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A method for separation and purification of macromolecular phenolic acids in tree moss extract

A technology of molecular depsidic acid and tree moss extract, which is applied in the directions of tobacco, tobacco processing, tobacco preparation, etc., can solve the problem of inability to separate macromolecular depsidic acid compounds, and achieves improved use value, expanded application fields and effects. significant effect

Active Publication Date: 2022-04-29
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Similarly, this method can only separate the soluble and volatile small molecule aroma-generating substances in the tree moss extract, but cannot separate the macromolecular depsipated phenolic compounds in the tree moss extract

Method used

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  • A method for separation and purification of macromolecular phenolic acids in tree moss extract
  • A method for separation and purification of macromolecular phenolic acids in tree moss extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] S1. Weigh 20g of acetonitrile solvent and pour it into a large beaker, stir with a magnetic stirrer at a stirring speed of 400r / min, weigh 2g of tree moss extract liquid in a small beaker, and then use a dropper to remove the tree moss extract liquid in the small beaker. Add the liquid moss extract dropwise into a large beaker to obtain a mixed solution. After the addition, continue to stir for 40 minutes, then pour the mixed solution into a Buchner funnel with a vacuum suction bottle for suction and filtration, and control its vacuum degree to 5kPa After filtering, add acetonitrile solvent to the filter cake to wash and filter to obtain 0.91 g of brown depsipolic acid solid crude product;

[0032] S2. Pour 30mL of ethylene glycol solvent into a round-bottomed flask, add 0.91g of brown depsipphenolic acid solid crude product into the round-bottomed flask for stirring, then put a condensation reflux device on the flask, heat up to 120°C, and stir for 20 min;

[0033] S3...

Embodiment 2

[0035]S1. Weigh 40g of dimethylformamide solvent and pour it into a large beaker, stir with a magnetic stirrer at a stirring speed of 600 r / min, weigh 3g of tree moss extract liquid in a small beaker, and then use a dropper to The tree moss extract liquid was added dropwise in a large beaker to obtain a mixed solution. After the addition was completed, continue to stir for 30 minutes, then pour the mixed solution into a Buchner funnel with a vacuum bottle for suction and filtration, and control its vacuum degree to be 10kPa, after filtering, add dimethylformamide solvent to filter cake and wash and filter, obtain 1.35 g brown depsipphenolic acid solid crude product;

[0036] S2. Pour 30 mL of acetic acid solvent into a round-bottomed flask, add 1.35 g of brown depsipphenolic acid solid crude product into the round-bottomed flask for stirring, then put a condensation reflux device on the flask, heat up to 100 °C, and stir for 30 min;

[0037] S3, after the brown phenolic acid s...

Embodiment 3

[0039] S1. Weigh 60g of dimethyl sulfoxide solvent and pour it into a large beaker, stir with a magnetic stirrer at a stirring speed of 800 r / min, weigh 2g of tree moss extract liquid in a small beaker, and then use a dropper to The tree moss extract liquid was added dropwise in a large beaker to obtain a mixed solution. After the addition was completed, continue to stir for 20 minutes, then pour the mixed solution into a Buchner funnel with a vacuum bottle for suction and filtration, and control its vacuum degree to be 20kPa, after filtering, add dimethyl sulfoxide solvent to filter cake and wash and filter, obtain 0.92 g brown depsipphenolic acid solid crude product;

[0040] S2. Pour 30 mL of dimethylformamide solvent into a round-bottomed flask, add 0.92 g of brown depsipphenolic acid solid crude product into the round-bottomed flask for stirring, then put a condensation reflux device on the flask, and heat up to 80°C. Stir for 40 min;

[0041] S3. After the brown phenoli...

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Abstract

The invention discloses a method for separating and purifying macromolecular phenolic acids in tree moss extract. According to the physical and chemical properties of the functional groups in the molecular structure of tree moss extract, the aprotic polarity of specific molecular structure is selected. Non-toxic organic solvent, dissolves and extracts all the easily soluble small molecular aroma substances in the tree moss extract, and at the same time makes the macromolecular substances of depsipolic acids precipitate in the solvent due to poor solubility, reaching the small molecular substances and The effect of complete separation of macromolecular phenolic acids. The isolated depsipolic acid solids are purified by recrystallization from a suitable organic solvent to obtain depsipolic acid solids with lighter color and higher purity. The separation method provided by the invention can improve the use value of the tree moss extract and expand its application field. The purified depsipated phenolic acid solid is in the form of granules, which is loose, dry, non-sticky, easy to use and add, etc. It has a good application prospect in both traditional cigarettes and new tobaccos.

Description

technical field [0001] The invention relates to the field of separation and purification of macromolecular latent aroma substances in tree moss extract, in particular to a method for separation and purification of macromolecular depsipated phenolic acids in tree moss extract. Background technique [0002] The tree moss extract is composed of powdery flat branches attached to the trunks of pine, fir, spruce, fir, etc., and clustered tree flowers attached to the trunks of oak and oak, soaked in benzene, petroleum ether or hot alcohol Get it. The benzene extract is dark brown to green-brown solid, and the petroleum ether extract is dark brown thick paste. It has green aroma and pine wood smell. The main ingredients include orcinol, orcinol monomethyl ether, ethyl orcinol carboxylate, methyl lentilate, ethyl lentilate, methyl erythrinate, etc., which are soluble and volatile Molecular aroma components, as well as insoluble macromolecular latent aroma substances, are mainly a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A24B15/30A24B15/12A24B3/12A24B3/14
CPCA24B15/302A24B15/12A24B3/12A24B3/14
Inventor 朱龙杰张媛曹毅刘梦梦吴洋张华朱怀远王珂清秦艳华李炜
Owner CHINA TOBACCO JIANGSU INDAL
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