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2017-04-11 发布于江苏
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FI manifolds for liquid–liquid extraction without phase separation assisted by ultrasound.pdf

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FI manifolds for liquid–liquid extraction without phase separation assisted by ultrasound

Analytica Chimica Acta 489 (2003) 1–11 Flow injection manifolds for liquid–liquid extraction without phase separation assisted by ultrasound J. Ruiz-Jiménez, M.D. Luque de Castro ? Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, Annex Marie Curie Building, E-14071 Córdoba, Spain Received 7 February 2003; received in revised form 22 May 2003; accepted 3 June 2003 Abstract Flow injection (FI) manifolds based on iterative change of the flow direction have been designed to study the influence of auxiliary energy on continuous liquid–liquid extraction without phase separation and compare it with the non-assisted process in a single experiment. In order to demonstrate the utility of ultrasounds as auxiliary energy for the extraction of polyphenols from an organic phase, the approach has been applied to samples of extra virgin olive oil, using an alkaline aqueous phase as extractant and subsequent derivatization with the Folin–Ciocalteu reagent. The proposed method provides results similar to those from the official method-recoveries between 97 and 100%. The sensitivity of the proposed method is 3.5 times higher than that of the non-ultrasound-assisted method. The precision, expressed as relative standard deviation (R.S.D.) for n = 5, was within 1–5% and the relative errors for the irradiated and non-irradiated method were within 3 and 5%, respectively. The repeatability and within-laboratory reproducibility, studied at two concentration levels (379 and 813 g ml?1) ranged between 0.7–4.4% and 0.6–4.8%, respectively. The proposed manifolds can also be applied to either other type of auxiliary energies—microwave, thermal—or two different types of auxiliary energies at the same time. ? 2003 Elsevier B.V. All rights reserved. Keywords: Flow injection; Liquid–liquid extraction; Ultrasound assisted 1. Introduction The use of auxiliary energies for assisting sample preparation is one of the strongest trends in analytical chemistry nowadays [1]. Th