Sanches Filho Pedro José, Rios Angel, Valcarcel Miguel, Melecchi Maria Inês Soares, Caramão Elina Bastos
Instituto de Química, UFRGS, Porto Alegre, RS, Av. Bento Gonçalves 9500, 90160-970 Porto Alegre, RS, Brazil.
J Agric Food Chem. 2007 Feb 7;55(3):603-7. doi: 10.1021/jf062382j.
In this paper, the use of supercritical fluid extraction (SFE) and micellar electrokinetic capillary chromatography (MEKC) is proposed for the complete analysis of volatile nitrosamines in sausages. The extraction fluid used was CO2 and variables such as density, temperature of thimbles, extraction time, modifier, fluid flow, and kind of traps were investigated. Several experiments were carried out to obtain the most favorable conditions for analysis of volatile nitrosamines in sausages. The recoveries ranged from 21 to 82% for the five nitrosamines studied. The optimal condition of extraction was 0.2 g of sample fortified with 10 mg/kg, using dynamic extraction during 20 min and with adsorbent Florisil in the trap. The solvent selected for the elution of the analytes was methanol.
本文提出采用超临界流体萃取(SFE)和胶束电动毛细管色谱法(MEKC)对香肠中的挥发性亚硝胺进行全面分析。所用萃取流体为二氧化碳,并研究了诸如密度、萃取管温度、萃取时间、改性剂、流体流速和捕集阱种类等变量。进行了多项实验以获得分析香肠中挥发性亚硝胺的最有利条件。在所研究的五种亚硝胺中,回收率在21%至82%之间。萃取的最佳条件是0.2 g添加了10 mg/kg的样品,采用动态萃取20分钟,并在捕集阱中使用吸附剂弗罗里硅土。选择用于洗脱分析物的溶剂为甲醇。