Zhu Yamei, Cui Qun, Wang Haiyan
College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, China.
Se Pu. 2010 Jan;28(1):59-63. doi: 10.3724/sp.j.1123.2010.00059.
The hydrazones have the absorption in the ultraviolet-visible (UV-vis) spectral region. The hydrazones can be formed by the reaction of aldehyde group and dinitrophenylhydrazine (DNPH) in acidic solution. The determination of glyoxal and glyoxalic acid in aldehyde solution was performed by high performance liquid chromatography (HPLC). The proper derivatization conditions were as follows: the reaction temperature of 70 degrees C, the pH of the system of 1.75; the molar ratio of DNPH to carbonyl of 6, the reaction time of 150 min. The saturated concentration of glyoxal dihydrazone in acetonitrile solution at pH 1.75 and 20 degrees C was 20.2 mg/L. The standard curves for glyoxal and glyoxalic acid both had good linear relations in the ranges of 2 - 20 mg/L and 10 - 100 mg/L, respectively. The glyoxal and glyoxalic acid contents in the solution of oxidation of acetaldehyde to glyoxal by nitric acid were determined by this method, the repeatabilities of analysis results were excellent and the relative error compared to chemical analysis of glyoxal was 1.77%. The spiked recoveries of glyoxal and glyoxalic acid were 99.6% - 103.3% and 98.1% - 102.4%, respectively. The method is simple, accurate and efficient for determining aldehydes and dicarbonyl compounds.
腙类化合物在紫外可见（UV-vis）光谱区域有吸收。腙类化合物可通过醛基与2,4-二硝基苯肼（DNPH）在酸性溶液中反应形成。采用高效液相色谱（HPLC）法测定醛溶液中的乙二醛和乙醛酸。合适的衍生化条件如下：反应温度70℃，体系pH值1.75；DNPH与羰基的摩尔比为6，反应时间150分钟。在pH值1.75、20℃的乙腈溶液中，乙二醛二腙的饱和浓度为20.2mg/L。乙二醛和乙醛酸的标准曲线在2 - 20mg/L和10 - 100mg/L范围内均具有良好的线性关系。采用该方法测定了硝酸将乙醛氧化为乙二醛溶液中的乙二醛和乙醛酸含量，分析结果的重复性良好，与乙二醛化学分析法相比，相对误差为1.77%。乙二醛和乙醛酸的加标回收率分别为99.6% - 103.3%和98.1% - 102.4%。该方法用于测定醛类和二羰基化合物简单、准确且高效。
