Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and 1H NMR Analysis of Chemical Weapons Convention Related Compounds,ACS Applied Materials & Interfaces

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Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and 1H NMR Analysis of Chemical Weapons Convention Related Compounds
ACS Applied Materials & Interfaces ( IF 8.3 ) Pub Date : 2019-04-09 00:00:00 , DOI: 10.1021/acsami.9b02354
Kanchan Sinha Roy ₁ , Raghavender Goud D ₁ , Avik Mazumder ₁ , Buddhadeb Chandra ₁ , Ajay Kumar Purohit ₁ , Meehir Palit ₁ , Devendra Kumar Dubey ₁

Affiliation

The strict monitoring and precise measurements of chemical warfare agents (CWAs) in environmental and other complex samples with high accuracy have great practical significance from the forensic and Chemical Weapons Convention (CWC) verification point of view. Therefore, this study was aimed to develop an efficient extraction and enrichment method for identification and quantification of toxic agents, especially with high sensitivity and multidetection ability in complex samples. It is the first study on solid-phase extraction (SPE) of CWAs and their related compounds from hydrocarbon backgrounds using covalent triazine-based frameworks (CTFs). This nitrogen-rich CTF sorbent has shown an excellent SPE performance toward sample cleanup by selective elimination of hydrocarbon backgrounds and enrich the CWC related analytes in comparison with the conventional and other reported methods. The best enrichment of the analytes was found with the washing solvent (1 mL of n-hexane) and the extraction solvent (1 mL of dichloromethane). Under the optimized conditions, the SPE method had good linearity in the concentration range of 0.050–10.0 μg mL^–1 for organophosphorus esters, 0.040–20.0 μg mL^–1 for nerve agents, and 0.200–20.0 μg mL^–1 for mustards with correlation coefficients (r²) between 0.9867 and 0.9998 for all analytes. Limits of detection (S/N = 3:1) in the SIM mode were found to be in the range of 0.015–0.050 μg mL^–1 for organophosphorus esters, 0.010–0.030 μg mL^–1 for nerve agents, and 0.050–0.100 μg mL^–1 for blister agents. Limits of quantification (S/N = 10:1) were found in the range of 0.050–0.200 μg mL^–1 for organophosphorus esters, 0.040–0.100 μg mL^–1 for nerve agents, and 0.180–0.350 μg mL^–1 for blister agents in the SIM mode. The recoveries of all analytes ranged from 87 to 100% with the relative standard deviations ranging from 1 to 8%. This method was also successfully applied for the sample preparation of ¹H NMR analysis of sulfur and nitrogen mustards in the presence of hydrocarbon backgrounds. Therefore, this SPE method provides the single sample preparation for both NMR and GC–MS analyses.

中文翻译：

基于三嗪的共价有机框架：有效消除有机样品中GC-MS和化学武器常规相关化合物的¹ H NMR分析的烃背景的有希望的吸附剂

从法医和化学武器公约（CWC）验证的角度来看，对环境和其他复杂样品中的化学战剂（CWA）进行严格的监视和精确测量具有重要的现实意义。因此，本研究旨在开发一种有效的提取和富集方法，用于鉴定和定量有毒物质，尤其是对复杂样品具有高灵敏度和多重检测能力。这是首次使用基于共价三嗪的骨架（CTF）从烃类背景中固相萃取CWA及其相关化合物的研究。与常规方法和其他已报道的方法相比，这种富氮的CTF吸附剂通过选择性消除烃类背景并富集与CWC相关的分析物，在样品净化方面表现出出色的SPE性能。使用洗涤溶剂（1 mLÑ己烷）和萃取溶剂（1毫升二氯甲烷中）。在优化的条件下，SPE方法曾在的0.050-10.0浓度范围微克毫升良好的线性^-1有机磷酯，0.040-20.0微克毫升^-1神经剂和0.200-20.0微克毫升^-1用于与相关氮芥所有分析物的系数（r ²）在0.9867至0.9998之间。检测限（小号/ Ñ = 3：1）在SIM模式被发现是在0.015-0.050微克mL范围^-1有机磷酯，0.010-0.030微克毫升^-1为神经毒剂，和0.050-0.100微克mL ^–1用于起泡剂。定量限（小号/ Ñ = 10：1）中的0.050-0.200的范围内被发现微克毫升^-1有机磷酯，0.040-0.100微克毫升^-1为神经毒剂，和0.180-0.350微克毫升^-1泡罩SIM模式下的业务代表。所有分析物的回收率范围为87％至100％，相对标准偏差范围为1％至8％。该方法也成功地用于在烃背景下对硫和氮芥子气进行¹ H NMR分析的样品制备。因此，这种SPE方法可为NMR和GC-MS分析提供单一样品前处理。

更新日期：2019-04-09

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