Laboratorio de Espectroscopía Atómica, Departamento de Química, Universidad Simón Bolívar, Caracas 1080A, Venezuela.
Anal Chim Acta. 2011 Feb 14;687(1):50-5. doi: 10.1016/j.aca.2010.12.006. Epub 2010 Dec 11.
A new miniaturized methodology based on the combination of headspace single drop microextraction and microvolume fluorospectrometry is proposed in this work for the determination of free and hydrolyzed formaldehyde in textile samples. The proposed method is based on the extraction and in-drop derivatization of free and hydrolyzed formaldehyde using the Hantzsch reaction. The effect of experimental variables affecting the performance of the proposed method, such as fluorescence parameters, nature of the extractant phase composition (including acetylacetone concentration, pH, ammonium acetate concentration and presence of an organic solvent), sample temperature, NaCl concentration and microextraction time was carefully investigated. Under optimized conditions, instrumental detection and quantification limits were 26 and 87 μg L(-1), respectively, whereas procedural detection and quantification limits were 1.0 and 3.5 mg kg(-1), respectively. Repeatability, expressed as relative standard deviation, was 4.6% (n=9). The method was successfully applied to the determination of free and hydrolyzed formaldehyde in several textile samples, the found results being in good agreement with those obtained with the EN ISO 14184-1:1998 method.
本工作提出了一种基于顶空单滴微萃取和微量荧光光谱法结合的新的微型化方法，用于测定纺织样品中的游离和水解甲醛。该方法基于 Hantzsch 反应，使用乙酰丙酮对游离和水解甲醛进行萃取和衍生化。仔细研究了影响所提出方法性能的实验变量，如荧光参数、萃取相组成的性质（包括乙酰丙酮浓度、pH 值、乙酸铵浓度和有机溶剂的存在）、样品温度、NaCl 浓度和微萃取时间。在优化条件下，仪器检测限和定量限分别为 26 和 87μg L(-1)，而程序检测限和定量限分别为 1.0 和 3.5mg kg(-1)。重复性（以相对标准偏差表示）为 4.6%（n=9）。该方法成功应用于几种纺织样品中游离和水解甲醛的测定，所得结果与 EN ISO 14184-1:1998 方法的结果吻合良好。
