Summary of the invention
First technical problem to be solved by this invention is the preparation method of the Ramulus et folium taxi cuspidatae Extract providing a kind of dissolution rate effectively to improve for the state of the art.
Second technical problem to be solved by this invention is to provide a kind of application of Ramulus et folium taxi cuspidatae Extract.
The present invention solves the technical scheme that above-mentioned first technical problem adopt: a kind of preparation method of Ramulus et folium taxi cuspidatae Extract, comprises the steps:
(1) Ramulus et folium taxi cuspidatae raw material is prepared;
(2) ultrasonication process, stirs immersion by Ramulus et folium taxi cuspidatae raw material, obtains soak in soaking agent, carries out ultrasonication process, obtain feed liquid to described soak;
(3) enzymolysis, described feed liquid is gone in reaction vessel, the neutral protease accounting for Ramulus et folium taxi cuspidatae raw material weight 0.3% ~ 1.0% (such as 0.5%, 0.7%, 0.8%) is added in described reaction vessel, obtain mixed liquor, regulate pH to 6.8 ~ 7.0 of mixed liquor, enzymolysis makes the free protein in glycoprotein and polysaccharide be hydrolyzed, and enzyme denaturing, obtains serosity;
(4) carry out reflux, extract, process to described serosity, obtain extracting solution, filter, concentrate, obtain concentrated solution, concentrated solution filters, and obtains filtrate;
(5) spraying dry, obtains Ramulus et folium taxi cuspidatae Extract.
Wherein, the operating process of step (1) is, branch of Ramulus et folium taxi cuspidatae and/or leaf are dried, pulverized, and cross 60 ~ 80 mesh sieves, siftage is Ramulus et folium taxi cuspidatae raw material.Wherein, Ramulus et folium taxi cuspidatae is preferably artificially-induced bezoar.
Wherein, in step (2), stirring the operating process of soaking is, Ramulus et folium taxi cuspidatae raw material is dropped in ultrasonication pot for solvent extraction, add the soaking agent of Ramulus et folium taxi cuspidatae raw material weight 10 ~ 20 times, stir under 45 DEG C ~ 55 DEG C (such as 48 DEG C, 50 DEG C, 52 DEG C) and soak 1h ~ 1.5h (such as 1.2h, 1.3h, 1.4h);
Preferred soaking agent is water.
Wherein, in step (2), supersonic generator is adopted to carry out ultrasonication process, the power of described ultrasonic generator is 15 ~ 30KW, such as 18KW, 20KW, 25KW, 28KW, and frequency is 20 ~ 25KHz, such as 22 KHz, 23KHz, 24KHz, the sound intensity is 2 ~ 5W/cm
2, the time of ultrasonication process is 20 ~ 60min, such as 30min, 40min, 50min.
Wherein, in step (3), described reaction vessel is for stirring extraction pot;
Preferably, enzymolysis time is 80min ~ 100min, such as 85min, 90min, 95min;
Preferably, enzyme-removal temperature is 85 ~ 95 DEG C, such as 88 DEG C, 90 DEG C, 92 DEG C, and the enzyme denaturing time is 10min ~ 15min, such as 12min, 13min, 14min.
Wherein, in step (4), the operating process of described reflux, extract, process is, is gone to by described serosity in reflux, extract, tank, reflux, extract, 3 ~ 5h under 85 ~ 95 DEG C (such as 88 DEG C, 90 DEG C, 92 DEG C);
Preferably, in step (4), the operating process of described filtration is, described extracting solution is by plate-and-frame filtration or microporous filter, filtering order number is 120 ~ 200 orders (such as 150 orders, 170 orders, 190 orders), and filter pressure is 0.3 ~ 0.6MPa, such as 0.4MPa, 0.5MPa;
Preferably, in step (4), described concentrated operating process is that the supernatant obtained after described extracting liquid filtering pumps in concentrating under reduced pressure tank, and being evaporated to concentration is 10% ~ 20%, such as 12%, 15%, 17%.
Wherein, after step (4), also comprise step (4a) before step (5), after described concentrated solution filters, with diluent, filtrate being adjusted to concentration is 12% ~ 18%, such as 13%, 15%, 17%.
Wherein, described diluent is water.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: the Ramulus et folium taxi cuspidatae Extract prepared according to above-mentioned preparation method is preparing the application in antitumor, diabetes, raising immunity, adjusting blood lipid level, blood pressure lowering, treatment rheumatism, prevention medicaments for coronary disease.
Wherein, the form of described medicine is tablet, capsule or granule.
Compared with prior art, the invention has the advantages that: the method that preparation method adopts ultrasonication, bio-enzyme degradation combines with reflux, extract, of this Ramulus et folium taxi cuspidatae Extract, remain effective ingredient, degradation biological macromole, improve dissolution rate, reduce process procedure, capable of reducing energy consumption, accelerate extraction rate.Adopt this preparation method can provide a kind of goods close to China's Traditional Chinese Medicine clinical application medicine component, i.e. Ramulus et folium taxi cuspidatae Extract, these goods can directly be applied, and also can be used as the Ramulus et folium taxi cuspidatae raw material extracting monomer further.The further exploitation of the present invention to artificial growth taxus resource has positive effect.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1
The preparation method of the Ramulus et folium taxi cuspidatae Extract of the present embodiment, comprises the steps:
(1) prepare Ramulus et folium taxi cuspidatae raw material, branch of Ramulus et folium taxi cuspidatae and leaf are dried, are pulverized, and cross 80 mesh sieves, siftage is Ramulus et folium taxi cuspidatae raw material, for subsequent use.
