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聚[(2-(甲基丙烯酰氧基)乙基)三甲基氯化铵]薄膜固相萃取法用于神经毒剂降解产物的提取。

Solid-phase extraction of nerve agent degradation products using poly[(2-(methacryloyloxy)ethyl)trimethylammonium chloride] thin films.

机构信息

Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon 34141, South Korea; Chemical and Biological Defense Department, Agency for Defense Development, Daejeon 34186, South Korea.

Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon 34141, South Korea.

出版信息

Talanta. 2019 May 15;197:500-508. doi: 10.1016/j.talanta.2019.01.048. Epub 2019 Jan 14.

Abstract

In this study, a simple solid-phase extraction (SPE) technique was developed to extract organophosphonic acids as degradation products of nerve agents from aqueous samples for identification by instrumental analyses such as FT-IR, TOF-SIMs and GC-MS. To selectively extract the organophosphonic acids, we synthesized an anion exchange polymer film on a gold plate using surface-initiated controlled radical polymerization with 2-[(methacryloyloxy)ethyl]trimethylammonium chloride. Extraction of the organophosphonic acids onto the plates was successfully confirmed by polarized angle fourier transformation-infra red (FT-IR) spectroscopy, X-ray photoelectron spectroscopy, and time-of-flight secondary ion mass spectrometry analyses. The limit of detection of the developed SPE method satisfied the detection limit of Chemical Warfare Agents verification criteria by FT-IR analysis. After optimization, the detection limit values were found to be between 0.1 and 0.4 µg mL, and the recovery ranged from 50% to 110% in aqueous solution containing various interference. In addition, the SPE process was successfully applied to the detection of pinacolyl methylphosphonic acid, the degradation product of soman, in the 35th Organization for Prohibition of Chemical Weapons proficiency test sample.

摘要

在这项研究中,开发了一种简单的固相萃取 (SPE) 技术,用于从水样中提取有机膦酸作为神经毒剂的降解产物,以便通过 FT-IR、TOF-SIMS 和 GC-MS 等仪器分析进行鉴定。为了选择性地提取有机膦酸,我们使用表面引发可控自由基聚合,在金盘上合成了一种阴离子交换聚合物膜,使用 2-[(甲基丙烯酰氧基)乙基]三甲基氯化铵。通过偏光角傅里叶变换红外 (FT-IR) 光谱、X 射线光电子能谱和飞行时间二次离子质谱分析,成功证实了有机膦酸在板上的萃取。开发的 SPE 方法的检测限满足 FT-IR 分析的化学战剂验证标准的检测限。经过优化,检测限值在 0.1 至 0.4 µg mL 之间,在含有各种干扰物的水溶液中的回收率在 50%至 110%之间。此外,SPE 过程成功应用于 soman 降解产物甲基膦酸频那醇酯在第 35 次禁止化学武器组织能力测试样品中的检测。

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