Simultaneous Quantification of Amorphous and Crystalline Valsartan in Tablets Using Raman Spectroscopy and Chemometrics Tools

Simultaneous Quantification of Amorphous and Crystalline Valsartan in Tablets Using Raman Spectroscopy and Chemometrics Tools

Valsartan is an antihypertensive active pharmaceutical ingredient (API), it is used in the amorphous state in the commercial products. As amorphous materials are metastable, amorphous valsartan can crystallize to valsartan E, promoting changes in the dissolution and bioavailability of the drug. Tabl...

Full description

Saved in:
Bibliographic Details
Published in:Journal of the Brazilian Chemical Society Vol. 33; no. 2; pp. 157 - 162
Main Authors: Domingos, Rafael C., Pinheiro, Adonilson, de Alvarenga Jr, Benedito, Carneiro, Renato, Farias, Marco
Format: Journal Article
Language:English
Published: Sociedade Brasileira de Química 01-02-2022
Subjects:
CHEMISTRY, MULTIDISCIPLINARY
NAS
valsartan
chemometrics
parameters of merit
iPLS
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary:Valsartan is an antihypertensive active pharmaceutical ingredient (API), it is used in the amorphous state in the commercial products. As amorphous materials are metastable, amorphous valsartan can crystallize to valsartan E, promoting changes in the dissolution and bioavailability of the drug. Tablets containing metastable forms of APIs need special conditions for transport and storage in order to avoid crystallization (from amorphous state) or polymorphic transitions (from less stable crystalline structures). A multivariate calibration model based on interval partial least squares (iPLS) regression allied to net analyte signal (NAS) algorithm was built to simultaneously quantify amorphous (VAL-AM) and crystalline (VAL-E) valsartan. Mixtures of VAL-AM and VAL-E were used to produce tablets in order to simulate the crystallization of VAL-AM in a range from 0 to 100% of conversion. The calibration set included 11 samples and 5 samples were used as the external validation set. The following parameters of merit (POM) were obtained for both polymorphs in order to evaluate the calibration model quality: root mean square error (RMSE) for cross validation (RMSECV), validation (RMSEV) and calibration (RMSEC), sensitivity (SEN), selectivity (SEL), analytical sensitivity (γ), inverse analytical sensitivity (γ-1), limit of detection (LOD) and limit of quantification (LOQ).
ISSN:0103-5053
1678-4790
DOI:10.21577/0103-5053.20210132