二硝基苯肼测定空气中微量甲醛的柱前衍生高效液相色谱法

Determination of trace formaldehyde in air by DNPH precolumn derivatization high performance liquid chromatography

目的探讨DNPH柱前衍生高效液相色谱法测定空气中微量甲醛的方法。方法采用大型气泡吸收管采样,吸收液在60℃的水浴中衍生20 min,用环己烷提取后于液相色谱仪进行分析定量。结果甲醛在0～8.0μg/ml浓度范围内,标准曲线线性关系良好,相关系数r为0.999 8,相对标准偏差为0.9%～2.6%,加标回收率为96.2%～101.3%,采样效率为92.3%～96.8%。结论该方法不但可以克服酚试剂分光光度法的缺点,还具有选择性好、灵敏度高、干扰少、精密度和准确度好等优点,而且快捷,适合大批量的检测工作。

[ Objective ] To explore DNPH precolumn derivatization high performance liquid chromatography in determination of trace formaldehyde in air. [Methods] A large bubble absorption tube was used, absorption solution was in 60 ℃ water bath 20 min for derivative, then extracted with cyclohexane and quantitatively analyzed in liquid chromatography. [ Results] Within 0-8μ g/ml con- centration range, the standard curve of formaldehyde bad good linear relationship, correlation coefficient r = 0. 999 8 ; relative standard deviation was 0.9%-2.6% ; and the recovery was 96.2%-101.3% ; the sampling efficiency was 92. 3%-96.8%. [ Conclusion] This method can not only overcome the phenol reagent spectrophotometry shortcomings, but also has good selectivity, high sensitivity, less interference, good precision and accuracy etc, and fast, suitable for mass detection.