Method for on-line enrichment and purification of diosmetin in dandelion

A technology of diosmin and dandelion, applied in chemical instruments and methods, separation methods, organic chemistry, etc., can solve the problems of high cost and heavy pollution, and achieve the effect of enhanced adsorption performance, simple operation, and economical and effective

Active Publication Date: 2022-04-29
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for online enrichment and purification of diosmin in dandelion to solve the pr

Method used

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  • Method for on-line enrichment and purification of diosmetin in dandelion
  • Method for on-line enrichment and purification of diosmetin in dandelion
  • Method for on-line enrichment and purification of diosmetin in dandelion

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Embodiment 1

[0038] The synthesis of embodiment 1 MOF material

[0039] Add 2-aminoterephthalic acid (1.80 g), chromium nitrate nonahydrate (4.0 g) and sodium hydroxide (0.9 g) into 75 mL of deionized water in turn and transfer to the reaction kettle, react at 150 °C for 12 h, and The reaction mixture was centrifuged, and the obtained solid was washed three times with N,N-dimethylformamide (DMF) and absolute ethanol respectively. C reacted for 12 h to purify the material, centrifuge and dry to obtain MOF material.

Embodiment 2

[0040] Example 2 Derivatization of MOF materials (method 1)

[0041] Add methacrylic acid (0.50 mL) and the MOF material prepared in Example 1 (0.20 g) into 20 mL of deionized water in sequence, and ultrasonicate for 30 min. After heating for 12 h, the resulting precipitate was washed three times with absolute ethanol and dried to obtain a solid material.

Embodiment 3

[0042] Example 3 Derivatization of MOF materials (method 2)

[0043] 2-(7-Azobenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate (2.3 g), methacrylic acid (0.50 mL), triethylamine (1.39 mL) and 0.5 g of the MOF material prepared in Example 1 were added to 30 mL of DMF, stirred and reacted at 30 °C for 10 h, the obtained precipitate was washed three times with DMF and absolute ethanol, and dried to obtain a solid material.

[0044] The infrared spectrum comparison between the MOF material obtained after derivatization using method 1 and method 2 and the original MOF material is as follows figure 1 As shown, it can be seen that the infrared spectrum of the derivatized material obtained using method 2 is at 1680 cm -1 The C=C stretching vibration peak appears at , and the infrared spectrum of the derivatized material obtained by using method 1 is at 1600~1700 cm -1 There is no stretching vibration peak of C=C in the range, so the derivatization by method 1 fails, an...

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Abstract

The invention provides a method for on-line enrichment and purification of diosmetin in dandelion. The method comprises the following steps: (a) synthesis of an MOF material; (b) derivatization of the MOF material; (c) preparing the monolithic column; (d) enriching and purifying diosmetin on line; and (e) separating the diosmetin. According to the prepared MOF/polymer monolithic column, the defects that a traditional polymer monolithic column is small in specific surface area and low in porosity are overcome, the adsorption performance of the MOF/polymer monolithic column on diosmetin is enhanced, and the material can effectively separate and enrich diosmetin. Meanwhile, by adopting a mode of combining normal phase chromatography and reversed phase chromatography, the separation effect of diosmetin and impurities is enhanced, and high-purity diosmetin can be effectively prepared. The method has the advantages of simplicity in operation, economy and effectiveness.

Description

technical field [0001] The invention relates to the technical field of separation and purification of diosmin, in particular to a method for online enrichment and purification of diosmin in dandelion. Background technique [0002] Diosmetin is a flavonoid compound derived from natural Chinese herbal medicines. It is abundant in citrus fruits and also exists in some medicinal plants of Rosaceae and Cruciferae. It has the functions of anti-inflammation, antibacterial, anti-oxidation, inhibition of tumor cell proliferation, and induction of tumor cell apoptosis, and has a wide range of applications in the treatment of various diseases. [0003] Diyerin has a variety of pharmacological activities and has a wide range of application prospects. It is mainly extracted from medicinal plants. However, the extracts of Chinese herbal medicines have complex components and many impurities. A series of methods such as extraction, chromatography, and recrystallization are usually used to e...

Claims

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Application Information

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IPC IPC(8): B01D15/20B01D15/26B01D15/42B01J20/30B01J20/26C07D311/30C07D311/40
CPCB01D15/206B01D15/424B01D15/26B01J20/226B01J20/262C07D311/30C07D311/40
Inventor 刘海燕王杉白立改闫宏远
Owner HEBEI UNIVERSITY
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