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A method for preparing low-acid ginkgo extract by negative pressure boiling extraction

A technology of ginkgo extract and negative pressure extraction, which is applied in the directions of medical raw materials, drug combinations, cardiovascular system diseases, etc. derived from Ginkgo biloba The problem of low ester content, etc., achieves the effect of simple process operation, shortened extraction time and improved extraction rate

Active Publication Date: 2017-05-24
邳州恒翔生物制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic ginkgo biloba extract manufacturers mostly use traditional heat reflux extraction, such as soaking and percolation. The most prominent problems in the production process are: long time, low extraction efficiency; damage to flavonoids and terpene lactones More; the quality of the extract is not high, the content of flavonoids and lactones is low, and there are many impurities, resulting in complicated subsequent purification processes, such as concentration, alcohol precipitation, water precipitation, filtration, centrifugation, adsorption, etc., resulting in long production cycles and energy consumption. And the cost is greatly increased, and the waste of resources is serious
However, this method has high production cost, low product yield, and uses a large amount of toxic organic solvents, which is not suitable for industrial production

Method used

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  • A method for preparing low-acid ginkgo extract by negative pressure boiling extraction
  • A method for preparing low-acid ginkgo extract by negative pressure boiling extraction
  • A method for preparing low-acid ginkgo extract by negative pressure boiling extraction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1. HPLC analysis method of total flavonoids in ginkgo extract

[0053] Using UV detection method

[0054] (1) Chromatographic conditions: Column C 18 ODS (Φ4.6mm×200mm, 5μm), mobile phase: methanol-water (containing 0.4% phosphoric acid) volume ratio 50:50, detection wavelength 360nm, flow rate 1mL / min.

[0055] (2) Standard curve drawing: accurately weigh out appropriate amounts of quercetin, kaempferol, and isorhamnetin reference substances, place them in a 10mL volumetric flask, dissolve and dilute to the mark with methanol, shake well, and make a concentration of 0.854 respectively , 0.562, 0.259mg / mL mixed reference solution; sequentially accurately measure the mixed reference solution 0.05, 0.10, 0.15, 0.20, 0.25, 0.30, 0.40, 0.50mL in a 5mL volumetric flask, dilute to the mark with methanol, After shaking up, 10μL of samples were taken for chromatographic analysis. The standard curve equation of quercetin is y=51908x+63760, r=0.996; the standard curve equation of kaem...

Embodiment 2

[0072] Vacuum extraction and extraction liquid pretreatment

[0073] Crush the fresh ginkgo leaves or dried ginkgo leaves to less than 0.5cm, use 40-80% ethanol as the extraction solvent, and extract by negative pressure boiling for 30-90 min, preferably 45-60 min. The ratio of extraction solvent to ginkgo leaf powder is 1-30: 1, preferably 5-15:1, extraction temperature is 20-70°C, preferably 40-60°C, extraction pressure is 0.01-0.09MPa, preferably 0.06-0.09MPa, extraction is 1 to 4 times, preferably 2 to 3 times, extraction The solution is filtered by quartz sand with a particle size of 100-300 mesh, and then subjected to microporous centrifugal filtration with a pore size of 1.0 μm to 1.5 μm and a centrifugal speed of 3000 to 6000 rpm; the extraction rate of total flavonoids of Ginkgo biloba is greater than 90%. The extraction rate is greater than 80%.

[0074] The present invention studies the influence of extraction pressure, alcohol concentration, material-to-liquid ratio an...

Embodiment 3

[0083] Membrane purification process

[0084] Pass the filtrate through a ceramic membrane with a pore size of 0.1μm~0.8μm, preferably a ceramic membrane with a pore size of 0.5μm and an operating pressure of 0.15~0.3MPa, and continue to pass the ceramic membrane permeate through an ultrafiltration membrane with a rejection relative molecular mass of 5000~50,000 Preferably, the relative molecular mass of the ultrafiltration membrane is 10000, the permeate of the ultrafiltration membrane is concentrated with a nanofiltration membrane with a relative molecular mass of 100-300, the concentrated solution is decompressed to recover ethanol, and the pH of the concentrated solution is adjusted with acid After 4-6, the upper column liquid is obtained.

[0085] The present invention selects ceramic membrane pore sizes of 0.1 μm, 0.2 μm, 0.5 μm, and 0.8 μm to investigate the influence of the membrane pore size on the membrane flux, the transfer rate of total flavonoids and total lactones, an...

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Abstract

The invention relates to a method for negative-pressure boiling extraction and preparation of a low-acid ginkgo extract from ginkgo leaves. According to the method, crushed fresh ginkgo leaves or dry ginkgo leaves are used as a raw material, hydrous ethanol is used as an extraction solvent, negative-pressure boiling extraction is carried out, then a liquid extract is filtered and then pretreated by using quartz sand and microporous centrifugal filtration, a filtrate is separated and purified by using a ceramic membrane and an ultrafiltration membrane, a solution passing through the ultrafiltration membrane is concentrated by using a nanofiltration membrane, then ethanol is recovered, a concentrate is subjected to purification with a macroporous resin and phenolic acid removal with a deacidification resin, and negative-pressure microwave spray drying or vacuum freeze drying is carried out so as to obtain the low-acid ginkgo extract. The low-acid ginkgo extract prepared by using the method has a low acid value, high purity, ginkgetin content of more than 28%, lactone content of more than 8% and ginkgolic acid of no greater than 1 ppm, and the method may become a novel technology for industrial production of a low-acid ginkgo extract product.

Description

Technical field [0001] The invention relates to the technical field of plant extracts, in particular to a method for preparing a low-acid ginkgo extract from ginkgo leaves by negative pressure boiling extraction. Background technique [0002] Ginkgo Biloba (Ginkgo Biloba L.) is a living fossil and a symbol of longevity. Ginkgo biloba is rich in anti-disease biologically active factors, such as flavonoids, lactones, polypentenol, polysaccharides, proteins, etc., and has attracted international attention. The German Schwabe company uses solvent extraction technology to produce standard ginkgo biloba extract (GBE761). The main active substances are flavonoids and lactones, which are best-selling botanicals for the treatment of cardiovascular and cerebrovascular diseases. Internationally, the annual sales of Ginkgo biloba extract (GBE) and preparations reached 6.5 billion U.S. dollars, consistently ranking the top three in the US herbal medicine market. Ginkgo is an important econo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/16A61P9/00A61K127/00
Inventor 王成章周昊
Owner 邳州恒翔生物制品有限公司
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