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液相色谱/串联质谱联用柱前衍生法测定空气中的肼。

Determination of hydrazine in air by liquid chromatography/tandem mass spectrometry combined with precolumn derivatization.

作者信息

Takemine Shusuke, Motegi Mamoru, Takayanagi Manabu, Usui Sunao, Kuroda Ikuma

机构信息

Center for Environmental Science in Saitama, 914 Kamitanadare, Kazo, Saitama, 347-0115, Japan.

Center for Environmental Science in Saitama, 914 Kamitanadare, Kazo, Saitama, 347-0115, Japan.

出版信息

Talanta. 2023 Jun 1;258:124411. doi: 10.1016/j.talanta.2023.124411. Epub 2023 Mar 4.

DOI:10.1016/j.talanta.2023.124411
PMID:36907163
Abstract

In this study, we developed a determination method for hydrazine in the air. Hydrazine was derivatized with p-dimethyl amino benzaldehyde (DBA) to yield p-dimethylaminobenzalazine, which was subjected to liquid chromatography-electrospray tandem mass spectrometry (LC/MS/MS) analysis. The derivative exhibited good sensitivity in the LC/MS/MS analysis, and its instrument detection limit and instrument quantification limit were 0.003 and 0.008 ng/mL, respectively. The air sample was collected using an air sampler equipped with a peristaltic pump at 0.2 L/min for 8 h. We demonstrated that a silica cartridge impregnated with DBA and 1,2-bis(4-pyridyl) ethylene can collect hydrazine in the air stably. The mean recovery rates in outdoor and indoor locations were 97.6% and 92.4%, respectively. Further, the method detection and quantification limits were 0.1 and 0.4 ng/m, respectively. The proposed method does not require any pretreatment and/or concentration step, enabling high-throughput analyses.

摘要

在本研究中,我们开发了一种空气中肼的测定方法。肼用对二甲氨基苯甲醛(DBA)衍生化生成对二甲氨基苯甲酰肼,然后进行液相色谱-电喷雾串联质谱(LC/MS/MS)分析。该衍生物在LC/MS/MS分析中表现出良好的灵敏度,其仪器检测限和仪器定量限分别为0.003和0.008 ng/mL。使用配备蠕动泵的空气采样器以0.2 L/min的流量采集空气样品8小时。我们证明,浸渍有DBA和1,2-双(4-吡啶基)乙烯的硅胶柱可以稳定地收集空气中的肼。室外和室内地点的平均回收率分别为97.6%和92.4%。此外,方法检测限和定量限分别为0.1和0.4 ng/m。所提出的方法不需要任何预处理和/或浓缩步骤,能够进行高通量分析。

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