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J Chromatogr B Analyt Technol Biomed Life Sci ; 879(28): 3034-40, 2011 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-21925977

RESUMO

The new pre-concentration technique, hollow fiber-solid phase microextraction based on carbon nanotube reinforced sol-gel and liquid chromatography-photodiode array detection was applied to determination of aflatoxins B(1), B(2) (AFB(1), AFB(2)) in rice, peanut and wheat samples. This research provides an overview of trends related to synthesis of solid phase microextraction (SPME) sorbnents that improves the assay of aflatoxins as the semi-polar compounds in several real samples. It mainly includes summary and a list of the results for a simple carbon nanotube reinforced sol-gel in-fiber device. This device was used for extraction, pre-concentration and determination of aflatoxins B1, B2 in real samples. In this technique carbon nanotube reinforced sol was prepared by the sol-gel method via the reaction of phenyl trimethoxysilane (PTMS) with a basic catalyst (tris hydroxymethyl aminomethan). The influences of microextraction parameters such as pH, ageing time, carbon nanotube contents, desorption conditions, desorption solvent and agitation speed were investigated. Optimal HPLC conditions were: C(18) reversed phase column for separation, water-acetonitril-methanol (35:10:55) as the mobile phase and maximum wavelength for detection was 370 nm. The method was evaluated statistically and under optimized conditions, the detection limits for the analytes were 0.074 and 0.061 ng/mL for B1 and B2 respectively. Limit of quantification for B1 and B2 was 0.1 ng/mL too (n=7). The precisions were in the range of 2.829-2.976% (n=3), and linear ranges were within 0.1 and 400 ng/mL. The method was successfully applied to the analysis of cereals (peanut, wheat, rice) with the relative recoveries from 47.43% to 106.83%.


Assuntos
Aflatoxina B1/análise , Aflatoxinas/análise , Cromatografia Líquida de Alta Pressão/métodos , Grão Comestível/química , Nanocompostos/química , Microextração em Fase Sólida/métodos , Adsorção , Aflatoxina B1/isolamento & purificação , Aflatoxinas/isolamento & purificação , Cromatografia Líquida de Alta Pressão/instrumentação , Contaminação de Alimentos/análise , Microextração em Fase Sólida/instrumentação
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