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J Sep Sci ; 29(13): 1977-87, 2006 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-17017010

RESUMEN

A well established method of direct injection of larger than conventional sample volumes ranging from 0.1 mL to 10 mL in HPLC is the injection valve method in which a loop of tubing is totally or partially filled with sample. Recent HPLC pumps have a flow-rate setting accuracy of +/- 1-2% over a flow-rate range from 0.1 mL/min to 10 mL/min and the flow stability is 0.2% or less. Quarternary low pressure gradient pumps are widely available and used, but all their hydraulic lines are seldom utilised. The idea of using one line of a common commercial HPLC quaternary low-pressure pump for direct on-column injection (pumping) of large sample volumes ranging from 1 mL to 100 mL was tested. This approach was evaluated during practical work on the development of an RP-HPLC method of determination of residual atrazine and hydroxyatrazine. In lysimetric environmental experiments hydroxyatrazine was formed in situ in a soil column by hydrolysis of atrazine. The results proved the applicability of this approach not only in experiments with model mixtures of analytes at microg/L levels in solutions. Analysis of 20 mL of soil leachates and extracts of soil samples containing atrazine and hydroxyatrazine at the 10 microg/kg level (in dry soil) revealed that good figures-of-merit were preserved, even in the presence of a large excess of humic substances.


Asunto(s)
Atrazina/análisis , Cromatografía Líquida de Alta Presión/métodos , Suelo/análisis , Atrazina/análogos & derivados , Atrazina/normas , Cromatografía Líquida de Alta Presión/normas , Herbicidas/análisis , Herbicidas/normas , Concentración de Iones de Hidrógeno , Estándares de Referencia , Contaminantes del Suelo/análisis , Solventes
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