2,4-二硝基苯肼柱前衍生-高效液相色谱法测定水中的微量乙醛

Determination of trace acetaldehyde in water by 2,4-dinitrophenylhydrazine pre-column derivation-high performance liquid chromatography

中文关键词:  2,4-二硝基苯肼  水  乙醛  衍生化  高效液相色谱法

英文关键词:2,4-dinitrophenylhydrazine  water  acetaldehyde  pre-column derivatization  high performance liquid chromatography

中文摘要:

      目的 探讨2,4-二硝基苯肼(2,4-dinitrophenylhydrazine, DNPH)柱前衍生高效液相色谱法测定水中微量乙醛的方法。方法 将样品在60 ℃水浴中用DNPH衍生化20 min, 由正己烷萃取, 以乙腈: 水(52: 48, V:V)为流动相, 于365 nm波长下进行测定。结果 乙醛在0.015~1.00 mg/L浓度范围内线性关系良好, 相关系数r为0.9999, 加标回收率为80.2%~99.8%, 相对标准偏差为4.6%~7.4%, 方法最低检出浓度为0.003 mg/L。结论 该方法样品前处理简单快捷、检出限低、灵敏度高, 能够满足生活饮用水卫生规范的要求, 并且能够同时测定大批量样品, 为解决国家标准中检测方法最低检出限与其乙醛的限值相矛盾的问题提供参考。

英文摘要:

      Objectives To investigate the determination of acetaldehyde in water by 2,4-dinitrophenylhydrazine (DNPH) pre-column derivation-high performance liquid chromatography. Methods The samples were derivated with DNPH for 20 min in a 60 ℃ water bath, extracted with n-hexane, and determined at a wavelength of 365 nm using acetonitrile: water (52:48, V:V) as mobile phase. Results The acetaldehyde had good linear relationships in the range of 0.015?1.00 mg/L, and the correlation coefficients were 0.9999. The limit of detection was 0.003 mg/L. The recoveries were 80.2%?99.8%, with the relative standard deviations of 4.6%?7.4%. Conclusion The method has the advantages of simple and rapid sample preparation, low detection limit and high sensitivity, which can meet the requirements of sanitary specifications for drinking water, and can simultaneously detect large batch samples, so as to provide a reference for solving the problem of the contradiction between the minimum detection limit of national standard and the limit of acetaldehyde.