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采用巯基棉和 2,4-二硝基苯肼固相萃取柱净化-高效液相色谱法测定尿中丙烯醛。

Determination of acrolein and other carbonyls in cigarette smoke using coupled silica cartridges impregnated with hydroquinone and 2,4-dinitrophenylhydrazine.

机构信息

Department of Environmental Health, National Institute of Public Health, Wako City, Saitama 351-0197, Japan.

出版信息

J Chromatogr A. 2010 Jun 25;1217(26):4383-8. doi: 10.1016/j.chroma.2010.04.056. Epub 2010 Apr 27.

Abstract

A new method for the determination of acrolein and other carbonyls in cigarette smoke using a dual cartridge system has been developed. Each cartridge consists of reagent-impregnated silica particles. The first contains hydroquinone (HQ) for the inhibition of acrolein polymerization, while the second contains 2,4-dinitrophenylhydrazine (DNPH) for the derivatization of carbonyls. Smoke samples were firstly drawn through the cartridge containing HQ-impregnated silica (HQ-silica) and then through the DNPH-impregnated silica (DNPH-silica). Acrolein in the sample was completely trapped in the first HQ-silica cartridge. Some other airborne carbonyls were also trapped by the HQ-silica, and those that pass through were trapped in the second DNPH-silica cartridge. Extraction was performed in the reverse direction to air sampling. When solvent was eluted through the dual-cartridges, excess DNPH was washed into the HQ bed where it reacted with acrolein and other trapped carbonyls to form the corresponding hydrazone derivatives. All of the hydrazones derived from airborne carbonyls were completely separated and measured using high-performance liquid chromatography. This HQ-DNPH-method can be applied for the determination of acrolein and other alpha,beta-unsaturated aldehydes, such as crotonaldehyde, in cigarette smoke.

摘要

已开发出一种使用双筒系统测定香烟烟雾中丙烯醛和其他羰基化合物的新方法。每个试剂盒由试剂浸渍的硅胶颗粒组成。第一个包含对苯二酚 (HQ) 以抑制丙烯醛聚合,而第二个包含 2,4-二硝基苯肼 (DNPH) 以衍生羰基化合物。烟雾样品首先通过含有 HQ 浸渍硅胶 (HQ-silica) 的试剂盒,然后通过含有 DNPH 浸渍硅胶 (DNPH-silica) 的试剂盒进行抽取。样品中的丙烯醛完全被第一个 HQ-silica 试剂盒捕获。HQ-silica 还捕获了一些其他空气传播的羰基化合物,而那些通过的则被第二个 DNPH-silica 试剂盒捕获。提取是在与空气采样相反的方向进行的。当溶剂通过双筒洗脱时,过量的 DNPH 被冲入 HQ 床中,在那里它与丙烯醛和其他捕获的羰基化合物反应,形成相应的腙衍生物。所有源自空气传播的羰基化合物的腙衍生物都使用高效液相色谱法完全分离和测量。这种 HQ-DNPH 方法可用于测定香烟烟雾中的丙烯醛和其他α,β-不饱和醛,如巴豆醛。

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