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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Sociedad Chilena de Química
2015
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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 |
work_keys_str_mv |
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_version_ |
1718445529598263296 |