Using single-isomer octa(6-O-sulfo)-gamma-cyclodextrin for fast capillary zone electrophoretic enantioseparation of pindolol: Determination of complexation constants, software-assisted optimization, and method validation

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216208%3A11310%2F18%3A10379256" target="_blank" >RIV/00216208:11310/18:10379256 - isvavai.cz</a>

Výsledek na webu

<a href="https://doi.org/10.1016/j.chroma.2018.07.020" target="_blank" >https://doi.org/10.1016/j.chroma.2018.07.020</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1016/j.chroma.2018.07.020" target="_blank" >10.1016/j.chroma.2018.07.020</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Using single-isomer octa(6-O-sulfo)-gamma-cyclodextrin for fast capillary zone electrophoretic enantioseparation of pindolol: Determination of complexation constants, software-assisted optimization, and method validation

Popis výsledku v původním jazyce

The present study describes a rapid and effective capillary electrophoresis (CE) method for the enantioseparation of pindolol using single-isomer octa(6-O-sulfo)-gamma-cyclodextrin. The complexation parameters were determined under neutral and high pH conditions to identify optimal separation conditions using a theoretical model. Baseline separation of pindolol enantiomers was achieved within 6 min in a sodium/MOPS buffer, pH 7.2, with a selector concentration of 6 mM. The method was validated according to the ICH guidelines using imidazole as an internal standard. Low limits of detection and quantification were found, specifically 1.2 mu g/mL and 4 mu g/mL (0.6 mu g/mL and 2 mu g/mL per enantiomer), respectively. The calibration curves showed good linearity, with a coefficient of determination R-2 &gt;= 0.999 over a 5 - 55 mu g/mL concentration range and over a 50 - 300 mu g/mL concentration range of the racemic mixture. The relative standard deviations (%RSD) of intra-day and inter-day precision were lower than 8% at LOQ level, lower than 3% at 50 mu g/mL level and lower than 1.5% at 300 mu g/mL level. Accuracy ranged from 95 to 103% (106% at LOQ level). The proposed method was successfully tested on a medical formulation of Visken (R) Sandoz intravenous solution and Visken (R) Teofarma pills for oral use.

Název v anglickém jazyce

Using single-isomer octa(6-O-sulfo)-gamma-cyclodextrin for fast capillary zone electrophoretic enantioseparation of pindolol: Determination of complexation constants, software-assisted optimization, and method validation

Popis výsledku anglicky

The present study describes a rapid and effective capillary electrophoresis (CE) method for the enantioseparation of pindolol using single-isomer octa(6-O-sulfo)-gamma-cyclodextrin. The complexation parameters were determined under neutral and high pH conditions to identify optimal separation conditions using a theoretical model. Baseline separation of pindolol enantiomers was achieved within 6 min in a sodium/MOPS buffer, pH 7.2, with a selector concentration of 6 mM. The method was validated according to the ICH guidelines using imidazole as an internal standard. Low limits of detection and quantification were found, specifically 1.2 mu g/mL and 4 mu g/mL (0.6 mu g/mL and 2 mu g/mL per enantiomer), respectively. The calibration curves showed good linearity, with a coefficient of determination R-2 &gt;= 0.999 over a 5 - 55 mu g/mL concentration range and over a 50 - 300 mu g/mL concentration range of the racemic mixture. The relative standard deviations (%RSD) of intra-day and inter-day precision were lower than 8% at LOQ level, lower than 3% at 50 mu g/mL level and lower than 1.5% at 300 mu g/mL level. Accuracy ranged from 95 to 103% (106% at LOQ level). The proposed method was successfully tested on a medical formulation of Visken (R) Sandoz intravenous solution and Visken (R) Teofarma pills for oral use.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

10406 - Analytical chemistry

Projekt

<a href="/cs/project/GA16-05942S" target="_blank" >GA16-05942S: Gradientová chromatofokusace a izoelektrická fokusace - nástroje pro separaci proteinů</a><br>

Návaznosti

P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)

Rok uplatnění

2018

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název periodika

Journal of Chromatography A

ISSN

0021-9673

e-ISSN

—

Svazek periodika

1568

Číslo periodika v rámci svazku

September

Stát vydavatele periodika

NL - Nizozemsko

Počet stran výsledku

8

Strana od-do

214-221

Kód UT WoS článku

000443669600023

EID výsledku v databázi Scopus

2-s2.0-85049580456