通过液相色谱 - 质谱联用对作为2,4 - 二硝基苯肼衍生物收集后的羰基化合物进行痕量分析。

Trace analysis of carbonyl compounds by liquid chromatography-mass spectrometry after collection as 2,4-dinitrophenylhydrazine derivatives.

作者信息

Sakuragawa A, Yoneno T, Inoue K, Okutani T

机构信息

Department of Industrial Chemistry, College of Science and Technology, Nihon University, Tokyo, Japan.

出版信息

J Chromatogr A. 1999 Jun 4;844(1-2):403-8. doi: 10.1016/s0021-9673(99)00307-6.

DOI:10.1016/s0021-9673(99)00307-6

PMID:10399334

Abstract

This study describes the utilization of carbonyl- 2,4-dinitrophenylhydrazine (DNPH) derivatives for the determination of a micro amount of carbonyl compounds in air by liquid chromatography-mass spectrometry (LC-MS). After the carbonyl compounds are collected using a Waters Sep-Pak C18 cartridge column with-impregnated DNPH on octadecylsilica, they are eluted by acetonitrile as carbonyl-DNPH derivatives. A 20-mm3 aliquot of eluent is injected into the LC-MS system. The four derivatives (formaldehyde-, acetaldehyde-, acrolein- and acetone-DNPH) were eluted within 7 min with acetonitrile-water (60:40, v/v) as the mobile phase. The proposed method offers sub-ppb sensitivity and good reproducibility and was applied to the determination of these carbonyl compounds in actual air samples from store rooms, laboratories and offices. The relative standard deviations for these samples (n = 6) were 1 to 3%.

摘要

本研究描述了利用羰基-2,4-二硝基苯肼（DNPH）衍生物，通过液相色谱-质谱联用（LC-MS）测定空气中微量羰基化合物的方法。使用在十八烷基硅胶上浸渍了DNPH的沃特世Sep-Pak C18柱收集羰基化合物后，它们以羰基-DNPH衍生物的形式用乙腈洗脱。取20立方毫米的洗脱液等分试样注入LC-MS系统。以乙腈-水（60:40，v/v）作为流动相时，四种衍生物（甲醛-DNPH、乙醛-DNPH、丙烯醛-DNPH和丙酮-DNPH）在7分钟内被洗脱。所提出的方法具有亚ppb级的灵敏度和良好的重现性，并应用于测定来自储藏室、实验室和办公室的实际空气样品中的这些羰基化合物。这些样品（n = 6）的相对标准偏差为1%至3%。