Development, validation and comparison of near infrared and Raman spectroscopic methods for fast characterization of tablets with amlodipine and valsartan.
The objective of this study was to develop, validate and compare NIR and Raman spectroscopic methods for fast characterization in terms of API content and tensile strength of fixed-dose combination tablets containing amlodipine and valsartan. For the APIs assay NIR-transmittance and Raman-reflectance methods were considered, whereas for the tensile strength assay Raman spectra were recorded in reflectance configuration and NIR spectra were recorded in both reflectance and transmittance. Multivariate calibration models (PLS) were built by applying different pre-processing methods (SNV, MSC, SD+SNV) on certain spectral regions. Correlating pre-processed spectral data with tablet properties resulted in highly predictive models except in the case of NIR-transmittance spectra for tensile strength estimation. The best models selected by cross-validation were further validated on independent samples in terms of linearity, trueness, accuracy and precision. Using Bland and Altman analysis the analytical performance of the NIR and Raman methods were compared, demonstrating their similarity considering the investigated applications. The two spectroscopic methods can be used in association to confirm each others results for at-line characterization of the pharmaceutical product.
Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy "Iuliu Hatieganu", 400012 Cluj-Napoca, Romania.
Tibor
T
Casian
Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy "Iuliu Hatieganu", 400012 Cluj-Napoca, Romania.
Andra
A
Reznek
Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy "Iuliu Hatieganu", 400012 Cluj-Napoca, Romania; "Lucian Blaga" University, Sibiu 550169, Romania.
Andreea Loredana
AL
Vonica-Gligor
Laboratory of Pharmaceutical Process Analytical Technology, Faculty of Pharmacy, Gent University, B-9000 Gent, Belgium.
Jeroen
J
Van Renterghem
Laboratory of Pharmaceutical Process Analytical Technology, Faculty of Pharmacy, Gent University, B-9000 Gent, Belgium.
Thomas
T
De Beer
Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy "Iuliu Hatieganu", 400012 Cluj-Napoca, Romania. Electronic address: tomutaioan@umfcluj.ro.
Ioan
I
Tomuță
D017311:Amlodipine / Q000737:chemistry*; D002138:Calibration; D013055:Spectrophotometry, Infrared / Q000379:methods*; D013059:Spectrum Analysis, Raman / Q000379:methods*; D013607:Tablets; D013718:Tensile Strength; D013997:Time Factors; D000068756:Valsartan / Q000737:chemistry*
D013607:Tablets; D017311:Amlodipine; D000068756:Valsartan
Near infrared spectroscopy; Pharmaceutical tablets; Process analytical technology; Raman spectroscopy; Validation