Determination of Atropine Enantiomers in Ophthalmic Solutions by Liquid Chromatography Using a Chiral AGP (R) Column


Autoria(s): SOARES, Renata; SINGH, Anil Kumar; KEDOR-HACKMANN, Erika Rosa Maria; SANTORO, Maria Ines Rocha Miritello
Contribuinte(s)

UNIVERSIDADE DE SÃO PAULO

Data(s)

19/10/2012

19/10/2012

2009

Resumo

Many therapeutic agents are commercialized under their racemic form. The enantiomers can show differences in the pharmacokinetic and pharmacodynamic profile. The use of a pure enantiomer in pharmaceutical formulations may result in a better therapeutic index and fewer adverse effects. Atropine, an alkaloid of Atropa belladonna, is a racemic mixture of l-hyoscyamine and d-hyoscyamine. It is widely used to dilate the pupil. To quantify these enantiomers in ophthalmic solutions, an HPLC method was developed and validated using a Chiral AGP (R) column at 20 degrees C. The mobile phase consisted of a buffered phosphate solution (containing 10 mM 1-octanesulfonic acid sodium salt and 7.5 mM triethylamine, adjusted to pH 7.0 with orthophosphoric acid) and acetonitrile (99 + 1, v/v). The flow rate was 0.6 mL/min, with UV detection at 205 nm. In the concentration range of 14.0-26.0 mu g/mL, the method was found to be linear (r > 0.9999), accurate (with recovery of 100.1-100.5%), and precise (RSD system: <= 0.6%; RSD intraday: <= 1.1%; RSD interday: <= 0.9%). The method was specific, and the standard and sample solutions were stable for up to 72 h. The factorial design assures robustness with a variation of +/-10% in the mobile phase components and 2 degrees C of column temperature. The complete validation, including stress testing and factorial design, was studied and is presented in this research.

Identificador

JOURNAL OF AOAC INTERNATIONAL, v.92, n.6, p.1663-1672, 2009

1060-3271

http://producao.usp.br/handle/BDPI/19684

http://apps.isiknowledge.com/InboundService.do?Func=Frame&product=WOS&action=retrieve&SrcApp=EndNote&UT=000273591600009&Init=Yes&SrcAuth=ResearchSoft&mode=FullRecord

Idioma(s)

eng

Publicador

AOAC INT

Relação

Journal of Aoac International

Direitos

restrictedAccess

Copyright AOAC INT

Palavras-Chave #HUMAN ALPHA(1)-ACID GLYCOPROTEIN #BONDED STATIONARY PHASE #CAPILLARY-ELECTROPHORESIS #ALPHA-1-ACID GLYCOPROTEIN #TROPANE ALKALOIDS #EXPERIMENTAL-DESIGN #CIRCULAR-DICHROISM #GENETIC-VARIANTS #BINDING #ROBUSTNESS #Chemistry, Analytical #Food Science & Technology
Tipo

article

original article

publishedVersion