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全氟羧酸与溴甲基芳香族化合物的酯化反应用于气相色谱-激光电离质谱联用分析。

Esterification of perfluorinated carboxylic acids with bromomethyl aromatic compounds for gas chromatography combined with laser ionization mass spectrometry.

机构信息

Department of Environmental Design, Faculty of Design, Kyushu University, 4-9-1, Shiobaru, Minami-ku, Fukuoka 815-8540, Japan: 744 Motooka, Nishi-ku, Fukuoka 819-0395, Japan.

Department of Environmental Design, Faculty of Design, Kyushu University, 4-9-1, Shiobaru, Minami-ku, Fukuoka 815-8540, Japan: 744 Motooka, Nishi-ku, Fukuoka 819-0395, Japan; Present address: Yanshan University, Qinhuangdao, Hebei 066004, China.

出版信息

J Chromatogr A. 2021 Oct 25;1656:462546. doi: 10.1016/j.chroma.2021.462546. Epub 2021 Sep 10.

DOI:10.1016/j.chroma.2021.462546
PMID:34547552
Abstract

Perfluorinated carboxylic acids (PFCAs) were derivatized with two types of aromatic compounds that contained a bromomethyl group, i.e., 2-(bromomethyl)naphthalene (BMN) and benzyl bromide (BB). The conditions for derivatization were optimized in terms of reaction temperature and time and the concentration of derivatizing reagent. Using these optimal conditions, the PFCAs-MN and PFCAs-B derivatives were measured by gas chromatography (GC) combined with mass spectrometry using an ultraviolet femtosecond laser (267 nm) as the ionization source. The efficiency of derivatization for PFCAs-B was higher than that for PFCAs-MN because of the smaller size of the chromophore (benzene). The ionization efficiency of PFCAs-MN, however, was better than PFCAs-B, since a larger sized chromophore (naphthalene) and then a larger molar absorptivity was preferable for resonance-enhanced two-photon ionization. Due to superior GC separation, BB was successfully used as the derivatizing agent for the trace analysis of PFCAs, with detection limits of 6.0, 8.4, and 9.5 ng/mL for perfluoroheptanoic, perfluorooctanoic, and perfluorononanoic acids, respectively. The other bromomethyl aromatic compounds were evaluated for use as a derivatization reagent in future studies.

摘要

全氟羧酸(PFCAs)与两种含溴甲基的芳香族化合物进行了衍生化反应,即 2-(溴甲基)萘(BMN)和溴化苄(BB)。从反应温度、时间和衍生化试剂浓度等方面对衍生化条件进行了优化。在最佳条件下,采用气相色谱(GC)结合紫外飞秒激光(267nm)作为电离源的质谱法(MS)对 PFCAs-MN 和 PFCAs-B 衍生物进行了测量。由于生色团(苯)较小,PFCAs-B 的衍生化效率高于 PFCAs-MN。然而,PFCAs-MN 的离子化效率优于 PFCAs-B,因为较大的生色团(萘)和较大的摩尔吸光率有利于共振增强双光子电离。由于出色的 GC 分离性能,BB 成功用作痕量分析 PFCAs 的衍生化试剂,对于全氟庚酸、全氟辛酸和全氟壬酸,检测限分别为 6.0、8.4 和 9.5ng/mL。其他溴甲基芳香族化合物也被评估为未来研究中的衍生化试剂。

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