DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE

The development of a simple and efficient analytical method for determination of enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine was presented. The method was based on pre-column derivatization of 2-(aminomethyl)-1-ethylpyrrolidine with 4-nitrobenzoic acid completing separation of the enan...

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Autores principales: WANG,DAO-CAI, YAO,TIAN, QIAN,GUO-FEI, PU,LING-XIANG, YAO,SHUN, SONG,HANG
Lenguaje:English
Publicado: Sociedad Chilena de Química 2015
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Acceso en línea:http://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072015000100002
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spelling oai:scielo:S0717-970720150001000022015-04-21DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINEWANG,DAO-CAIYAO,TIANQIAN,GUO-FEIPU,LING-XIANGYAO,SHUNSONG,HANG HPLC enantiomeric separation 2-(aminomethyl)-1-ethylpyrrolidine pre-column derivatization The development of a simple and efficient analytical method for determination of enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine was presented. The method was based on pre-column derivatization of 2-(aminomethyl)-1-ethylpyrrolidine with 4-nitrobenzoic acid completing separation of the enantiomers on high performance liquid chromatographic (HPLC) chiral stationary phase (CSP). After optimizing all the effective parameters, the best performances were achieved on a Chiralcel OD-H analytical column (250 × 4.6 mm) using n-hexane: ethanol (98:2, v/v) containing 0.2% triethylamine as mobile phase with a flow rate of 1.0 mL min-1 at 25°C. Online UV and optical rotation (OR) detection was performed at 254 nm. The parameters which have an effect on chiral separation were investigated, including mobile phase additive, organic modifier type and concentration, column temperature and flow rate. The method was tested for precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness. The present method is expected to be accurate, stable, rapid and sensitive and can be used for the determination of the enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine in bulk samples.info:eu-repo/semantics/openAccessSociedad Chilena de QuímicaJournal of the Chilean Chemical Society v.60 n.1 20152015-03-01text/htmlhttp://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072015000100002en10.4067/S0717-97072015000100002
institution Scielo Chile
collection Scielo Chile
language English
topic HPLC
enantiomeric separation
2-(aminomethyl)-1-ethylpyrrolidine
pre-column derivatization
spellingShingle HPLC
enantiomeric separation
2-(aminomethyl)-1-ethylpyrrolidine
pre-column derivatization
WANG,DAO-CAI
YAO,TIAN
QIAN,GUO-FEI
PU,LING-XIANG
YAO,SHUN
SONG,HANG
DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
description The development of a simple and efficient analytical method for determination of enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine was presented. The method was based on pre-column derivatization of 2-(aminomethyl)-1-ethylpyrrolidine with 4-nitrobenzoic acid completing separation of the enantiomers on high performance liquid chromatographic (HPLC) chiral stationary phase (CSP). After optimizing all the effective parameters, the best performances were achieved on a Chiralcel OD-H analytical column (250 × 4.6 mm) using n-hexane: ethanol (98:2, v/v) containing 0.2% triethylamine as mobile phase with a flow rate of 1.0 mL min-1 at 25°C. Online UV and optical rotation (OR) detection was performed at 254 nm. The parameters which have an effect on chiral separation were investigated, including mobile phase additive, organic modifier type and concentration, column temperature and flow rate. The method was tested for precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness. The present method is expected to be accurate, stable, rapid and sensitive and can be used for the determination of the enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine in bulk samples.
author WANG,DAO-CAI
YAO,TIAN
QIAN,GUO-FEI
PU,LING-XIANG
YAO,SHUN
SONG,HANG
author_facet WANG,DAO-CAI
YAO,TIAN
QIAN,GUO-FEI
PU,LING-XIANG
YAO,SHUN
SONG,HANG
author_sort WANG,DAO-CAI
title DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
title_short DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
title_full DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
title_fullStr DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
title_full_unstemmed DEVELOPMENT OF AN EFFICIENT HPLC METHOD WITH PRE-COLUMN DERIVATIZATION FOR DETERMINATION OF ENANTIOMERIC PURITY OF 2-(AMINOMETHYL)-1-ETHYLPYRROLIDINE
title_sort development of an efficient hplc method with pre-column derivatization for determination of enantiomeric purity of 2-(aminomethyl)-1-ethylpyrrolidine
publisher Sociedad Chilena de Química
publishDate 2015
url http://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072015000100002
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