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Optimization of a solid‐phase microextraction procedure for the determination of herbicides by micellar electrokinetic chromatography
Author(s) -
FríasGarcía Sergio,
Sánchez M. J.,
RodríguezDelgado Miguel Á.
Publication year - 2004
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200401768
Subject(s) - solid phase microextraction , micellar electrokinetic chromatography , chromatography , extraction (chemistry) , chemistry , desorption , detection limit , sample preparation , solid phase extraction , electrokinetic phenomena , analytical chemistry (journal) , adsorption , mass spectrometry , gas chromatography–mass spectrometry , organic chemistry
The use of a different optimization procedure that involves Experimental Design (ED) and Artificial Neural Networks (ANN) for the off ‐line coupling solid‐phase microextraction‐micellar electokinetic chomatography (SPME‐MEKC) is presented. This combination of ED and ANN, mathematical tools not previously used in SPME‐MEKC optimization, allowed us to obtain good extraction efficiencies in the SPME procedure for the determination of a group of eleven triazine herbicides in groundwater samples. Both extraction and desorption steps were carried out by solution stirring at 900 rpm. Optimal conditions for the off ‐line SPME procedure were: extraction with a poly(dimethylsiloxane)/divinylbenzene SPME fiber for 120 min, 10% ( w/v ) NaCl, desorption time 40 min, and 70% ( v/v ) of methanol/buffer as desorption mixture. Detection limits lay between 0.80 μg L –1 and 4.89 μg L –1 . Finally, the optimized method was applied to the determination of these compounds in spiked and non‐spiked groundwater samples using a previously optimized MEKC separation.

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