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HERO ID
7696313
Reference Type
Journal Article
Title
Determination of Enantiomeric Purity of 2-Piperidinemethanamine by HPLC Combined With Pre-Column Derivation
Author(s)
Zhang, Y; Luo, Ji; Zeng, Hao; Yao, S; Chen, Hao; Song, H; ,
Year
2013
Is Peer Reviewed?
Yes
Journal
Asian Journal of Chemistry
ISSN:
0970-7077
EISSN:
0975-427X
Publisher
ASIAN JOURNAL OF CHEMISTRY
Location
SAHIBABAD
Volume
25
Issue
3
Page Numbers
1353-1356
Language
English
Web of Science Id
WOS:000312621400038
Abstract
A new HPLC method has been developed and validated for determination of enantiomeric purity of 2-piperidinemethanamine within a short run time of less than 10 min. The method was based on pre-column derivation of 2-piperidinemethanamine with 3,5-dinitrobenzoic acid and complete separation of enantiomers has been achieved on a CHI-DMB analytical column (250 mm x 4.6 mm) using n-hexane: ethanol (85:15 v/v) as mobile phase at a flow rate of 1.0 mL min(-1) under UV photodiode-array detector detection. Then the effects of mobile phase and temperature on enantioselectivity were further evaluated. The method was validated with respect to precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness. The recoveries were between 99.1 and 102.3 % with percentage relative standard deviation less than 1.17 %. The LOD and LOQ for first enantiomer were 13.7 and 46.3 mu g mL(-1) and for second enantiomer were 15.2 and 51.4 mu g mL(-1), respectively. This method is expected to be accurate, stable, rapid and sensitive for determination of the enantiomeric purity of 2-piperidinemethanamine in bulk samples.
Keywords
2-Piperidinemethanamine; Enantiomeric purity; Liquid chromatography; Method validation; Pre-column derivation
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