Summary of the invention
The object of the present invention is to provide a kind of preparation method of Radix Berberidis Amurensis berry extract.
The present invention is achieved through the following technical solutions:
The present invention is raw materials used: Radix Berberidis Amurensis is really the dry mature fruit of Berberidaceae plant Berberis nummularia Bge. Berberis nummularia Bge..
The preparation method of a kind of Radix Berberidis Amurensis berry extract of the present invention, is characterized in that preparing according to the following steps:
(1) Radix Berberidis Amurensis fruit, uses concentration 0-30% ethanol as solvent, extracts temperature 50 C-95 ℃, and extraction time is 1-3 time, and each extraction time is 1-4 hour, and each solvent load is 6-15 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.10-1.18, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, pass through nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by polar macroporous resin, use again the alcoholic solution eluting nonpolar macroporous adsorption resin of concentration 30%-70%, collect different concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting polar macroporous adsorption resin of concentration 50%-95% again, collect different concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
A preparation method for Radix Berberidis Amurensis berry extract, is characterized in that preparing according to the following steps:
(1) Radix Berberidis Amurensis fruit, as solvent, extracts temperature 70 C with concentration 20% ethanol, and extraction time is 3 times, and each extraction time is 3 hours, and each solvent load is 14 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.12, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by D101 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of LSA-40, use again the alcoholic solution eluting D101 nonpolar macroporous adsorption resin of concentration 50%, collect 50% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting LSA-40 polar macroporous adsorption resin of concentration 80% again, collect 80% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
A preparation method for Radix Berberidis Amurensis berry extract, is characterized in that preparing according to the following steps:
(1), by Radix Berberidis Amurensis fruit, water is as solvent, heating and refluxing extraction, and extraction time is 2 times, and each extraction time is 2 hours, and each solvent load is 12 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.12, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by D101 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of LSA-40, use again the alcoholic solution eluting D101 nonpolar macroporous adsorption resin of concentration 50%, collect 50% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting LSA-40 polar macroporous adsorption resin of concentration 80% again, collect 80% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
The preparation method of a kind of Radix Berberidis Amurensis berry extract of the present invention, is characterized in that: described Radix Berberidis Amurensis berry extract mainly contains: berberine, jateorhizine, palmatine, magnoflorine, pelargonidin, enidin.
The preparation method of a kind of Radix Berberidis Amurensis berry extract of the present invention, is characterized in that: the nonpolar macroporous adsorption resin adopting is D101 macroporous adsorbent resin, AB-8 macroporous adsorbent resin; The polar macroporous adsorption resin adopting is LSA-40 macroporous resin, HPD600 macroporous resin.
Radix Berberidis Amurensis berry extract of the present invention, by the various adjuvants that add pharmaceutics to allow, makes the peroral dosage forms such as tablet on pharmaceutics, granule, capsule.
The specific embodiment
Below by specific experiment example and embodiment, the preparation method of a kind of Radix Berberidis Amurensis berry extract of the present invention is described further, but is not limited to the present invention.
Below by specific embodiment, be described in further detail.
Embodiment 1: the preparation of Radix Berberidis Amurensis berry extract and monomer component research
(1) Radix Berberidis Amurensis fruit 20kg, water is as solvent, heating and refluxing extraction, extraction time is 2 times, and each extraction time is 2 hours, and each solvent load is 12 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.12, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by D101 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of LSA-40, use again the alcoholic solution eluting D101 nonpolar macroporous adsorption resin of concentration 50%, collect 50% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting LSA-40 polar macroporous adsorption resin of concentration 80% again, collect 80% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
Radix Berberidis Amurensis berry extract carries out silica gel column chromatography, Preparative TLC chromatograph and Sephadex LH mono-2O column chromatography, obtains respectively sloughing off berberine, jateorhizine, palmatine, magnoflorine, pelargonidin, enidin.The chemical constitution of each compound is all through wave spectrum means confirmations such as mass spectrum and nuclear magnetic resonance, NMR above, and purity detects and is all greater than 98% through high performance liquid chromatography.
