CAJ | 학술논문

利用醛基与2,4-二硝基苯肼(DNPH)反应得到的腙产物对紫外-可见光有吸收的特性,采用高效液相色谱法(HPLC)测定乙醛溶液中乙二醛和乙醛酸的含量.结果表明,DNPH衍生乙二醛成腙反应的适宜条件为:反应温度70 ℃, pH 1.75, DNPH与羰基的物质的量比为6,反应时间150 min.在20 ℃、pH 1.75的乙腈溶液中,乙二醛二腙的溶解度为20.2 mg/L.乙二醛质量浓度在2～20 mg/L 范围内,乙二醛二腙的峰面积与乙二醛的质量浓度之间呈良好的线性关系;乙醛酸质量浓度在10～100 mg/L 范围内,乙醛酸腙的峰面积与乙醛酸的质量浓度之间呈良好的线性关系.用HPLC测定乙醛硝酸氧化法制乙二醛反应液中乙二醛和乙醛酸的含量,结果的重复性好;对乙二醛的测定结果与应用化学分析法测定结果的平均相对误差为1.77% ;对反应液中乙二醛、乙醛酸含量的测定有着较高的加标回收率,分别为99.6% ～103.3%和98.1% ～102.4% .所建立的方法为醛及二羰基化合物的测定提供了准确、便捷的方法.
이용철기여2,4-이초기분정(DNPH)반응득도적종산물대자외-가견광유흡수적특성,채용고효액상색보법(HPLC)측정을철용액중을이철화을철산적함량.결과표명,DNPH연생을이철성종반응적괄의조건위:반응온도70 ℃, pH 1.75, DNPH여탄기적물질적량비위6,반응시간150 min.재20 ℃、pH 1.75적을정용액중,을이철이종적용해도위20.2 mg/L.을이철질량농도재2～20 mg/L 범위내,을이철이종적봉면적여을이철적질량농도지간정량호적선성관계;을철산질량농도재10～100 mg/L 범위내,을철산종적봉면적여을철산적질량농도지간정량호적선성관계.용HPLC측정을철초산양화법제을이철반응액중을이철화을철산적함량,결과적중복성호;대을이철적측정결과여응용화학분석법측정결과적평균상대오차위1.77% ;대반응액중을이철、을철산함량적측정유착교고적가표회수솔,분별위99.6% ～103.3%화98.1% ～102.4% .소건립적방법위철급이탄기화합물적측정제공료준학、편첩적방법.
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 ℃, 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 ℃ 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.