CN1172669A - Method for extracting and separating flavone and terlactone from ginkgo leaf by supercritical carbon dioxide - Google Patents

Abstract

A process for extracting and separation gingko flavone and gingko terpene lactone from ginko leaves by means of supercritical CO2 features that the composition of alcohol (3-7%) and water (93-97%) is used as polar modifier and dynamic extraction takes place at 50-60 deg. C and 25-35 MPa for 3-5 hr dynamically. The substance discharged from extractor contains gingko flavone up to 22-26%, and the substance output from separator contains gingko terpene lactone up to 85-90%.

Description

The method of supercritical carbon dioxide extract and separate flavone and terpene lactones from Folium Ginkgo

The present invention relates to a kind of method that adopts supercritical CO 2 extract and separate ginkgetin class and Folium Ginkgo terpene lactones class from Folium Ginkgo.

As everyone knows, the ginkgetin class and the Folium Ginkgo terpene lactones class mixture that from Folium Ginkgo, extract at present, mostly be to adopt the chemical solvent method, its shortcoming is that solvent-oil ratio is big, flow process is numerous and diverse and extraction yield is extremely low, the former is effective especially for the treatment cardiovascular diseases, and therefore the latter then evident in efficacy for the treatment cerebrovascular, how to work out one-step extracting and isolate this two component the problem that is current the world of medicine.

The object of the present invention is to provide the super CO that faces of a kind of employing ₂From Folium Ginkgo one-step extracting and isolate ginkgetin class (as trihydroxyflavone alcohol Kaempferol etc.) and the Folium Ginkgo terpene lactones class as the method for (as Ginkgolides).

This embodiment is as follows: add in extraction process and with 3-7% ethanol and 93-97% aqueous polar modifier strong polar ginkgetin class is not extracted to stay in the extraction kettle, semipolar Folium Ginkgo terpene lactones class then can be extracted, and separates from separator.Its extraction process condition is:

Folium Ginkgo is packed in the extraction kettle, be warmed up to 50-60 ℃, start CO ₂Pump boosts to the 25-35 MPa, starts the modifier pump and makes CO ₂Preheating in preheater enters extraction kettle again with modifier, dynamic extraction 3-5 hour, left alone without help pump blood pressure lowering, emits the extract that contains the ginkgetin class, the separating medium of emitting the Folium Ginkgo terpene lactones class in separator in extraction kettle.

Following preference is described in detail the present invention, but does not mean that limitation of the scope of the invention in conjunction with flow chart.

Example 1, the Semen Ginkgo pyrite class that contains that will clean airing are 7 kilograms of 1% Folium Ginkgos, put into general extraction kettle, be warmed up to 58 ℃, start CO ₂Pump, boost to 30 MPas, with flow velocity be 30 liters/time, be preheating to 58 ℃ by preheater, start the modifier pump simultaneously, with flow velocity be 1.5 liters/time send 5% ethanol, the modifier that 95% water is formed is also by preheater and be preheating to 58 ℃, and these two bursts of logistics are all by extractor and two placed in-line separators, gaseous state CO ₂Be condensed into the liquid recirculation by refrigerator and return CO ₂Pump, dynamic extraction be after 4 hours, termination of pumping, emits to contain 6.6 kilograms of ginkgetin class raffinate and respectively emit the 0.4 kilogram of analysis result of extract that contains Folium Ginkgo terpene lactones class mixture from 2 series connection separators from extractor and see Table 1

Table 1

	Extraction kettle			Separating still
						Example	Folium Ginkgo weight (kilogram) before the extraction	Extraction back raffinate weight (kilogram)	Raffinate contains flavone %	Extract weight (kilogram)	Contain terpene lactones %
1	????7.0	????6.6	????26	????0.4	????90
						2	????7.0	????6.4	????24	????0.6	????85

Example 2, remove extraction temperature and change 52 ℃ into, extracting pressure changes 25 MPas into, it is that 3% water is to change into outside 3 hours 97% compositions and extraction time that modifier changes ethanol into, and all the other conditions are identical with example 1, each gets 6.4 kilograms of the apricot yellow ketone raffinate of argentiferous and contains 0.6 kilogram of Semen Ginkgo terpene lactones extract.Analysis result also sees Table 1.

Advantage of the present invention is:

1, the short separating rate of flow process is fast, and yield is high.

2, extraction, thing argentiferous flavonoids be up to more than 22%, and lactone content is below 0.01%, high this 85-90% of extract composition containing ginkgo terpene lactones class in the separator. Fig. 1: the 1.CO2 high-pressure pump, 2. modifier pump, 3. preheater, 4. extraction still,

5. separating still, 6. separating still, 7. refrigerator

Claims (2)

1, a kind of method that adopts supercritical carbon dioxide extract and separate ginkgetin class and Folium Ginkgo terpene lactones class from Folium Ginkgo, it is characterized in that: Folium Ginkgo is packed in the extraction kettle, be warmed up to 50-60 ℃, start carbon dioxide pump, boost to the 25-35 MPa, start modifier and pump out modifier, make the preheating and send into extraction kettle in preheater of carbon dioxide and modifier, dynamic extraction 3-5 hour, termination of pumping, blood pressure lowering, emit from extraction kettle and to contain ginkgetin class raffinate and in separator, to emit Folium Ginkgo terpene lactones class extract.

2, according to the method for claim 1, it is characterized in that: following extraction conditions is the best,

A, extraction temperature are 58 ℃, and extracting pressure is 30 MPas, and the extraction time is 4 hours

B, modifier contain 5% ethanol, the compositions of 95% water.

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