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Method for preparing dihydrochalcone molecular imprinting solid phase extraction column filler material

A technology of dihydrochalcone and solid phase extraction column, which is applied in chemical instruments and methods, other chemical processes and other directions, can solve the problems of complex composition of natural products, low content of dihydrochalcone, poor selectivity and the like

Inactive Publication Date: 2008-10-01
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005]Because the content of dihydrochalcone in natural products is very low, and the composition of natural products is very complex, it is extracted with traditional organic solvents, and the column layer of ordinary packing Separation methods such as analysis are time-consuming, laborious, and have poor selectivity, and it is difficult to meet the current separation requirements. Therefore, research on efficient separation technologies has become the focus and difficulty of natural product research and development.

Method used

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  • Method for preparing dihydrochalcone molecular imprinting solid phase extraction column filler material
  • Method for preparing dihydrochalcone molecular imprinting solid phase extraction column filler material
  • Method for preparing dihydrochalcone molecular imprinting solid phase extraction column filler material

Examples

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Effect test

Embodiment 1

[0015] Example 1: Preparation of packing materials for the molecularly imprinted solid phase extraction column of dragon blood B, see Table 1 for the specific raw materials and dosage.

[0016] Table 1 Reaction raw materials and consumption

[0017]

[0018] 1. The reaction raw material template molecule loureirin B (Loureirin B), functional monomer acrylamide, crosslinking agent ethylene glycol dimethacrylate and porogen acetonitrile are added to the grinding port successively according to the consumption of table 1 In the three-neck flask, ultrasonically mix for 30 minutes, after mixing evenly, add 30 mg of azobisisobutyronitrile, ultrasonic degassing for 10 minutes, nitrogen gas for 20 minutes, seal, and react in a water bath at 60°C for 24 hours to obtain crude dragon blood molecule B imprinted polymer;

[0019] 2. Grind the above-mentioned dragon blood B molecularly imprinted polymer to about 75 μm, put it into a Soxhlet extractor, and r...

Embodiment 2

[0027] Example 2: Preparation of packing materials for the molecularly imprinted solid-phase extraction column of dragon blood A, see Table 2 for the specific raw materials and dosage.

[0028] Table 2 Reaction raw materials and consumption

[0029]

[0030] 1. Add the reaction raw material Loureirin A (Loureirin A), the functional monomer acrylamide, the crosslinking agent ethylene glycol dimethacrylate and the porogen acetonitrile to the three-neck bottle with a ground mouth according to the dosage in Table 2. In the process, ultrasonically mix for 20 minutes, after mixing evenly, add 20 mg of azobisisobutyronitrile, ultrasonically degas for 15 minutes, pass nitrogen gas for 20 minutes, seal, and react in a water bath at 60°C for 36 hours to obtain a molecularly imprinted polymer of dragon blood A;

[0031] 2. Grind the above-mentioned dragon blood A molecularly imprinted polymer to about 75 μm, put it into a Soxhlet extractor, and use a mixed sol...

Embodiment 3

[0039] Example 3: Preparation of filling materials for phoenixin A molecularly imprinted solid-phase extraction column, the reaction raw materials and dosage are shown in Table 3.

[0040] Table 3 Reaction raw materials and consumption

[0041]

[0042] 1. Add the reaction raw material cochinchinenin A (cochinchinenin A), functional monomer acrylamide, cross-linking agent ethylene glycol dimethacrylate and porogen chloroform to the grinding port according to the consumption of Table 3 In the three-necked bottle, ultrasonically mix for 40 minutes, after mixing evenly, add 30 mg of azobisisobutyronitrile, ultrasonic degassing for 10 minutes, nitrogen gas for 20 minutes, seal it, and react in a water bath at 55°C for 36 hours to obtain crude phoenixin A molecularly imprinted polymer;

[0043] 2. Grind the above molecularly imprinted polymer of stegophyllin A to about 75 μm, put it into a Soxhlet extractor, and repeatedly extract it with a mixed solve...

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Abstract

The invention relates to a preparation method of dihydrochalcone molecule imprinted solid phase extraction column filling material. In the method, reaction raw materials: template module dihydrochalcone, acrylamide, crosslinking agent ethylene glycol dimethacrylate are added to pore-foaming agent such as acetonitrile or chloroform, uniformed mixed, initiator azobisisobutyronitrile is added, degassed and filled with nitrogen before being sealed, and are reacted under the temperature of 40-80 DEG C for 20-48 hours to obtain coarse molecule imprinted polymer which is then grinded to granularity of 15-80 micro meters; soxhlet extraction is carried out by a mixed solvent of methanol and acetic acid; acetone is then used for deposition so as to remove fine grains and to obtain dihydrochalcone molecule imprinted polymer; the polymer is uniformly filled in the polypropylene cylinder so as to obtain the dihydrochalcone molecule imprinted solid phase extraction column, thus separating enriched dihydrochalcone from natural outcome simply and efficiently.

Description

technical field [0001] The invention relates to a preparation method of a molecular imprinted solid phase extraction column filling material, in particular to a preparation method of a dihydrochalcone molecular imprinted solid phase extraction column filling material. Background technique [0002] Dihydrochalcone (dihydrochalcone, DHC) is a class of compounds with the core structure of benzochromone, which can be regarded as the product of C ring opening of dihydroflavone under alkaline conditions. It has been obtained from Liliaceae, It is isolated from plants such as Asteraceae, Rosaceae, and Rhododendronaceae. Dihydrochalcone is a very important class of medicinal active ingredients, which have antioxidant, antitumor, antidiabetic, antibacterial and antiepileptic effects. [0003] Yang Chongren et al. (Yang Chongren, Wang Jinliang, Li Xingcong et al. Chemical constituents and antifungal activity of D. yunnanensis. Yunnan Botanical Research, 1995, 17(3): 336-340.) isolate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30
Inventor 吕敬慈雍克岚霍世欣王玉芹陈旭
Owner SHANGHAI UNIV
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