Singh Varoon, Purohit Ajay Kumar, Chinthakindi Sridhar, Goud D Raghavender, Tak Vijay, Pardasani Deepak, Shrivastava Anchal Roy, Dubey Devendra Kumar
Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
Electron Microscopy Division, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
J Chromatogr A. 2016 Feb 19;1434:39-49. doi: 10.1016/j.chroma.2016.01.028. Epub 2016 Jan 15.
Magnetic hydrophilic-lipophilic balance (MHLB) hybrid resin was prepared by precipitation polymerization using N-vinylpyrrolidone (PVP) and divinylbenzene (DVB) as monomers and Fe2O3 nanoparticles as magnetic material. These resins were successfully applied for the extraction of chemical warfare agents (CWAs) and their markers from water samples through magnetic dispersive solid-phase extraction (MDSPE). By varying the ratios of monomers, resin with desired hydrophilic-lipophilic balance was prepared for the extraction of CWAs and related esters of varying polarities. Amongst different composites Fe2O3 nanoparticles coated with 10% PVP+90% DVB exhibited the best recoveries varying between 70.32 and 97.67%. Parameters affecting the extraction efficiencies, such as extraction time, desorption time, nature and volume of desorption solvent, amount of extraction sorbent and the effect of salts on extraction were investigated. Under the optimized conditions, linearity was obtained in the range of 0.5-500 ng mL(-1) with correlation ranging from 0.9911-0.9980. Limits of detection and limits of quantification were 0.5-1.0 and 3.0-5.0 ng mL(-1) respectively with RSDs varying from 4.88-11.32% for markers of CWAs. Finally, the developed MDSPE method was employed for extraction of analytes from water samples of various sources and the OPCW proficiency test samples.
以N-乙烯基吡咯烷酮（PVP）和二乙烯基苯（DVB）为单体，Fe2O3纳米颗粒为磁性材料，通过沉淀聚合法制备了磁性亲水亲脂平衡（MHLB）混合树脂。这些树脂通过磁分散固相萃取（MDSPE）成功应用于从水样中萃取化学战剂（CWA）及其标志物。通过改变单体比例，制备了具有所需亲水亲脂平衡的树脂，用于萃取不同极性的CWA及其相关酯类。在不同的复合材料中，涂覆10%PVP + 90%DVB的Fe2O3纳米颗粒表现出最佳回收率，在70.32%至97.67%之间。研究了影响萃取效率的参数，如萃取时间、解吸时间、解吸溶剂的性质和体积、萃取吸附剂的用量以及盐对萃取的影响。在优化条件下，线性范围为0.5 - 500 ng mL(-1)，相关系数在0.9911 - 0.9980之间。化学战剂标志物的检测限和定量限分别为0.5 - 1.0和3.0 - 5.0 ng mL(-1)，相对标准偏差（RSD）在4.88% - 11.32%之间。最后，所开发的MDSPE方法用于从各种来源的水样和禁止化学武器组织能力验证测试样品中萃取分析物。
