.
In this report, we describe an FT-Raman quantitative analysis of nifuroxazide, acetaminophen,
ibuprofen and naproxen in commercial oral suspensions. To quantify active pharmaceutical
ingredients (APIs) in the studied preparations systems mimicking analyzed products were
constructed. The spectral compatibility of the laboratory prepared samples with the studied
pharmaceuticals was checked on the basis of PCA analysis. The pharmaceutical suspensions
containing 1.7–4.0% (w/w) of the API were examined on the basis of partial least squares (PLS)
and counter-propagation artificial neural network models (CP-ANN). To compare the predictive
abilities of the developed models the relative standard errors of prediction were calculated for
the calibration and validation data sets.
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Fig. 1. FT Raman spectra of nifuroxazide and ibuprofen and their studied commercial suspensions.
Four medicines were successfully analyzed. The recovery for the quantified APIs was found to
be in the 99.3–101.2% and in the 98.2–100.2% ranges for PLS and ANN modeling, respectively.
The best results were obtained for suspensions containing nifuroxazide, an ingredient giving a
very strong Raman signal. The analyzed suspensions of acetaminophen, naproxen and ibuprofen
containing approximately 2% (w/w) of API can be quantified with an acceptable accuracy, but it
requires an improvement of the signal-to-noise (SNR) in their Raman spectra. The 20-fold
worsening of the SNR in comparison with the spectra of nifuroxazide suspensions resulted in an
approximately twofold increase of the prediction error values during modeling.
Keywords: oral suspension; Raman spectroscopy; quantitative analysi; multivariate calibration
XIV
h
International Conference on Molecular Spectroscopy, Białka Tatrzańska 2017
310
T6: P–18
Applications of Raman microscopy for on-line monitoring of
disintegration of pharmaceutical tablets
Tereza Helesicova
1,3
, Pavel Matejka
2
, and Tomas Pekarek
3
1 Department of Analytical Chemistry, University of Chemistry and Technology Prague, Technicka 5,
166 28, Prague, Czech Republic, e-mail: Tereza.Helesicova@vscht.cz
2 Department of Physical Chemistry, University of Chemistry and Technology Prague, Technicka 5,
166 28, Prague, Czech Republic
3 Zentiva, k.s, U Kabelovny 130, 102 37, Prague, Czech Republic
Raman spectroscopy is an effective technique for selective examination of multicomponent
materials, specifically in microscopic and imaging designs it has become a very powerful tool in
pharmaceutical research and development [1]. During development of pharmaceuticals forms,
the emphasis is focused on testing of physicochemical properties (solubility, temperature
stability and other) of active pharmaceutical ingredient (API) as well as on the features of the
final drug formulation. In vitro dissolution studies [2] represent an important and valuable tool
for development and characterization of drug forms. However, traditional dissolution tests do
not provide information; what is happened on the surface (outer interphase) of tested tablet
(composition and structure), that changes during dissolution. This information about the tested
drug is necessary to be obtained when the dissolution test failed and it is frequently very difficult
to determine what caused the failure.
The goal of this study is the methodological development of micro-spectroscopic tools with
the final application of Raman microscopy for more or less routine monitoring of disintegration
in dissolution medium (especially aqueous medium). The method is able to identify the surface
(interphase) changes, more precisely the changes in composition of tablet, which occur during
interaction of the drug form with dissolution medium. Time dependent Raman chemical maps
provide understanding of processes (solvation, solvent penetration, API dissolution etc.), which
occur on the surface on dissolving tablet.
Keywords: disintegration; Raman mapping; active pharmaceutical ingredient
References
[1] T. Vankeirsbilck, A. Vercauteren,W. Baeyens, G. Van der Weken, F. Verpoort, G. Vergote, J. P.
Remon, TRAC-Trend in Anal. Chem. 21 (2002) 869.
[2] J. Rivera-Leyva, M. Garcia-Flores, A. Valladares-Mendez, L. M. Orozco-Castellanos, M. Martinez-
Alfaro, Indian J. Pharm. Sci. 74 (2012) 312.
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