School of Pharmacy, Southwest Medical University, Luzhou, 646000, Sichuan, China.
School of Pharmacy, Chongqing University, Chongqing, 401331, China.
Anal Bioanal Chem. 2020 Feb;412(6):1365-1374. doi: 10.1007/s00216-019-02363-3. Epub 2020 Jan 3.
Molybdenum disulfide quantum dots (MoS QDs) were chosen as a functional two-dimensional material to improve the separation performance of a traditional C18 column. In this work, MoS QDs were synthesized by the combination of sonication and solvothermal treatment of bulk MoS. The prepared MoS QDs were characterized by transmission electron microscope (TEM), Zeta potential measurement, UV-visible absorption and fluorescence spectroscopy. Then, a novel MoS QDs embedded C18 (Sil-MoS-C18) stationary phase was prepared for performing mixed-mode liquid chromatography. The results of elemental analysis (EA), thermogravimetric analysis (TGA), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) and Brunauer-Emmett-Teller (BET) measurements indicated the stationary phase was prepared successfully. Five types of compounds including alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs), nucleosides and nucleobases, anilines and flavonoids were utilized to evaluate reversed phase, weak cation exchange and hydrophilic interaction of the new column. To a certain extent, the column could achieve separation for different properties of samples on one column, with less organic solvent and shorter time than conventional alkyl and amino columns. Furthermore, the mechanism for separation was studied by investigating effects of mobile phase composition and pH on retentions. In summary, the Sil-MoS-C18 stationary phase was deemed able to serve the performance of various types of phases, which revealed the prepared mixed-mode column could be potentially applied for the analysis of complex samples. Graphical abstract.
二硫化钼量子点（MoS QDs）被选为一种功能二维材料，以提高传统 C18 柱的分离性能。在这项工作中，通过超声处理和块状 MoS 的溶剂热处理相结合合成了 MoS QDs。通过透射电子显微镜（TEM）、Zeta 电位测量、紫外-可见吸收和荧光光谱对制备的 MoS QDs 进行了表征。然后，制备了一种新型的 MoS QDs 嵌入 C18（Sil-MoS-C18）固定相，用于执行混合模式液相色谱。元素分析（EA）、热重分析（TGA）、傅里叶变换红外光谱（FT-IR）、X 射线光电子能谱（XPS）、扫描电子显微镜（SEM）和 Brunauer-Emmett-Teller（BET）测量的结果表明固定相制备成功。利用包括烷基苯、多环芳烃（PAHs）、核苷和碱基、苯胺和黄酮类化合物在内的 5 种化合物，评估了新柱的反相、弱阳离子交换和亲水相互作用。在一定程度上，该柱可以在一根柱子上对不同性质的样品进行分离，与传统的烷基和氨基柱相比，有机溶剂用量更少，时间更短。此外，通过研究流动相组成和 pH 值对保留的影响，研究了分离的机理。总之，Sil-MoS-C18 固定相能够发挥各种类型相的性能，表明所制备的混合模式柱有望用于复杂样品的分析。
