Department of Applied Chemistry and Life Science, Toyohashi University of Technology, Toyohashi 441-8580, Japan.
Department of Applied Chemistry, University of Yamanashi, Kofu 400-8511, Japan.
J Chromatogr A. 2020 Feb 22;1613:460694. doi: 10.1016/j.chroma.2019.460694. Epub 2019 Nov 9.
A novel miniaturized sample preparation device with braid-type extraction medium was successfully developed. Introducing a set of bundles of fine synthetic filaments as the materials of the braid-type extraction medium and also the application of an appropriate tension during the braiding process, the outer diameter of the resulting braid has been controlled. Optimization of the tension enables an easy preparation of a group of braids that can be well-compatible to various internal diameters of capillaries to be packed. The extraction conditions were systematically optimized, and the efficient extraction was confirmed under the optimized conditions. All the parameters affects the desorption efficiency were also optimized, where typical extraction efficiency was more than 90% for the extraction of phenanthrene (1.0 μg/mL) in water. The extracted analyte was desorbed sufficiently by employing a sequential pumping process of two organic solvents. During the preparation of the braid, a different type of fibrous materials could be inserted to the opening at the center of the braid. Taking advantage of this feature of the braid, a stainless steel wire was inserted into the center of the braid. By applying low voltages to the stainless steel wire, a heat-assisted desorption of the extracted analyte was also studied. Experimentally complete desorption (higher than 99.0%) was obtained with the voltage application of 2 V. The lowest limit of quantification (LOQ) and the lowest limit of detection (LOD) for phenanthrene were 0.048 and 0.014 μg/mL, respectively.
成功开发了一种带有编织型萃取介质的新型微型样品制备装置。引入了一组细合成纤维束作为编织型萃取介质的材料，并在编织过程中施加适当的张力，从而控制了编织后得到的编织物的外径。通过优化张力，可以轻松制备一组与各种内径的毛细管兼容的编织物。优化了萃取条件，在优化条件下证实了高效萃取。还优化了所有影响解吸效率的参数，其中对于水中 1.0μg/mL 的菲的萃取，典型的萃取效率超过 90%。通过采用两种有机溶剂的顺序泵送过程，可以充分解吸提取的分析物。在编织物的制备过程中，可以将不同类型的纤维材料插入编织物中心的开口中。利用编织物的这一特点，将不锈钢丝插入编织物的中心。通过对不锈钢丝施加低电压，还研究了热辅助解吸提取的分析物。实验中，施加 2V 电压即可实现完全解吸（高于 99.0%）。菲的最低定量下限 (LOQ) 和最低检测限 (LOD) 分别为 0.048μg/mL 和 0.014μg/mL。
