Simultaneous Determination of C<sub>1</sub>−C<sub>4</sub> Carboxylic Acids and Aldehydes Using 2,4-Dinitrophenylhydrazine-Impregnated Silica Gel and High-Performance Liquid Chromatography
作者:Shigehisa Uchiyama、Erika Matsushima、Shohei Aoyagi、Masanori Ando
DOI:10.1021/ac0493471
日期:2004.10.1
4-dinitrophenylhydrazides exhibited maximum absorption wavelengths of 331-334 nm and molar absorption coefficients of 1.4 x 10(4) L/mol/cm. They were completely separated by high-performance liquid chromatography (HPLC) with an RP-Amide C16 column. Cartridges packed with DNPH-coated silica particles (DNPH cartridge) were used for sampling formic acid and aldehydes. Formic acid was physically adsorbed on
描述了一种同时测定空气中脂肪族羧酸和醛类的新方法。在这项工作中,使羧酸与2,4-二硝基苯肼(DNPH)反应形成相应的羧基2,4-二硝基苯肼。这些衍生物具有出色的热稳定性,其熔点比相应的高32-50摄氏度。C1-C4羧酸2,4-二硝基苯酰肼的最大吸收波长为331-334 nm,摩尔吸收系数为1.4 x 10(4)L / mol / cm。使用RP-Amide C16色谱柱的高效液相色谱(HPLC)将它们完全分离。使用装有DNPH涂层的二氧化硅颗粒的小柱(DNPH小柱)对甲酸和醛进行采样。作为采样机制的第一步,甲酸物理吸附在二氧化硅颗粒上。随后与DNPH逐渐反应。甲酸在室温(20摄氏度)下与DNPH反应非常缓慢,但在80摄氏度下历时4小时完全反应。在现场测量中,通过DNPH滤芯吸入样品空气。取样后,将小柱在80摄氏度下加热5小时,然后用乙腈萃取进行HPLC分析。在这些优化条件下,对于以100 mL