Document Detail


HPLC/ELSD analysis of amidated bile acids: An effective and rapid way to assist continuous flow chemistry processes.
MedLine Citation:
PMID:  23141350     Owner:  NLM     Status:  In-Data-Review    
Abstract/OtherAbstract:
The employment of the flow N-acyl amidation of natural bile acids (BAs) required the in-line connection with suitable analytical tools enabling the determination of reaction yields as well as of the purity grade of the synthesized glyco- and tauro-conjugated derivatives. In this framework, a unique HPLC method was successfully established and validated for ursodeoxycholic (UDCA), chenodeoxycholic (CDCA), deoxycholic (DCA) and cholic (CA) acids, as well as the corresponding glyco- and tauro-conjugated forms. Because of the shared absence of relevant chromophoric moieties in the sample structure, an evaporative light scattering detector (ELSD) was profitably utilized for the analysis of such steroidal species. For each of the investigated compounds, all the runs were contemporarily carried out on the acidic free and the two relative conjugated variants. The different ELSD response of the free and the corresponding conjugated BAs, imposed to build-up separate calibration curves. In all the cases, very good precision (RSD% values ranging from 1.04 to 6.40% in the long-period) and accuracy (Recovery% values ranging from 96.03 to 111.14% in the long-period) values along with appreciably low LOD and LOQ values (the former being within the range 1-27ngmL(-1) and the latter within the range 2-44ngmL(-1)) turned out.
Authors:
Roccaldo Sardella; Antimo Gioiello; Federica Ianni; Francesco Venturoni; Benedetto Natalini
Publication Detail:
Type:  Journal Article     Date:  2012-08-10
Journal Detail:
Title:  Talanta     Volume:  100     ISSN:  1873-3573     ISO Abbreviation:  Talanta     Publication Date:  2012 Oct 
Date Detail:
Created Date:  2012-11-12     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  2984816R     Medline TA:  Talanta     Country:  Netherlands    
Other Details:
Languages:  eng     Pagination:  364-71     Citation Subset:  IM    
Copyright Information:
Copyright © 2012 Elsevier B.V. All rights reserved.
Affiliation:
Dipartimento di Chimica e Tecnologia del Farmaco, Università degli Studi di Perugia, Perugia, Italy.
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