Embodiment 2: the preparation of Radix Berberidis Amurensis berry extract and monomer component research
(1) Radix Berberidis Amurensis fruit 15kg, as solvent, extracts temperature 70 C with concentration 20% ethanol, and extraction time is 3 times, and each extraction time is 3 hours, and each solvent load is 14 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.12, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by D101 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of LSA-40, use again the alcoholic solution eluting D101 nonpolar macroporous adsorption resin of concentration 50%, collect 50% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting LSA-40 polar macroporous adsorption resin of concentration 80% again, collect 80% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
Radix Berberidis Amurensis berry extract carries out silica gel column chromatography, Preparative TLC chromatograph and Sephadex LH mono-2O column chromatography, obtains respectively sloughing off berberine, jateorhizine, palmatine, magnoflorine, pelargonidin, enidin.The chemical constitution of each compound is all through wave spectrum means confirmations such as mass spectrum and nuclear magnetic resonance, NMR above, and purity detects and is all greater than 98% through high performance liquid chromatography.
Embodiment 3: the preparation of Radix Berberidis Amurensis berry extract and monomer component research
(1) Radix Berberidis Amurensis fruit 30kg, as solvent, extracts temperature 50 C with concentration 30% ethanol, and extraction time is 1 time, and each extraction time is 4 hours, and each solvent load is 15 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.18, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by AB-8 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of HPD600, use again the alcoholic solution eluting AB-8 nonpolar macroporous adsorption resin of concentration 70%, collect 70% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting HPD600 polar macroporous adsorption resin of concentration 95% again, collect 95% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
Radix Berberidis Amurensis berry extract carries out silica gel column chromatography, Preparative TLC chromatograph and Sephadex LH mono-2O column chromatography, obtains respectively sloughing off berberine, jateorhizine, palmatine, magnoflorine, pelargonidin, enidin.The chemical constitution of each compound is all through wave spectrum means confirmations such as mass spectrum and nuclear magnetic resonance, NMR above, and purity detects and is all greater than 98% through high performance liquid chromatography.
Embodiment 4: the preparation of Radix Berberidis Amurensis berry extract and monomer component research
(1) Radix Berberidis Amurensis fruit 15kg, as solvent, extracts 95 ℃ of temperature with concentration 5% ethanol, and extraction time is 3 times, and each extraction time is 1 hour, and each solvent load is 6 times of Radix Berberidis Amurensis fruit weight; Filter, merge extractive liquid,, reclaims ethanol, is concentrated into relative density d=1.10, filters, and obtains medicinal liquid A;
(2) medicinal liquid A step (1) being obtained, by D101 nonpolar macroporous adsorption resin, first wash with water, water elution liquid is directly by the polar macroporous resin of LSA-40, use again the alcoholic solution eluting D101 nonpolar macroporous adsorption resin of concentration 30%, collect 30% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract A; Use the alcoholic solution eluting LSA-40 polar macroporous adsorption resin of concentration 50% again, collect 50% concentration ethanol eluent, concentrate drying, obtains Radix Berberidis Amurensis berry extract B;
(3) above-mentioned Radix Berberidis Amurensis berry extract A and Radix Berberidis Amurensis berry extract B are mixed, obtain Radix Berberidis Amurensis berry extract of the present invention.
Radix Berberidis Amurensis berry extract carries out silica gel column chromatography, Preparative TLC chromatograph and Sephadex LH mono-2O column chromatography, obtains respectively sloughing off berberine, jateorhizine, palmatine, magnoflorine, pelargonidin, enidin.The chemical constitution of each compound is all through wave spectrum means confirmations such as mass spectrum and nuclear magnetic resonance, NMR above, and purity detects and is all greater than 98% through high performance liquid chromatography.
Embodiment 5: the preparation of Radix Berberidis Amurensis berry extract tablet
Get embodiment 1 Radix Berberidis Amurensis berry extract 235g, add starch 45g, mix, granulate, dry, sieve, add microcrystalline Cellulose 35g, magnesium stearate 3.5g, mixes, and is pressed into 1000, obtains Radix Berberidis Amurensis berry extract tablet.
Embodiment 6: the preparation of Radix Berberidis Amurensis berry extract granule
Get embodiment 2 Radix Berberidis Amurensis berry extract 265g, add dextrin 50g, sucrose 50g, mixes, and granulates, and dry, granulate, obtains Radix Berberidis Amurensis berry extract granule.
Embodiment 7: the preparation of Radix Berberidis Amurensis berry extract capsule
Get embodiment 3 Radix Berberidis Amurensis berry extract 225g, add starch 65g, mix, granulate, dry, granulate,, obtains Radix Berberidis Amurensis berry extract capsule by encapsulated 1000.