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Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram

A novel economic procedure for the simultaneous stereospecific separation and analysis of (R)- and (S)-citalopram and its related substances or impurities has been developed and validated. Chromatography was performed on silica gel 60 F254 plates with acetonitrile: methanol: water (15:2.5:2.5: v/v/v...

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Autor principal: Soliman, Suzan Mahmoud
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Master Publishing Group 2012
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3614854/
https://www.ncbi.nlm.nih.gov/pubmed/23675256
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author Soliman, Suzan Mahmoud
author_facet Soliman, Suzan Mahmoud
author_sort Soliman, Suzan Mahmoud
collection PubMed
description A novel economic procedure for the simultaneous stereospecific separation and analysis of (R)- and (S)-citalopram and its related substances or impurities has been developed and validated. Chromatography was performed on silica gel 60 F254 plates with acetonitrile: methanol: water (15:2.5:2.5: v/v/v) as a mobile phase containing 1.5 mM norvancomycin or 2.5 mM vancomycin as a selector at ambient temperature. (R)- and (S)-citalopram enantiomers in presence of its related substances; citalopram citadiol and citalopram N-oxide were well separated with significant Rf values of 0.33 ± 0.02, 0.85 ± 0.02, 0.45 ± 0.02 and 0.22 ± 0.02, respectively. The spots were detected with either iodine vapor, or by use of a UV lamp followed by densitometric measurement at 239 nm. All variables affecting the resolution, such as concentration of chiral selectors, mobile phase system at different temperatures and pH-values were investigated and the conditions were optimized. Calibration plots for analysis of (R)- and (S)-enantiomers were linear in the range of 0.2-16.8 μg/10 μl (R≥0.9994, n=6) with acceptable precision (%RSD<2.0) and accuracy (99.70 ± 0.85% and 99.51 ± 0.61% for (S)-citalopram and escitalopram, respectively). The limit of detection and quantification were 0.08 μg/10 μl and 0.25 μg/10 μl, respectively, for (R)- and (S)-citalopram. The proposed method is simple, selective, and robust and can be applied for quantitative determination of enantiomeric purity of (R)- and (S)-citalopram (escitalopram) as well as the related impurities in drug substances and pharmaceutical preparations. The method can be useful to investigate adulteration of pure isomer with the cheep racemic form.
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spelling pubmed-36148542013-05-01 Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram Soliman, Suzan Mahmoud Int J Biomed Sci Article A novel economic procedure for the simultaneous stereospecific separation and analysis of (R)- and (S)-citalopram and its related substances or impurities has been developed and validated. Chromatography was performed on silica gel 60 F254 plates with acetonitrile: methanol: water (15:2.5:2.5: v/v/v) as a mobile phase containing 1.5 mM norvancomycin or 2.5 mM vancomycin as a selector at ambient temperature. (R)- and (S)-citalopram enantiomers in presence of its related substances; citalopram citadiol and citalopram N-oxide were well separated with significant Rf values of 0.33 ± 0.02, 0.85 ± 0.02, 0.45 ± 0.02 and 0.22 ± 0.02, respectively. The spots were detected with either iodine vapor, or by use of a UV lamp followed by densitometric measurement at 239 nm. All variables affecting the resolution, such as concentration of chiral selectors, mobile phase system at different temperatures and pH-values were investigated and the conditions were optimized. Calibration plots for analysis of (R)- and (S)-enantiomers were linear in the range of 0.2-16.8 μg/10 μl (R≥0.9994, n=6) with acceptable precision (%RSD<2.0) and accuracy (99.70 ± 0.85% and 99.51 ± 0.61% for (S)-citalopram and escitalopram, respectively). The limit of detection and quantification were 0.08 μg/10 μl and 0.25 μg/10 μl, respectively, for (R)- and (S)-citalopram. The proposed method is simple, selective, and robust and can be applied for quantitative determination of enantiomeric purity of (R)- and (S)-citalopram (escitalopram) as well as the related impurities in drug substances and pharmaceutical preparations. The method can be useful to investigate adulteration of pure isomer with the cheep racemic form. Master Publishing Group 2012-03 /pmc/articles/PMC3614854/ /pubmed/23675256 Text en © Suzan Mahmoud Soliman et al. Licensee Master Publishing Group http://creativecommons.org/licenses/by/2.5/ This is an open-access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/2.5/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.
spellingShingle Article
Soliman, Suzan Mahmoud
Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title_full Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title_fullStr Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title_full_unstemmed Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title_short Validated Densitometric TLC-Method for the Simultaneous Analysis of (R)- and (S)-Citalopram and its Related Substances Using Macrocyclic Antibiotic as a Chiral Selector: Application to the Determination of Enantiomeric Purity of Escitalopram
title_sort validated densitometric tlc-method for the simultaneous analysis of (r)- and (s)-citalopram and its related substances using macrocyclic antibiotic as a chiral selector: application to the determination of enantiomeric purity of escitalopram
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3614854/
https://www.ncbi.nlm.nih.gov/pubmed/23675256
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