title: Inter-laboratory verification of European pharmacopoeia monograph on derivative spectrophotometry method and its application for chitosan hydrochloride.
abstract: Inter-laboratory verification of European pharmacopoeia (EP) monograph on derivative spectrophotometry (DS) method and its application for chitosan hydrochloride was carried out on two generation of instruments (earlier GBC Cintra 20 and current technology TS Evolution 300). Instruments operate with different versions of Savitzky-Golay algorithm and modes of generating digital derivative spectra. For resolution power parameter, defined as the amplitude ratio A/B in DS method EP monograph, comparable results were obtained only with algorithm's parameters smoothing points (SP) 7 and the 2nd degree polynomial and those provided corresponding data with other two modes on TS Evolution 300 Medium digital indirect and Medium digital direct. Using quoted algorithm's parameters, the differences in percentages between the amplitude ratio A/B averages, were within accepted criteria (±3%) for assay of drug product for method transfer. The deviation of 1.76% for the degree of deacetylation assessment of chitosan hydrochloride, determined on two instruments, (amplitude (1)D202; the 2nd degree polynomial and SP 9 in Savitzky-Golay algorithm), was acceptable, since it was within allowed criteria (±2%) for assay deviation of drug substance, for method transfer in pharmaceutical analyses.
authors.affiliation: Department of Pharmaceutical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia. Electronic address: bojan@pharmacy.bg.ac.rs.
authors.forename: Bojan
authors.initials: B
authors.lastname: Marković
authors.affiliation: Department of Pharmaceutical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia.
authors.forename: Janko
authors.initials: J
authors.lastname: Ignjatović
authors.affiliation: Department of Analytical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia.
authors.forename: Mirjana
authors.initials: M
authors.lastname: Vujadinović
authors.affiliation: Department of Pharmaceutical Technology, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia.
authors.forename: Vedrana
authors.initials: V
authors.lastname: Savić
authors.affiliation: Department of Pharmaceutical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia.
authors.forename: Sote
authors.initials: S
authors.lastname: Vladimirov
authors.affiliation: Department of Analytical Chemistry, University of Belgrade, Faculty of Pharmacy, Vojvode Stepe 450, 11221 Belgrade, Serbia.
authors.forename: Katarina
authors.initials: K
authors.lastname: Karljiković-Rajić
mesh_terms: D000107:Acetylation; D000465:Algorithms; D048271:Chitosan / Q000737:chemistry*; D013053:Spectrophotometry; D013056:Spectrophotometry, Ultraviolet
chemical_list: D048271:Chitosan
keywords: Chitosan hydrochloride-degree of deacetylation; Derivative spectrophotometry (DS); European pharmacopoeia (EP); Instrumental and algorithm’s parameters; Method transfer; Resolution power parameter the amplitude A/B ratio