Wang Licheng, Shangguan Yangnan, Hou Xiudan, Jia Yong, Liu Shujuan, Sun Yingxin, Guo Yong
CAS Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Lanzhou, China.
Exploration and Development Research Institute, Changqing Oilfield, Xi'an, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Aug 15;1060:91-96. doi: 10.1016/j.jchromb.2017.05.034. Epub 2017 May 31.
As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment.
作为一种新型固相萃取材料，氧化锌晶须被用于提取黄酮类化合物，并表现出良好的提取能力。采用X射线衍射、带能谱的扫描电子显微镜和比表面积/孔体积对吸附剂进行了表征。将氧化锌填充到固相萃取微柱中，并通过四种黄酮类化合物模型评估其提取能力。对样品加载和洗脱参数进行了优化，建立了基于氧化锌的黄酮类化合物分析方法。结果表明，该方法线性范围宽，为1至150μg/L，检测限低，为0.25μg/L。单柱重复性和柱间重现性的相对标准偏差分别小于6.8%和10.6%。采用所建立的方法对多个实际样品进行了分析，获得了满意的结果。计算了黄酮类化合物与氧化锌之间的相互作用，证明其源于锌原子的4p和5d轨道与黄酮类苯基相邻π轨道之间的范德华力。此外，氧化锌晶须表现出良好的稳定性，在操作条件下可重复使用50次以上。这项工作证明氧化锌晶须是富集黄酮类化合物的良好候选材料。
