title: A fully automated effervescence assisted dispersive liquid-liquid microextraction based on a stepwise injection system. Determination of antipyrine in saliva samples.
abstract: A first attempt to automate the effervescence assisted dispersive liquid-liquid microextraction (EA-DLLME) has been reported. The method is based on the aspiration of a sample and all required aqueous reagents into the stepwise injection analysis (SWIA) manifold, followed by simultaneous counterflow injection of the extraction solvent (dichloromethane), the mixture of the effervescence agent (0.5 mol L(-1) Na2CO3) and the proton donor solution (1 mol L(-1) CH3COOH). Formation of carbon dioxide microbubbles generated in situ leads to the dispersion of the extraction solvent in the whole aqueous sample and extraction of the analyte into organic phase. Unlike the conventional DLLME, in the case of EA-DLLME, the addition of dispersive solvent, as well as, time consuming centrifugation step for disruption of the cloudy state is avoided. The phase separation was achieved by gentle bubbling of nitrogen stream (2 mL min(-1) during 2 min). The performance of the suggested approach is demonstrated by determination of antipyrine in saliva samples. The procedure is based on the derivatization of antipyrine by nitrite-ion followed by EA-DLLME of 4-nitrosoantipyrine and subsequent UV-Vis detection using SWIA manifold. The absorbance of the yellow-colored extract at the wavelength of 345 nm obeys Beer's law in the range of 1.5-100 µmol L(-1) of antipyrine in saliva. The LOD, calculated from a blank test based on 3σ, was 0.5 µmol L(-1).
authors.affiliation: Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg, Russia.
authors.forename: Kseniia
authors.initials: K
authors.lastname: Medinskaia
authors.affiliation: Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg, Russia.
authors.forename: Christina
authors.initials: C
authors.lastname: Vakh
authors.affiliation: Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg, Russia.
authors.forename: Darina
authors.initials: D
authors.lastname: Aseeva
authors.affiliation: Department of Analytical Chemistry, University of P.J. Šafárik, SK-04154 Košice, Slovakia. Electronic address: vasil.andruch@upjs.sk.
authors.forename: Vasil
authors.initials: V
authors.lastname: Andruch
authors.affiliation: Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg, Russia.
authors.forename: Leonid
authors.initials: L
authors.lastname: Moskvin
authors.affiliation: Department of Analytical Chemistry, Institute of Chemistry, Saint Petersburg State University, RU-198504 Saint Petersburg, Russia. Electronic address: bulatov_andrey@mail.ru.
authors.forename: Andrey
authors.initials: A
authors.lastname: Bulatov
mesh_terms: D000983:Antipyrine / Q000032:analysis*; D001331:Automation; D006801:Humans; D059627:Liquid Phase Microextraction; D012463:Saliva / Q000737:chemistry*; D013056:Spectrophotometry, Ultraviolet
chemical_list: D000983:Antipyrine
keywords: Antipyrine; Automation; Effervescence dispersive liquid–liquid microextraction; Saliva; Stepwise injection analysis