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合成一种聚合物型咪唑嵌入十八烷基离子液体接枝硅胶吸附剂,用于提取黄酮类化合物。

Synthesis of a polymeric imidazolium-embedded octadecyl ionic liquid-grafted silica sorbent for extraction of flavonoids.

机构信息

State Key Laboratory of Biobased Material and Green Papermaking, Qilu University of Technology, Shandong Academy of Sciences, Jinan 250353, China; School of Food Science and Engineering, Qilu University of Technology, Shandong Academy of Sciences, Jinan 250353, China.

Nanjing Agricultural University, Nanjing 210095, China.

出版信息

J Chromatogr A. 2019 Nov 22;1606:460376. doi: 10.1016/j.chroma.2019.460376. Epub 2019 Jul 18.

Abstract

In this work, a polymeric imidazolium-embedded octadecyl ionic liquid (poly(1-vinyl-3-octadecylimidazolium naphthalene sulfonate))-grafted silica (poly(CVImNapSO)@SiO) sorbent was prepared and applied as a solid-phase extraction (SPE) sorbent in extraction of flavonoids. The synthesized poly(CVImNapSO)@SiO sorbent was characterized by X-ray photoelectron spectrogram (XPS) and fourier transform infrared spectroscopy (FT-IR). The thermodynamic and kinetic adsorption models of the prepared poly(CVImNapSO)@SiO sorbent towards flavonoids were discussed by nonlinear fitting adsorption curve and the results indicated the thermodynamic adsorption model in this work was tended to be Freundlich model rather than Langmuir one and the pseudo-second order model could be used to describe the dynamic adsorption process. In addition, the adsorption amounts indicated the sorbent has satisfactory extraction capabities towards flavonoids. For investigating the influence of independent variables and their interactions on the extraction efficiency, a Box-Behnken design was used for optimizing three greatly influential parameters after performing single-factor experiments. The interaction energies between flavonoids and two ionic liquids were calculated to understand the adsorption mechanism. Under the optimal conditions, a method used for determining flavonoids was developed by combining SPE technique with high performance liquid chromatography (HPLC), and the developed method exhibited low limits of detection (0.25-0.4 μg L), good linearities with correlation coefficients (R) in the range of 0.9951-0.9996 and satisfactory recoveries ranging from 83.6% to 114.1%, which confirmed the proposed method could be successfully used to determine trace flavonoids in real samples.

摘要

在这项工作中,制备了一种聚合离子液体(聚(1-乙烯基-3-十八烷基咪唑啉萘磺酸盐))嵌入十八烷基离子液体(poly(1-vinyl-3-octadecylimidazolium naphthalene sulfonate))-接枝二氧化硅(poly(CVImNapSO)@SiO)吸附剂,并将其作为固相萃取(SPE)吸附剂用于黄酮类化合物的提取。通过 X 射线光电子能谱(XPS)和傅里叶变换红外光谱(FT-IR)对合成的 poly(CVImNapSO)@SiO 吸附剂进行了表征。通过非线性拟合吸附曲线讨论了制备的 poly(CVImNapSO)@SiO 吸附剂对黄酮类化合物的热力学和动力学吸附模型,结果表明,本工作中的热力学吸附模型倾向于 Freundlich 模型,而不是 Langmuir 模型,并且可以使用拟二级动力学模型来描述动态吸附过程。此外,吸附量表明该吸附剂对黄酮类化合物具有良好的提取能力。为了研究独立变量及其相互作用对萃取效率的影响,在进行单因素实验后,使用 Box-Behnken 设计优化了三个影响较大的参数。计算了黄酮类化合物与两种离子液体之间的相互作用能,以了解吸附机理。在最佳条件下,结合固相萃取技术和高效液相色谱(HPLC)开发了一种用于测定黄酮类化合物的方法,该方法的检测限低(0.25-0.4μg L),线性范围宽(0.9951-0.9996),回收率良好(83.6%-114.1%),证实了该方法可成功用于测定实际样品中的痕量黄酮类化合物。

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