de Oliveira Fabio Santos, Sousa Eliane Teixeira, de Andrade Jailson B
Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, 40170-290 Salvador, BA, Brazil.
Talanta. 2007 Sep 30;73(3):561-6. doi: 10.1016/j.talanta.2007.04.027. Epub 2007 May 4.
A sensitive FIA method was developed for the selective determination of formaldehyde in alcoholic beverages. This method is based on the reaction of Fluoral-P (4-amine-3-pentene-2-one) with formaldehyde, leading to the formation of 3,5-diacetyl-1,4-dihydrolutidine (DDL), which fluoresces at lambda(ex)=410nm and lambda(em)=510nm. The analytical parameters were optimized by the response surface method using the Box-Behnken design. The proposed flow injection system allowed for the determination of up to 3.33x10(-5)molL(-1) of formaldehyde with R.S.D.<2.5% and a detection limit of 3.1ngmL(-1). The method was successfully applied to determine formaldehyde in alcoholic beverages, without requiring any sample pretreatment, and the results agreed with the reference at a 95% confidence level by paired t-test. In the optimized condition, the FIA system proved able to analyze up to 60 samples/h.
开发了一种灵敏的流动注射分析法(FIA)用于选择性测定酒精饮料中的甲醛。该方法基于氟代乙酰丙酮(4-氨基-3-戊烯-2-酮)与甲醛的反应,生成3,5-二乙酰基-1,4-二氢卢剔啶(DDL),其在激发波长(λex)=410nm和发射波长(λem)=510nm处发荧光。采用Box-Behnken设计的响应面法对分析参数进行了优化。所提出的流动注射系统能够测定高达3.33×10⁻⁵mol·L⁻¹的甲醛,相对标准偏差(R.S.D.)<2.5%,检测限为3.1ng·mL⁻¹。该方法成功应用于酒精饮料中甲醛的测定,无需任何样品预处理,通过配对t检验,结果在95%置信水平下与参考值一致。在优化条件下,流动注射分析系统能够每小时分析多达60个样品。