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用于从水样中分散固相萃取化学战剂的氧化铁功能化石墨烯纳米复合材料

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

作者信息

Chinthakindi Sridhar, Purohit Ajay, Singh Varoon, Tak Vijay, Goud D Raghavender, Dubey D K, Pardasani Deepak

机构信息

Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior -474002, India.

Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior -474002, India.

出版信息

J Chromatogr A. 2015 May 15;1394:9-17. doi: 10.1016/j.chroma.2015.03.033. Epub 2015 Mar 23.

Abstract

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals.

摘要

本研究涉及基于石墨烯的磁性纳米复合材料的制备与评估,用于从水样中分散固相萃取与《化学武器公约》(CWC)相关的化学品。通过将二氧化硅包覆的Fe3O4共价键合到石墨烯片上,合成了纳米复合材料Fe3O4@SiO2-G。神经毒剂(NA)、硫芥(SM)及其无毒环境标志物为目标分析物。对吸附剂用量、萃取时间和解吸条件等萃取参数进行了优化。将20毫克吸附剂分散在200毫升水样中20分钟,然后用甲醇/氯仿萃取,目标分析物的回收率平均至良好(27 - 94%)。实际毒剂的回收率对样品pH值和离子强度有很大依赖性。沙林在弱酸性条件下回收率最高(pH 5时为56%),而VX需要碱性介质(pH 9时为83%)。发现水样中盐的存在是有利的,硫芥的回收率提高到高达94%。硫芥和VX的出色检测限(分别为0.11 ngmL(-1)和0.19 ngmL(-1))证明了所开发方法用于对与《化学武器公约》相关化学品进行现场外分析的实用性。

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