Determination of piceid by photochemically induced fluorescence and second-derivative: response surface methodology for the optimization of a liquid-liquid extraction procedure for its analysis in wine samples.
trans-Piceid itself is weakly fluorescent, but the fluorescence signal (lambda(exc/em)=260/361nm) is greatly enhanced by UV-irradiation of its hydroethanolic solutions. Employing the photoinduced emission signal at 361nm or the amplitude of the second-derivative-photoinduced emission spectrum, between 353 and 361nm, a linear relation is found in the assayed range 5.7-31.4ngmL(-1) of trans-piceid and limits of detection of 1.7 and 2.1ngmL(-1), respectively, are obtained. A previous liquid-liquid extraction is necessary for the determination of piceid in wine. Experimental design (Central Composite Design) together with the Response Surface Methodology have been used to find optimum conditions for the extraction procedure. For this purpose, the difference between the photoinduced-fluorescence signal (lambda(exc/em)=260/361nm) of the aqueous phase, before and after being extracted, has been considered as Response Function. A tartrate buffer (pH 5.0) concentration of 0.15molL(-1) and a phase ratio of 1 are determined as optimum conditions. The amplitude of the second-derivative-emission spectrum, corresponding to the evaporated and re-dissolved organic phase, between 353 and 361nm has been employed as analytical signal. Standard addition method has been applied to the analysis of piceid in different wine samples under optimum conditions. Results of wine analysis have been satisfactorily validated by HPLC.
Merás
Isabel Durán
ID
Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz, Spain. iduran@unex.es
Díaz
Teresa Galeano
TG
Rodríguez
Diego Airado
DA
D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D010777:Photochemistry; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet; D014920:Wine / Q000032:analysis*