Preparation method of pine needle flavone

A technology of pine needles and flavonoids, applied in the direction of anti-toxins, medical raw materials derived from gymnosperms, drug combinations, etc., can solve problems such as difficult operation, low efficiency, and pine needle damage, and achieve good product quality, high equipment requirements, The effect of mild enzymatic conditions

Inactive Publication Date: 2014-01-15
CHINA JILIANG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

However, the current desertification and soil erosion in our country are relatively serious. The country calls for returning farmland to forests and prohibits large-scale felling. Therefore, it is not the best strategy to mainly rely on large-scale felling of pine needles to obtain pine needles
And relying on simple manual harvesting of pine needles or pine needle skins not only causes great damage to pine needles, but also is difficult to operate, inefficient, and expensive, so it is not practical

Method used

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  • Preparation method of pine needle flavone
  • Preparation method of pine needle flavone
  • Preparation method of pine needle flavone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Preparation of raw materials: select the larch needles of Masson pine produced in Zhejiang Province, remove the impurities, wash and dry at 60°C, and turn it from time to time. After the pine needles become brittle, take them out and crush them, sieve them, and take 20- 40 mesh, 40-100 mesh, 100-150 mesh, 150-200 mesh, 200-300 mesh, more than 300 mesh powder, refrigerated and ready for use.

[0043] 2. Reagents: ethanol, standard rutin, sodium nitrite, aluminum nitrate, sodium hydroxide, hemicellulase (3000u / g), cellulase (40000u / g).

[0044] 3. Instruments: HMB-701C pulverizer, H1650 high-speed centrifuge, DZF-6050 vacuum drying oven, DK-8D electric heating constant temperature water tank (temperature fluctuation: ±0.5°C), RE-52A rotary evaporator, AL-104 electronic balance ( Graduation value: 0.0001g), UV-2100 ultraviolet-visible spectrophotometer, HH-2 digital display constant temperature water bath, ZXE-Z rotary vane vacuum pump, vortex oscillator, etc.

[0045]...

Embodiment 2

[0136] Processing of raw materials: Take 10g of dry pine needle powder (with a particle size of 150-200 mesh), add citric acid-sodium citrate buffer solution (0.1mol / L) 40 times the mass of pine needle dry powder (400g), mix well to obtain a mixture , add 0.1% cellulase (enzyme activity: 40000u / g) in the mass of the mixture, and ultrasonically hydrolyze for 120 minutes at 45°C and pH 5.0, then add 5% hemicellulase (enzyme activity) in the mass of the mixture 3000u / g), raise the temperature to 50°C, and then ultrasonically hydrolyze for 90 minutes, raise the temperature to 90°C and keep it for 5 minutes, then lower it to 80°C, add 700g of 79% ethanol aqueous solution for extraction, ethanol aqueous solution and lemon The mass ratio of the total mass of the acid-sodium citrate buffer solution to the dry powder of pine needles is 110:1, extracted at a temperature of 78°C for 128min, then centrifuged, and the flavonoid content in the supernatant was detected to be 72.24mg / g, filter...

Embodiment 3

[0138] Processing of raw materials: Take 10g of dry pine needle powder (with a particle size of 150-200 mesh), add citric acid-sodium citrate buffer solution (0.1mol / L) 40 times the mass of pine needle dry powder (400g), mix well to obtain a mixture , add 0.5% cellulase (enzyme activity: 40000u / g) in the mass of the mixture, and ultrasonically hydrolyze for 90 minutes at 45°C and pH 5.0, then add 1% hemicellulase in the mass of the mixture (enzyme activity 3000u / g), raise the temperature to 55°C, and then ultrasonically hydrolyze for 150min, then raise the temperature to 90°C and keep it for 5min, then lower it to 80°C, add 700g of 79% ethanol aqueous solution for extraction, ethanol aqueous solution and lemon The mass ratio of the total mass of the acid-sodium citrate buffer solution to the dry powder of pine needles is 110:1, extracted at a temperature of 78°C for 128min, and then centrifuged to detect that the flavonoid content in the supernatant is 69.17mg / g, according to t...

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Abstract

The invention discloses a preparation method of pine needle flavone, which comprises the steps that pine needle drying powder is added to a citric acid-sodium citrate buffer solution; ultrasonic enzymolysis is performed by cellulase; hemicellulase is added for the ultrasonic enzymolysis; high-temperature inactivation is performed; an alcohol aqueous solution is added for extraction; the alcohol-containing final mass concentration of an obtained extracting solution after the alcohol aqueous solution is added is 50%; the extraction is performed for 90-150min at 70-90 DEG C; centrifugation and filtering are performed; a filtrate is concentrated; a solvent is removed; and pine needle flavone is prepared. According to the preparation method, a yield of a natural flavonoid substance obtained after pine needle with the particle size of 150-200 meshes is prepared by sequential cellulase and hemicellulase treatment and an ultrasonic technology; an antioxidation effect is good; an extraction yield can reach 73.86mg/g; and the hydroxy radical and DPPH (1,1-diphenyl-2-picrylhydrazyl radical) scavenging capacity and the reducing capacity are approximate to VC (vinyl chloride) with the same concentration.

Description

(1) Technical field [0001] The invention relates to a method for preparing natural antioxidant flavonoids from pine needles. (2) Background technology [0002] Pine needles, also known as bristle pine hairs, pine hairs, and mountain pine whiskers, are needle-like leaves of Pinaceae plants. The main plant sources are Pinus massoniana Lamb., P. koraiensis Sieb.et Zucc., P. thunbergii Parl., P.tabuleaformis Carr., P.armandii Franch., P.yunnanensis Franch., P.taiwanensis Hayata, P.elliottii Engelm., etc. Pine needle is a traditional Chinese medicine in my country, which has been recorded in successive dynasties of herbal medicine. As recorded in "Compendium of Materia Medica": "Pine needles have a bitter, warm, and non-toxic smell. Taking it for a long time makes people not old, lightens the body and nourishes qi, controls rheumatic sores, grows hair, calms the five internal organs, keeps the middle, and prolongs life without hunger." Drinking pine needle tea can alleviate the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/15A61P39/06A61K127/00
Inventor 张拥军陈丛婧郑龙华张文革朱丽云
Owner CHINA JILIANG UNIV
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