Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract

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: 2014-08-06
邳州恒翔生物制品有限公司
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  • 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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  • Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract
  • Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract
  • Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. HPLC analysis method of total flavonoids in Ginkgo biloba extract

[0055] Using UV detection method

[0056] (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.

[0057] (2) Standard curve drawing: Accurately weigh appropriate amounts of quercetin, kaempferol, and isorhamnetin reference substances respectively, place them in a 10mL volumetric flask, dissolve them with methanol and dilute to the mark, shake well, and make the concentrations respectively 0.854 , 0.562, 0.259mg / mL mixed reference substance solution; successively accurately measure the mixed reference substance 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 well, 10 μL samples were taken for chromatographic analysis. The equation of quercetin standard curve is y=51908x+63...

Embodiment 2

[0074] Negative pressure extraction and extract pretreatment

[0075] Ginkgo fresh leaves or ginkgo dry leaves are crushed to below 0.5 cm, and 40-80% ethanol is used as an extraction solvent, and the negative pressure boiling is extracted for 30-90 minutes, preferably 45-60 minutes, and the ratio of the extraction solvent to the 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, extract 1-4 times, preferably 2-3 times, extract The solution is firstly filtered through quartz sand with a particle size of 100-300 mesh, and then 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 ginkgo flavonoids is greater than 90%, and the extraction rate of ginkgolides The extraction rate is greater than 80%.

[0076] The present invention has studied the influence of extraction pressu...

Embodiment 3

[0085] Membrane purification process

[0086] Pass the above filtrate through a ceramic membrane with a pore size of 0.1 μm to 0.8 μm, preferably a ceramic membrane with a pore size of 0.5 μm and an operating pressure of 0.15 to 0.3 MPa, and continue to pass the ceramic membrane permeate through an ultrafiltration membrane with a molecular weight cut-off of 5,000 to 50,000 , the preferred ultrafiltration membrane molecular mass cut-off is 10000, the ultrafiltration membrane permeate is concentrated with a nanofiltration membrane with a molecular mass cut-off of 100-300, the concentrated solution is decompressed to recover ethanol, and the pH value of the concentrated solution is adjusted with acid After 4 to 6, the upper column liquid is obtained.

[0087] The present invention selects 0.1 μ m, 0.2 μ m, 0.5 μ m, the ceramic membrane aperture of 0.8 μ m, investigates the impact of the membrane aperture on membrane flux, transfer rate and impurity removal rate of total flavonoid...

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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 low-acid ginkgo extract from ginkgo leaves by negative pressure boiling extraction. Background technique [0002] Ginkgo Biloba L. is a living fossil and a symbol of longevity. Ginkgo biloba is rich in disease-resistant bioactive factors, such as flavonoids, lactones, polyprenol, polysaccharides, proteins, etc., which have attracted international attention. German Schwabe company uses solvent extraction technology to produce standard ginkgo biloba extract (GBE761), the main active substances are flavonoids and lactones, which is a best-selling herbal medicine for the treatment of cardiovascular and cerebrovascular diseases. Internationally, the annual sales of Ginkgo biloba extract (GBE) and its preparations have reached 6.5 billion US dollars, ranking among the top three in the US herbal medicine market. Ginkgo is an important economic forest tree...

Claims

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Application Information

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Patent Type & Authority Applications(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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