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This work aims to explore a new method for the efficient enrichment of baicalin in Scutellaria baicalensis Georgi by using metal organic frameworks (MOFs) materials, and to open up new applications for MOFs in the adsorption direction. The zeolitic imidazolate framework-8 (ZIF-8) was synthesized by solvothermal method and characterized by structure to ensure its accurate synthesis. Baicalin was extracted from Scutellaria baicalinsis Georgi by ethanol extraction and acid precipitation method. The ZIF-8 was used to carry out the static adsorption experiment on the crude extract of Radix Scutellariae. After the adsorption equilibrium was reached, the mixture was centrifuged, and the residual concentration of baicalin was detected by high performance liquid chromatography method (HPLC). The recovered saturated adsorbed ZIF-8 material was washed with water and dried, and the phosphate buffered saline (PBS) solution of pH 6.8 was used as a desorption solution, and the desorption was performed by shaking. The content of baicalin in the desorbed solution was determined by HPLC to calculate the desorption rate and achieve the purpose of adsorbent recovery. In the adsorbing process, the effects of adsorbent dosage, pH and adsorbate concentration of the crude extract of Radix Scutellariae were also optimized, and the response surface test (RSM) was performed using Design Expert software to obtain optimal adsorption conditions. Under these conditions, the adsorption rate of ZIF-8 to baicalin in Radix Scutellariae was as high as 98.22%, and the adsorption effect was not significant on other components in Radix Scutellariae. The desorption rate of ZIF-8 adsorbed baicalin in pH 6.8 solution was 62.46%, and the purity of baicalin increased from 21.55% before adsorption to 64.27% after desorption, and ZIF-8 had good stability before and after adsorption, and the recovery rate reached 83.50%. Therefore, ZIF-8 has potential application value in the adsorption and purification of baicalin. The adsorption law and mechanism of ZIF-8 on baicalin were studied: The adsorption of baicalin on ZIF-8 accorded with the quasi-second-order kinetic equation, and the equilibrium adsorption data accorded with the Langmuir adsorption isotherm model. Keywords metal-organic framework; adsorption; X-ray photoelectron spectroscopy 1 引言 金属有机骨架(MOFs)是由无机金属离子(或者金属 簇)与含氮或氧的多齿有机配体通过配位作用自组装而 形成的具有规则的一维、二维或者三维的配位聚合物材 料 [1~3]. 由于 MOFs 具有较高的比表面积和孔容, 孔径 大小可调, 可调控的表面性质, 被认为是吸附 [4,5] 、 储存、 传感 [6~8] 和催化 [9~13] 反应的潜在材料. Henni 等 [14] 引入非 氨基基团制备了[Bnim][Ac]@ZIF-30, CO 2 容量达到 0.8 mmol•g-1. Li 等 [15] 采用高通量计算筛选方法, 在 2932 种 MOFs 材料中筛选出了 Y-BTC, 对甲醛吸附量最高为 0.38 mmol•g-1 , 而且直至第 5 次循环吸附时仍保持了首
This work aims to explore a new method for the efficient enrichment of baicalin in Scutellaria baicalensis Georgi by using metal organic frameworks (MOFs) materials, and to open up new applications for MOFs in the adsorption direction. The zeolitic imidazolate framework-8 (ZIF-8) was synthesized by solvothermal method and characterized by structure to ensure its accurate synthesis. Baicalin was extracted from Scutellaria baicalinsis Georgi by ethanol extraction and acid precipitation method. The ZIF-8 was used to carry out the static adsorption experiment on the crude extract of Radix Scutellariae. After the adsorption equilibrium was reached, the mixture was centrifuged, and the residual concentration of baicalin was detected by high performance liquid chromatography method (HPLC). The recovered saturated adsorbed ZIF-8 material was washed with water and dried, and the phosphate buffered saline (PBS) solution of pH 6.8 was used as a desorption solution, and the desorption was performed by shaking. The content of baicalin in the desorbed solution was determined by HPLC to calculate the desorption rate and achieve the purpose of adsorbent recovery. In the adsorbing process, the effects of adsorbent dosage, pH and adsorbate concentration of the crude extract of Radix Scutellariae were also optimized, and the response surface test (RSM) was performed using Design Expert software to obtain optimal adsorption conditions. Under these conditions, the adsorption rate of ZIF-8 to baicalin in Radix Scutellariae was as high as 98.22%, and the adsorption effect was not significant on other components in Radix Scutellariae. The desorption rate of ZIF-8 adsorbed baicalin in pH 6.8 solution was 62.46%, and the purity of baicalin increased from 21.55% before adsorption to 64.27% after desorption, and ZIF-8 had good stability before and after adsorption, and the recovery rate reached 83.50%. Therefore, ZIF-8 has potential application value in the adsorption and purification of baicalin. The adsorption law and mechanism of ZIF-8 on baicalin were studied: The adsorption of baicalin on ZIF-8 accorded with the quasi-second-order kinetic equation, and the equilibrium adsorption data accorded with the Langmuir adsorption isotherm model. Keywords metal-organic framework; adsorption; X-ray photoelectron spectroscopy 1 引言 金属有机骨架(MOFs)是由无机金属离子(或者金属 簇)与含氮或氧的多齿有机配体通过配位作用自组装而 形成的具有规则的一维、二维或者三维的配位聚合物材 料 [1~3]. 由于 MOFs 具有较高的比表面积和孔容, 孔径 大小可调, 可调控的表面性质, 被认为是吸附 [4,5] 、 储存、 传感 [6~8] 和催化 [9~13] 反应的潜在材料. Henni 等 [14] 引入非 氨基基团制备了[Bnim][Ac]@ZIF-30, CO 2 容量达到 0.8 mmol•g-1. Li 等 [15] 采用高通量计算筛选方法, 在 2932 种 MOFs 材料中筛选出了 Y-BTC, 对甲醛吸附量最高为 0.38 mmol•g-1 , 而且直至第 5 次循环吸附时仍保持了首
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