PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology

In this research, Analytical Quality by Design (AQbD) methodology was used to develop the HILIC-PDA-CAD method for the determination of magnesium, pyridoxine and thiamine content in a dietary supplement. Experiments were conducted on the Dionex Ulitimate 3000 HPLC system with PDA and CAD detectors....

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Autores principales: Rmandić Milena, Rađenović Miloš, Stanković Jovana, Protić Ana, Otašević Biljana, Malenović Anđelija
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Lenguaje:SR
Publicado: Pharmaceutical Association of Serbia, Belgrade, Serbia 2021
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Acceso en línea:https://doaj.org/article/5c644bf3aa284f508663722a5f37a925
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spelling oai:doaj.org-article:5c644bf3aa284f508663722a5f37a9252021-12-05T18:01:41ZPDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology0004-19632217-876710.5937/arhfarm71-32093https://doaj.org/article/5c644bf3aa284f508663722a5f37a9252021-01-01T00:00:00Zhttps://scindeks-clanci.ceon.rs/data/pdf/0004-1963/2021/0004-19632105378R.pdfhttps://doaj.org/toc/0004-1963https://doaj.org/toc/2217-8767In this research, Analytical Quality by Design (AQbD) methodology was used to develop the HILIC-PDA-CAD method for the determination of magnesium, pyridoxine and thiamine content in a dietary supplement. Experiments were conducted on the Dionex Ulitimate 3000 HPLC system with PDA and CAD detectors. Separations were performed on the ZIC-HILIC PEEK column (100 × 4.6 mm, 5 mm) with a mixture of acetonitrile, acetone and ammonium acetate/ammonium formate aqueous solution (48:12:40, v/v/v) as the mobile phase. The detection was performed at 220 nm. The optimal settings of CAD were defined with the one-factor-at-a-time approach: evaporation temperature 50°C, filter constant 10 s, pressure gas 60 psi. The influence of qualitative (salt type) and quantitative factors (pH and salt concentration) on the magnesium retention factor, k Mg and the selectivity factor between pyridoxine and chloride anion, a B6/Cl-, was tested using the I-optimal design. The design space was defined by Monte Carlo simulations and model coefficients' errors were propagated with the aim of identifying the conditions that meet the following criteria: k Mg <4 and a B6/Cl->3.5, with the probability p=95%. From the derived 2D-Design Space graph, 95 mM of ammonium formate pH 4.4 was selected as the optimal composition of the aqueous phase. The method was validated and its reliability in routine application was confirmed.Rmandić MilenaRađenović MilošStanković JovanaProtić AnaOtašević BiljanaMalenović AnđelijaPharmaceutical Association of Serbia, Belgrade, Serbiaarticlehilic-pda-cadmagnesiumpyridoxinethiamineaqbdPharmacy and materia medicaRS1-441SRArhiv za farmaciju, Vol 71, Iss 5, Pp 378-392 (2021)
institution DOAJ
collection DOAJ
language SR
topic hilic-pda-cad
magnesium
pyridoxine
thiamine
aqbd
Pharmacy and materia medica
RS1-441
spellingShingle hilic-pda-cad
magnesium
pyridoxine
thiamine
aqbd
Pharmacy and materia medica
RS1-441
Rmandić Milena
Rađenović Miloš
Stanković Jovana
Protić Ana
Otašević Biljana
Malenović Anđelija
PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
description In this research, Analytical Quality by Design (AQbD) methodology was used to develop the HILIC-PDA-CAD method for the determination of magnesium, pyridoxine and thiamine content in a dietary supplement. Experiments were conducted on the Dionex Ulitimate 3000 HPLC system with PDA and CAD detectors. Separations were performed on the ZIC-HILIC PEEK column (100 × 4.6 mm, 5 mm) with a mixture of acetonitrile, acetone and ammonium acetate/ammonium formate aqueous solution (48:12:40, v/v/v) as the mobile phase. The detection was performed at 220 nm. The optimal settings of CAD were defined with the one-factor-at-a-time approach: evaporation temperature 50°C, filter constant 10 s, pressure gas 60 psi. The influence of qualitative (salt type) and quantitative factors (pH and salt concentration) on the magnesium retention factor, k Mg and the selectivity factor between pyridoxine and chloride anion, a B6/Cl-, was tested using the I-optimal design. The design space was defined by Monte Carlo simulations and model coefficients' errors were propagated with the aim of identifying the conditions that meet the following criteria: k Mg <4 and a B6/Cl->3.5, with the probability p=95%. From the derived 2D-Design Space graph, 95 mM of ammonium formate pH 4.4 was selected as the optimal composition of the aqueous phase. The method was validated and its reliability in routine application was confirmed.
format article
author Rmandić Milena
Rađenović Miloš
Stanković Jovana
Protić Ana
Otašević Biljana
Malenović Anđelija
author_facet Rmandić Milena
Rađenović Miloš
Stanković Jovana
Protić Ana
Otašević Biljana
Malenović Anđelija
author_sort Rmandić Milena
title PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
title_short PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
title_full PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
title_fullStr PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
title_full_unstemmed PDA-CAD method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
title_sort pda-cad method for the determination of magnesium, pyridoxine and thiamine in a dietary supplement supported by analytical quality by design methodology
publisher Pharmaceutical Association of Serbia, Belgrade, Serbia
publishDate 2021
url https://doaj.org/article/5c644bf3aa284f508663722a5f37a925
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AT proticana pdacadmethodforthedeterminationofmagnesiumpyridoxineandthiamineinadietarysupplementsupportedbyanalyticalqualitybydesignmethodology
AT otasevicbiljana pdacadmethodforthedeterminationofmagnesiumpyridoxineandthiamineinadietarysupplementsupportedbyanalyticalqualitybydesignmethodology
AT malenovicanđelija pdacadmethodforthedeterminationofmagnesiumpyridoxineandthiamineinadietarysupplementsupportedbyanalyticalqualitybydesignmethodology
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