Department of Chemistry and Biotechnology, Tallinn University of Technology, Tallinn, Estonia.
Department of Chemistry and Biotechnology, Tallinn University of Technology, Tallinn, Estonia.
Chemosphere. 2018 May;198:460-468. doi: 10.1016/j.chemosphere.2018.01.157. Epub 2018 Feb 6.
In this study, SPE method using a carbon aerogel(CA)-based sorbent was developed and evaluated for the simultaneous extraction of sulfur mustard (HD) degradation products from environmental water samples. Applied CAs proved to be very promising materials for use as SPE sorbents, due to their high porosity, very low density and a large specific surface area. 10 degradation products of HD, both aliphatic and cyclic (thiodiglycol (TDG), TDG sulfoxide, TDG sulfone, 3,5-dithia-1,7-heptanediol, 3,6-dithia-1,8-octanediol, 1,4-thioxane, 1,3-dithiolane, 1,4-dithiane, 1,2,5-trithiepane, and 1,4,5-oxadithiepane) were extracted on a CA-based SPE cartridge. The concentrations of target analytes in the eluate were determined by HPLC-DAD and CE-DAD. Several parameters affecting the extraction efficiency, including the kind and volume of the eluting solvent, sample loading flow rate, volume and ionic strength as well as the reusability of the cartridge, were investigated and optimized to achieve the best performance for the analytes. A series of quantitative parameters such as linear range, coefficient of determination, LOD, LOQ and precision were examined under the optimized conditions. High sensitivity (LODs 0.17-0.50 μM) and high precision (intraday RSD = 2.0-7.7% and interday RSD = 2.7-9.9%) for all the analytes were achieved. The performance of the CA-based sorbent was compared with that of commonly used SPE sorbents. Applied for the analysis of spiked pore water samples collected from the Bornholm Basin, one of the largest chemical warfare dumping sites in the Baltic Sea, the proposed method allowed high SPE recoveries of all the analytes ranging from 83.5 to 99.7% to be obtained.
在这项研究中，开发并评估了一种基于碳气凝胶（CA）的固相萃取（SPE）方法，用于同时从环境水样中萃取硫芥（HD）降解产物。应用 CA 被证明是非常有前途的 SPE 吸附剂材料，因为它们具有高孔隙率、非常低的密度和大的比表面积。10 种 HD 的降解产物，包括脂族和环状的（硫代二甘醇（TDG）、TDG 亚砜、TDG 砜、3,5-二硫-1,7-庚二醇、3,6-二硫-1,8-辛二醇、1,4-噻烷、1,3-二硫杂环戊烷、1,4-二硫杂环戊烷、1,2,5-三噻戊烷和 1,4,5-氧杂二噻戊烷）被吸附在基于 CA 的 SPE 小柱上。洗脱液中目标分析物的浓度通过高效液相色谱-二极管阵列检测（HPLC-DAD）和毛细管电泳-二极管阵列检测（CE-DAD）进行测定。研究并优化了影响萃取效率的多个参数，包括洗脱溶剂的种类和体积、样品加载流速、体积和离子强度以及小柱的可重复使用性，以实现对分析物的最佳性能。在优化条件下，考察了一系列定量参数，如线性范围、相关系数、LOD、LOQ 和精密度。所有分析物均具有较高的灵敏度（LOD 为 0.17-0.50 μM）和较高的精密度（日内 RSD 为 2.0-7.7%，日间 RSD 为 2.7-9.9%）。与常用的 SPE 吸附剂相比，CA 基吸附剂的性能也得到了比较。将该方法应用于分析从波罗的海最大的化学战剂倾倒场之一的博恩霍尔姆湾采集的加标孔隙水样，该方法可以实现所有分析物的高 SPE 回收率（83.5%至 99.7%）。
