Development of micellar electrokinetic chromatography method for the determination of three defined impurities in indomethacin

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216208%3A11160%2F18%3A10382324" target="_blank" >RIV/00216208:11160/18:10382324 - isvavai.cz</a>

Výsledek na webu

<a href="http://onlinelibrary.wiley.com/doi/10.1002/elps.201800080" target="_blank" >http://onlinelibrary.wiley.com/doi/10.1002/elps.201800080</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1002/elps.201800080" target="_blank" >10.1002/elps.201800080</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Development of micellar electrokinetic chromatography method for the determination of three defined impurities in indomethacin

Popis výsledku v původním jazyce

A micellar electrokinetic chromatography method for the determination of indomethacin impurities (4-chlorobenzoic acid, 5-methoxy-2-methyl-3-indoleacetic acid, and 3,4-dichloroindomethacin) has been developed. A 64.5/56-cm fused silica 50 mu m id capillary with extended light path (150 mu m id) detection window was used. Internal standard was 1-naphthylacetic acid. The analytes were separated at 30 kV with DAD detection at 224 nm. A central composite face-centered design was applied for the optimization of the separation conditions. The effect of SDS concentration, content of methanol, concentration of phosphate buffer, and pH of the buffer were studied at three levels. The optimized background electrolyte was 20 mmol/L phosphate buffer (pH 7.57) containing 58 mmol/L SDS and 0% MeOH. Sufficient resolution of all compounds with Rs &gt;= 3.5 was achieved within 10 min. The method was validated for a range of 1.25-80 mu g/mL of each impurity corresponding to 0.05-3.2% relative to the concentration of indomethacin (2.5 mg/mL). The calibration curves were rectilinear with correlation coefficients r(2) exceeding 0.9994. The lower limit of quantification was 0.05% or 1.25 mu g/mL that complies with the reporting limits regarding the ICH Q3A guideline. The method was applied to purity assay of indomethacin in both bulk drug and gel.

Název v anglickém jazyce

Development of micellar electrokinetic chromatography method for the determination of three defined impurities in indomethacin

Popis výsledku anglicky

A micellar electrokinetic chromatography method for the determination of indomethacin impurities (4-chlorobenzoic acid, 5-methoxy-2-methyl-3-indoleacetic acid, and 3,4-dichloroindomethacin) has been developed. A 64.5/56-cm fused silica 50 mu m id capillary with extended light path (150 mu m id) detection window was used. Internal standard was 1-naphthylacetic acid. The analytes were separated at 30 kV with DAD detection at 224 nm. A central composite face-centered design was applied for the optimization of the separation conditions. The effect of SDS concentration, content of methanol, concentration of phosphate buffer, and pH of the buffer were studied at three levels. The optimized background electrolyte was 20 mmol/L phosphate buffer (pH 7.57) containing 58 mmol/L SDS and 0% MeOH. Sufficient resolution of all compounds with Rs &gt;= 3.5 was achieved within 10 min. The method was validated for a range of 1.25-80 mu g/mL of each impurity corresponding to 0.05-3.2% relative to the concentration of indomethacin (2.5 mg/mL). The calibration curves were rectilinear with correlation coefficients r(2) exceeding 0.9994. The lower limit of quantification was 0.05% or 1.25 mu g/mL that complies with the reporting limits regarding the ICH Q3A guideline. The method was applied to purity assay of indomethacin in both bulk drug and gel.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

30104 - Pharmacology and pharmacy

Projekt

<a href="/cs/project/EF15_003%2F0000465" target="_blank" >EF15_003/0000465: Vytvoření expertního týmu pro pokročilý výzkum v separačních vědách</a><br>

Návaznosti

P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)<br>S - Specificky vyzkum na vysokych skolach<br>I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Rok uplatnění

2018

Kód důvěrnosti údajů

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

Název periodika

Electrophoresis

ISSN

0173-0835

e-ISSN

—

Svazek periodika

39

Číslo periodika v rámci svazku

20

Stát vydavatele periodika

DE - Spolková republika Německo

Počet stran výsledku

8

Strana od-do

2550-2557

Kód UT WoS článku

000447441600007

EID výsledku v databázi Scopus

2-s2.0-85054766982