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1.
Anal Chem ; 73(16): 3838-44, 2001 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-11534705

RESUMO

Ionic substances with melting points at or close to room temperature are referred to as ionic liquids. Interest in ionic liquids for their potential in different chemical processes is increasing, because they are environmentally benign and are good solvents for a wide range of both organic and inorganic materials. In this study, a capillary electrophoretic method for resolving phenolic compounds found in grape seed extracts is reported. The method, in which 1-alkyl-3-methylimidazolium-based ionic liquids are used as the running electrolytes, is simple and reproducible. The separation mechanism seems to involve association between the imidazolium cations and the polyphenols. The role of the alkyl substituents on the imidazolium cations was investigated and will be discussed.

2.
Fresenius J Anal Chem ; 369(3-4): 212-9, 2001 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-11293696

RESUMO

Enantiomers of clenbuterol, salbutamol and tulobuterol were directly separated and quantitated from a spiked sample by capillary electrophoresis (CE) using sulfaited beta-cyclodextrin (SCD) as chiral selector and phosphate as running buffer. The SCD and buffer concentration, pH and field strength were the parameters studied to optimize the separation. Optimal separation was obtained using 50 mM of phosphate monobasic at pH = 2.24, 0.25% (w/w) of sulfated cyclodextrin and a field strength of 10 kV, with 20 min total time analysis. Comparison between two different injection modes (hydrodynamic and electrokinetic) was made. In the hydrodynamic mode, repeatability (expressed as relative standard deviation, RSD) was less than 1.2% for migration times for all the analyte peaks and less than 2% for peak area percentages. With respect to reproducibility, RSD was less than 3.8% for migration time and less than 3% for peak area percentages. Calibration curves were set up for two different sample concentration ranges (1 to 10 microg mL(-1) and 160-800 ng mL(-1), of each of the racemates studied). Although the electrokinetic injection mode for an aqueous sample appeared to suffer from some enantiodiscrimination, calibration curves were linear in the range between 1 and 10 ng mL(-1) with regression coefficients ranging from 0.9996 to 0.9952. As in the case of hydrodynamic injection, the method was tested with a spiked sample.


Assuntos
Albuterol/análise , Clembuterol/análise , Terbutalina/análogos & derivados , Terbutalina/análise , beta-Ciclodextrinas , Albuterol/química , Broncodilatadores/análise , Broncodilatadores/química , Soluções Tampão , Clembuterol/química , Ciclodextrinas , Eletroforese Capilar/métodos , Indicadores e Reagentes , Estrutura Molecular , Reprodutibilidade dos Testes , Estereoisomerismo , Terbutalina/química
3.
Fresenius J Anal Chem ; 369(5): 412-7, 2001 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-11270220

RESUMO

The enantioseparation capabilities of three different functionalized beta-cyclodextrins, two sulfated beta-cyclodextrins with 4 and 15 nominal degrees of substitution and a phosphated beta-cyclodextrin with 8 degrees of substitution, were compared. While anodic detection was used with both sulfated cyclodextrins, the phosphated cyclodextrin required cathodic detection suggesting either lower ionization of the phosphated cyclodextrin or generally lower affinity of the analytes for the phosphated cyclodextrin. The effects of several experimental parameters were evaluated with respect to enantioseparation. The degrees of substitution of the cyclodextrin, pH of the background electrolyte as well as the concentration of the functionalized beta-cyclodextrin, each had a significant influence on the successful enantiomeric separation of the chiral drugs investigated.


Assuntos
Ciclodextrinas/química , Eletroforese Capilar/métodos , Concentração de Íons de Hidrogênio , Fosfatos/química , Estereoisomerismo , Sulfatos/química
4.
Analyst ; 125(10): 1719-24, 2000 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-11070539

RESUMO

Continuous free flow electrophoresis was investigated as a tool for the preparative chiral separation of piperoxan using a sulfated cyclodextrin chiral additive. In the absence of chiral additive, the sample stream was deflected cathodically. However, the presence of sulfated cyclodextrin in the run buffer caused anodic deflection and splitting of the sample stream into two streams, each enriched in one enantiomer. Although the sulfated cyclodextrin used was comprised of a mixture of homologues and isomers, this polydispersity did not seem to significantly impact band dispersion. Sample introduction rates ranged from approximately 0.9-7.2 mg h-1. Maximum resolution was 0.53, using an applied voltage of 220 V, buffer composition of 0.075% sulfated cyclodextrin, 7.6 mM citrate (pH 3), 4.5 degrees C.


Assuntos
Antagonistas Adrenérgicos alfa/isolamento & purificação , Piperoxano/isolamento & purificação , beta-Ciclodextrinas , Ciclodextrinas , Eletroforese/métodos , Estereoisomerismo
5.
Analyst ; 125(11): 1919-23, 2000 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-11193077

RESUMO

A capillary electrophoretic method for resolving phenolic compounds found in grape seed extracts was developed using a quaternary ammonium salt as the main electrolyte solution. Seven polyphenols were separated and identified. The separation mechanism seems to involve association between quaternary ammonium cations and the polyphenols. Migration times roughly correlate with the size of the known phenols. The role of the alkyl substituents on the quaternary ammonium ions was investigated and is discussed. The method of analysis proposed herein exhibits high reproducibility in terms of migration times for a complex mixture using a single component background electrolyte.


Assuntos
Fenóis/análise , Rosales , Sementes/química , Eletrólitos , Eletroforese Capilar , Extratos Vegetais/química , Compostos de Tetraetilamônio
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