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Anal Bioanal Chem. 2012 Aug;404(3):909-17. doi: 10.1007/s00216-012-6159-4. Epub 2012 Jun 15.

Lab in a syringe: fully automated dispersive liquid-liquid microextraction with integrated spectrophotometric detection.

Analytical and bioanalytical chemistry

Fernando Maya, Burkhard Horstkotte, José Manuel Estela, Víctor Cerdà

Affiliations

  1. Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Palma de Mallorca, Illes Balears, Spain.

PMID: 22699237 DOI: 10.1007/s00216-012-6159-4

Abstract

A new approach for the integration of various analytical steps inside a syringe (Lab in a Syringe) is presented. Fully automated dispersive liquid-liquid microextraction with integrated spectrophotometric detection is carried out in-syringe using a very simple instrumental setup. The lighter-than-water organic droplets released in the extraction step accumulate at the head of the syringe, where two optical fibers are placed on both sides of the syringe, facing each other and enabling the in situ quantification of the extracted compounds. By this, monitoring of the progressively accumulating droplet in the head of the syringe was further possible. In this first report, the developed instrumental setup has been applied to the determination of the dye rhodamine B in water samples and soft drinks. The main parameters influencing the extraction such as the selection of the extractant and disperser solvents, extractant/disperser and organic/water phase ratios, pH of the aqueous phase, extraction flow rates, and extraction time were investigated. Under the selected conditions, rhodamine B was quantified in a working range of 0.023-2 mg L(-1) with a limit of detection of 0.007 mg L(-1). Good repeatability values of up to 3.2% (RSD) were obtained for ten consecutive extractions. The enrichment factor for a 1 mg L(-1) rhodamine B standard was 23, and up to 51 extractions were accomplished in 1 h.

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