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Use of moleculary imprinted polymers (MIP) for extraction and pre-concentration of orgnic analytes in biological samples and spectrophotometric determination

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Author(s):
Eduardo Costa de Figueiredo
Total Authors: 1
Document type: Doctoral Thesis
Press: Campinas, SP.
Institution: Universidade Estadual de Campinas (UNICAMP). Instituto de Química
Defense date:
Examining board members:
Marco Aurelio Zezzi Arruda; Pedro Orival Luccas; Ricardo Erthal Santelli; Anne Hélène Fostier; Dosil Pereira de Jesus
Advisor: Marco Aurelio Zezzi Arruda
Abstract

The objective of this Thesis was the association between molecularly imprinted polymers and spectrophotometry, with the selectivity obtained through specific binding between analytes and imprinted binding sites of the polymer. In the Chapter 1, a selective MIP for catechol was synthesized, characterized, and employed for the extraction of catechol from guarana (Paullinia cupana) and mate (Ilex paraguariensis) samples, followed by indirect spectophotometric determination of catecol by reduction of Mn(VII) for Mn(II). A limit of quantification, a relative standard deviation (20 mmol L, n = 10) and an analytical frequency of 2.7 mmol L, <5% and 15h, were obtained, respectively. Accuracy was validated using HPLC. In the Chapter 2, a MIP for nicotine was used for its extraction in urine samples of smokers, followed by its indirect quantification by spectrophotometry (reduction of Mn(VII) to Mn(VI) by nicotine). The limit of quantification and analytic frequency were of 1.1 mmol L and 11 h, respectively. Intra (10, 13 and 4%) and inter-day (12, 10 and 5%) precisions were obtained using 3, 10 and 30 mmol L nicotine standard solutions, respectively, and accuracy was validated through HPLC. Finally, in the Chapter 3, a MIP was employed for phenothiazinics (chlorpromazine and perphenazine) extraction in urine samples. Soon after, the drugs were eluted and separated using a low pressure and high-speed system, comprising a C18 column with particle size between 35 and 50 mm. The quantification limits were 5 mmol L for chlorpromazine and perphenazine, and the accuracy was validated using HPLC (AU)