Extractant, extraction process and analysis method of high-activity ginkgo leaf extractive

An extraction agent and technology of ginkgo biloba, which is applied in the field of natural product extraction, can solve the problems of inability to use trace samples for quantitative analysis, ginkgolic acid cannot be separated well, and cumbersome processing operations, so as to inhibit the dissolution of impurities and reduce the consumption of energy and solvents , the effect of improving the dissolution rate

Inactive Publication Date: 2003-08-20
HUAZHONG AGRI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Italy reported the separation and identification of ginkgolic acids by supercritical fluid extraction and capillary gas chromatography / mass spectrometry. This method has the advantage of less interference and can separate and identify various ginkgolic acids. For quantitative analysis of micro samples
The supercritical fluid extraction separation and high-performance liquid chromatography of ginkgolic acid have been reported in China, but the above problems also exist, and the ginkgolic acids cannot be separated well.

Method used

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  • Extractant, extraction process and analysis method of high-activity ginkgo leaf extractive
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  • Extractant, extraction process and analysis method of high-activity ginkgo leaf extractive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] The composition and proportion of the extractant (calculated by weight): sodium bisulfite 10kg; tap water 8000kg; pH5.0.

[0075] Clean 300kg of dried ginkgo leaves, filter the water, put them into the extraction tank, add 5000kg of extractant at 94°C, cover and seal, raise the temperature in the extraction tank to 97°C, and keep 1 atmospheric pressure, stirring every half an hour For 1 minute, the temperature in the tank was controlled to drop by 2.5°C per hour. After leaching for 16 hours, 4400kg of the feed liquid was filtered out. Then add 3000kg of extractant solution to the extraction tank for the second leaching, filter out 3100kg of feed liquid after 10 hours, combine the two feed liquids with a centrifugal filter to coarsely filter out impurities below 20 mesh, and sand filter to fine filter out Impurities below 200 mesh were removed, and the feed liquid was cooled to 30°C.

[0076] The feed liquid flows through the NKA-9 resin adsorption column at a flow rate...

Embodiment 2

[0079] The composition and proportion of the extractant (calculated by weight): sodium sulfite 5kg; water 6000kg; pH 5.5.

[0080] Take 300kg of dried ginkgo leaves (Hubei Anlu) and clean them, filter the water, put them into the extraction tank, add 4000kg of extractant at 93°C, cover and seal, stir for 3 minutes every half hour, and after leaching for 10 hours, the temperature in the tank drops to 60°C, filter out the feed liquid, add 2000kg of extractant for the second extraction, filter after 6 hours, combine the two extracts to a total of 5600kg, and use the centrifugal filter for coarse filtration of the feed liquid, sand filter for fine filtration, and cool to 35 ℃; Still using the resin column in Example 1 to refine, collect ethanol eluent 1300kg, after concentrating to 40kg, adopt spray drying to obtain 9.02kg light yellow ginkgo leaf extract.

[0081] Test results: total flavonoid glycosides 27.6%, total terpene lactones 8.1%, proanthocyanidins 9.6%, ginkgolic acid 4...

Embodiment 3

[0083] The composition and proportion of the extractant (calculated by volume): sodium bisulfite 9kg; tap water 4500kg; pH 4.8.

[0084] Take 600kg of freshly picked ginkgo leaves (water content 72%) and 3000kg of extractant and put them into the extraction tank together, control the temperature at 70°C, stir intermittently for 10 minutes per hour, after leaching for 20 hours, filter out the material liquid, and extract with 1500kg The second extraction was carried out for another 20 hours, the two extracts were combined and filtered, and 4400kg of the filtrate flowed through the ADS-17 resin adsorption column for three hours, followed by washing the column with 6000kg of tap water and 1000kg of deionized water, followed by washing with 70% ethanol After the ethanol eluate was concentrated to 20kg, it was freeze-dried to obtain 4.81kg of the product.

[0085] Test results: total flavonoid glycosides 36.0%, total terpene lactones 12.8%, proanthocyanidins 12.5%, ginkgolic acid 2...

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Abstract

The present invention is extractant, extraction process and analysis method of high-activity ginkgo leaf extractive. The key point of the present invention is one developed extractant for water extraction process of ginkgetin and EGb and the process has no step of eliminating ginkolic acid. These also includes one efficient liquid-phase chromatographic method for the quantitative analysis of ginkolic acid with secondary chemical balance. The product contains total flavone glycoside 24-32%, total terpenoid lactone 6-13%, protocyanidine 8-14% and ginkolic acid less than 5 ppm, and has yield of 2.8-3.6%. The extractant has low cost, small consumption, no residue, high stripping rate of flavones, terpenoid lactones and protocyanidin compound and has stripping of ginkolic acid.

Description

technical field [0001] The invention belongs to the technical field of natural product extraction, and the invention relates to an extraction agent and a water extraction method for producing ginkgo leaf extract by using ginkgo leaves as raw materials, and includes a method for quantitatively analyzing the content of ginkgophenolic acid. Background technique [0002] Ginkgo biloba extract has been used in treatment for more than 30 years. At present, there are many medicines and health foods with ginkgo biloba extract as the main ingredient in the domestic and foreign markets, such as Tianbaoning, Ginkgo, Tanakan, Tebonin, Ginkgo tea, etc. , is an effective plant medicine for the prevention and treatment of cardiovascular and nervous system diseases. The ginkgo leaf extract that is used for the above-mentioned purpose is characterized in that it contains 22%-27% flavonoid glycosides, 5%-7% terpene lactones (gingkolide A, B, C 2.8%-3.4%; bilobalid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C07B63/00C07C51/48C07C65/03C07D493/22C07H1/08C07H17/04
Inventor 胡慰望谢笔钧杨尔宁何静仁
Owner HUAZHONG AGRI UNIV
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