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1.
Analyst ; 137(8): 1956-62, 2012 Apr 21.
Artigo em Inglês | MEDLINE | ID: mdl-22398506

RESUMO

Fast capillary electrophoresis (CE) hyphenated to time-of-flight mass spectrometry (TOF-MS) of four organoarsenic species (glycerol oxoarsenosugar, sulfate oxoarsenosugar, arsenobetaine, arsenocholine) are presented using short length CE capillaries under high electric field strengths of up to 1.3 kV cm(-1) with small inner diameter (ID). The separation of arsenosugars by CE is demonstrated for the first time. An aqueous formic acid solution was employed as the background electrolyte (BGE) for the separation. Various acid concentrations were evaluated for their influence on migration times, separation efficiency as well as with regard to controlling the charge of the arsenic species. A 0.1 M formic acid/ammonium formate buffer (pH 2.8) proved to be suitable for the separation of the four species. A non-aqueous BGE was tested as an alternative buffer system for fast speciation analysis. Separation of arsenobetaine and arsenocholine could even be achieved within 10 s by pressure-assisted CE. Application of the optimized method for the analysis of extracts of a seagrass and a Wakame algae sample as well as the brown algae homogenate reference material IAEA-140/TM revealed a clear signal for the glycerol arsenosugar.


Assuntos
Arsênio/análise , Eletroforese Capilar/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Arsênio/classificação , Soluções Tampão , Pressão
2.
Anal Chim Acta ; 657(2): 83-99, 2010 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-20005319

RESUMO

Arsenic-containing carbohydrates, generally termed arsenosugars, have been the subject of increasing analytical interest in arsenic speciation analysis. The present review gives an overview concerning achievements and trends in the field of instrumental analysis of arsenosugars. The typical experimental approaches for sample pre-treatment, extraction, separation and detection are discussed. Current possibilities and limitations of modern instrumental techniques are pointed out.


Assuntos
Arseniatos/química , Monossacarídeos/química , Arseniatos/isolamento & purificação , Arseniatos/toxicidade , Fracionamento Químico/métodos , Cromatografia em Gel/métodos , Cromatografia por Troca Iônica/métodos , Cromatografia de Fase Reversa/métodos , Monitoramento Ambiental , Contaminação de Alimentos/análise , Espectrometria de Massas/métodos , Micro-Ondas , Monossacarídeos/isolamento & purificação , Monossacarídeos/toxicidade
3.
J Forensic Sci ; 51(4): 815-8, 2006 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-16882225

RESUMO

The detection of a mixture of nine explosive compounds, including nitrate esters, nitroaromatics, and a nitramine in less than 140 sec is described. The new method employs a commercially available pulsed-discharge electron capture detector (PDECD) coupled with a microbore capillary gas chromatography (GC) column in a standard GC oven to achieve on-column detection limits between 5 and 72 fg for the nine explosives studied. The PDECD has the benefit that it uses a pulsed plasma to generate the standing electron current instead of a radioactive source. The fast separation time limits on-column degradation of the thermally labile compounds and decreases the peak widths, which results in larger peak intensities and a concomitant improvement in detection limits. The combination of short analysis time and low detection limits make this method a potential candidate for screening large numbers of samples that have been prepared using techniques such as liquid-liquid extraction or solid-phase microextraction.

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