Process for extraction and separation of ginkgolides A, B, C, J, M and bilobalide

Abstract

The invention discloses a process for extraction and separation of ginkgolides A, B, C, J, M and bilobalide. The process comprises the following steps of: utilizing ginkgo leaves or gingko tree root skin as a raw material; extracting with weakly alkaline water as a solvent; concentrating, filtering and neutralizing extract; filling filtrate in polyamide column; collecting effluent; eluting the polyamide column with water; combining eluate with the effluent on macroporous resin column; eluting with ethanol; concentrating to small size; and separating in steps and crystallizing, wherein rough crystals are recrystallized by using ethanol, methanol and the like to obtain ginkgolides A, B, C, J, M and bilobalide monomer respectively; through HPLC (High Performance Liquid Chromatography) detection, the purity of the ginkgolides A, B, C and the bilobalide can reach 98 percent, and the purity of the ginkgolides J, M can reach 97.5 percent. The process has the advantages of simplicity, low cost and high yield.

Description

[0001] technical field

[0002] The invention relates to a method for extracting and separating effective monomers of traditional Chinese medicines, more specifically a process for extracting and separating ginkgolides A, B, C, J, M and bilobalide from ginkgo leaves or ginkgo root bark.

[0003] Background technique

[0004] One of the main functions of ginkgolides is to inhibit a substance called platelet activating factor (PAF), a mediator released from cells that causes platelets to aggregate (pilk together). High levels of PAF can lead to Nerve cell damage, decreased blood flow to the central nervous system, inflammation, and bronchoconstriction. Much like free radicals, high PAF levels can also lead to aging. Ginkgolides and bilobalides can Protect the nerve cells of the central nervous system from damage. This feature may be useful as an adjunct therapy for patients suffering from stroke. In addition to inhibiting platelet adhesion, Ginkgo extract regulates blood ve...

Examples

Embodiment 1

[0024] Ginkgo biloba as raw material

[0025] Take 200 kg of ginkgo leaves, add 2000 kg of weakly alkaline water (PH=8), heat and boil for 3 hours, filter, add 2000 kg of weakly alkaline water to the residue, heat and boil for 3 hours, filter, combine the filtrate, dilute Hydrochloric acid was neutralized to neutral, concentrated under reduced pressure to 1 / 3 volume, stood still for 8 hours, centrifuged, the supernatant was put on a polyamide resin column, and the effluent was collected, and the column was eluted with deionized water 3 times the volume of the column. The effluent and water eluate are put on a macroporous resin column, the column is first washed with water, and then eluted with 1000 liters of 80% ethanol (the amount of ethanol added is 3-5 times the volume of the column), and the ethanol eluate is concentrated under reduced pressure to 12 Liter (the ethanol eluate is concentrated to a volume-to-weight ratio of 1 / 15 to 1 / 25 of Ginkgo biloba, that is, 15KG crude ...

Embodiment 2

[0028] Ginkgo biloba root bark as raw material

[0029] Take 100 kg of ginkgo root bark, add 1000 kg of weak alkaline water (PH=8), heat and extract for 3 hours, filter, continue to add 1000 kg of weak alkaline water to the residue, heat and extract for 3 hours, filter, combine the filtrate, dilute hydrochloric acid Neutralize to neutral, concentrate under reduced pressure to 1 / 3 volume, let stand for 8 hours, centrifuge, put the supernatant on a polyamide resin column, collect the effluent, elute the column with deionized water 3 times the volume of the column, and flow out liquid and water eluent on the macroporous resin column, the column was washed with water earlier, and then eluted with 1000 liters of 80% ethanol, and the ethanol eluent was concentrated to 12 liters under reduced pressure (the ethanol eluent was concentrated to the volume and weight of Ginkgo biloba The ratio is 1 / 15 to 1 / 25, that is, 15KG crude drug - Ginkgo biloba, ethanol eluate is concentrated to 1 l...

[0001] technical field

[0002] The invention relates to a method for extracting and separating effective monomers of traditional Chinese medicines, more specifically a process for extracting and separating ginkgolides A, B, C, J, M and bilobalide from ginkgo leaves or ginkgo root bark.

[0003] Background technique

[0004] One of the main functions of ginkgolides is to inhibit a substance called platelet activating factor (PAF), a mediator released from cells that causes platelets to aggregate (pilk together). High levels of PAF can lead to Nerve cell damage, decreased blood flow to the central nervous system, inflammation, and bronchoconstriction. Much like free radicals, high PAF levels can also lead to aging. Ginkgolides and bilobalides can Protect the nerve cells of the central nervous system from damage. This feature may be useful as an adjunct therapy for patients suffering from stroke. In addition to inhibiting platelet adhesion, Ginkgo extract regulates blood ve...

Examples

Embodiment 1

[0024] Ginkgo biloba as raw material

[0025] Take 200 kg of ginkgo leaves, add 2000 kg of weakly alkaline water (PH=8), heat and boil for 3 hours, filter, add 2000 kg of weakly alkaline water to the residue, heat and boil for 3 hours, filter, combine the filtrate, dilute Hydrochloric acid was neutralized to neutral, concentrated under reduced pressure to 1 / 3 volume, stood still for 8 hours, centrifuged, the supernatant was put on a polyamide resin column, and the effluent was collected, and the column was eluted with deionized water 3 times the volume of the column. The effluent and water eluate are put on a macroporous resin column, the column is first washed with water, and then eluted with 1000 liters of 80% ethanol (the amount of ethanol added is 3-5 times the volume of the column), and the ethanol eluate is concentrated under reduced pressure to 12 Liter (the ethanol eluate is concentrated to a volume-to-weight ratio of 1 / 15 to 1 / 25 of Ginkgo biloba, that is, 15KG crude ...

Embodiment 2

[0028] Ginkgo biloba root bark as raw material

[0029] Take 100 kg of ginkgo root bark, add 1000 kg of weak alkaline water (PH=8), heat and extract for 3 hours, filter, continue to add 1000 kg of weak alkaline water to the residue, heat and extract for 3 hours, filter, combine the filtrate, dilute hydrochloric acid Neutralize to neutral, concentrate under reduced pressure to 1 / 3 volume, let stand for 8 hours, centrifuge, put the supernatant on a polyamide resin column, collect the effluent, elute the column with deionized water 3 times the volume of the column, and flow out liquid and water eluent on the macroporous resin column, the column was washed with water earlier, and then eluted with 1000 liters of 80% ethanol, and the ethanol eluent was concentrated to 12 liters under reduced pressure (the ethanol eluent was concentrated to the volume and weight of Ginkgo biloba The ratio is 1 / 15 to 1 / 25, that is, 15KG crude drug - Ginkgo biloba, ethanol eluate is concentrated to 1 l...

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