(2) ultrasonication process, extracting screen underflow, i.e. Ramulus et folium taxi cuspidatae raw material 10kg, drop in ultrasonication pot for solvent extraction, add soaking agent---the water of Ramulus et folium taxi cuspidatae raw material weight 15 times, stirs and soak 1h at 50 DEG C; Adopt supersonic generator to carry out ultrasonication process, the power of ultrasonic generator is 15 ~ 30KW, such as 20KW, and frequency is 20 ~ 25KHz, such as 23KHz, and the sound intensity is 2W/cm
2, ultrasonication process 30min, obtains feed liquid.
(3) enzymolysis, feed liquid is gone to reaction vessel---namely stir in extraction pot, add the neutral protease accounting for Ramulus et folium taxi cuspidatae raw material weight 0.3%, obtain mixed liquor, regulate pH to 6.8 ~ 7.0 of mixed liquor, such as 6.8, enzymolysis 90 minutes, makes the free protein in glycoprotein and polysaccharide be hydrolyzed, is warming up to 90 DEG C, enzyme denaturing 10 minutes, obtains serosity;
(4) proceeded to by serosity in reflux, extract, tank, reflux, extract, 3 hours at 90 DEG C, the extracting solution of acquisition is by plate-and-frame filtration (also can adopt microporous filter), filtering order number is 150 orders, filter pressure is 0.3 ~ 0.6MPa, such as 0.5MPa, filters the filtering residue obtained and separately uses it for anything else, and the supernatant that filtration obtains pumps in concentrating under reduced pressure tank, be evaporated to concentration 18% ~ 20%, such as 18%, obtain concentrated solution, concentrated solution filters, and obtains filtrate;
(5), after the concentrated solution that step (4) obtains filters, filtrate Direct spraying is dry, obtains Ramulus et folium taxi cuspidatae Extract 1.42kg.
The present embodiment also can increase step (4a) before step (5) after step (4), namely after concentrated solution filters, with diluent---it is 12% ~ 18% that filtrate is adjusted to concentration by water, such as 13%, obtain fluid extract, and then spraying dry, also can obtain Ramulus et folium taxi cuspidatae Extract.
Ramulus et folium taxi cuspidatae Extract prepared by the present embodiment contains the multiple water soluble ingredients with biological function such as flavone, polysaccharide, oligosaccharide, small molecular protein, peptide, aminoacid, the medicine of antitumor, diabetes, raising immunity, adjusting blood lipid level, blood pressure lowering, treatment rheumatism, prevention coronary heart disease can be used for preparing with this Ramulus et folium taxi cuspidatae Extract, as medicine or health product, the form of medicine is tablet, capsule or granule.
Embodiment 2
The preparation method of the Ramulus et folium taxi cuspidatae Extract of the present embodiment, comprises the steps:
(1) prepare Ramulus et folium taxi cuspidatae raw material, branch of Ramulus et folium taxi cuspidatae and leaf are dried, are pulverized, and cross 80 mesh sieves, siftage is Ramulus et folium taxi cuspidatae raw material, for subsequent use.
(2) ultrasonication process, extracting screen underflow, i.e. Ramulus et folium taxi cuspidatae raw material 10kg, drop in ultrasonication pot for solvent extraction, add soaking agent---the water of Ramulus et folium taxi cuspidatae raw material weight 15 times, stirs and soak 1h at 50 DEG C; Adopt supersonic generator to carry out ultrasonication process, the power of ultrasonic generator is 15 ~ 30KW, such as 15KW, and frequency is 20 ~ 25KHz, such as 20KHz, and the sound intensity is 2W/cm
2, ultrasonication process 40min, obtains feed liquid.
(3) enzymolysis, goes to reaction vessel by feed liquid---and namely stir in extraction pot, add the neutral protease accounting for Ramulus et folium taxi cuspidatae raw material weight 0.5%, obtain mixed liquor, regulate pH to 6.8 ~ 7.0 of mixed liquor, such as 6.9; Enzymolysis 90 minutes, the free protein in glycoprotein and polysaccharide is hydrolyzed, and be warming up to 90 DEG C, enzyme denaturing 10 minutes, obtains serosity;
(4) serosity is proceeded in reflux, extract, tank, reflux, extract, 4 hours at 90 DEG C, the extracting solution of acquisition is by plate-and-frame filtration (also can adopt microporous filter), and filtering order number is 150 orders, filter pressure is 0.3 ~ 0.6MPa, such as 0.4MPa, filters the filtering residue obtained and separately use it for anything else, and the supernatant that filtration obtains pumps in concentrating under reduced pressure tank, be evaporated to concentration 18% ~ 20%, such as 19%, obtain concentrated solution, concentrated solution filters;
(5), after the concentrated solution that step (4) obtains filters, filtrate Direct spraying is dry, obtains Ramulus et folium taxi cuspidatae Extract 1.32kg.
The present embodiment also can increase step (4a) before step (5) after step (4), namely after concentrated solution filters, with diluent---it is 12% ~ 18% that filtrate is adjusted to concentration by water, such as 16%, obtain fluid extract, and then spraying dry, also can obtain Ramulus et folium taxi cuspidatae Extract.
Ramulus et folium taxi cuspidatae Extract prepared by the present embodiment contains the multiple water soluble ingredients with biological function such as flavone, polysaccharide, oligosaccharide, small molecular protein, peptide, aminoacid, the medicine of antitumor, diabetes, raising immunity, adjusting blood lipid level, blood pressure lowering, treatment rheumatism, prevention coronary heart disease can be used for preparing with this Ramulus et folium taxi cuspidatae Extract, as medicine or health product, the form of medicine is tablet, capsule or granule.
Embodiment 3
The preparation method of the Ramulus et folium taxi cuspidatae Extract of the present embodiment, comprises the steps:
(1) prepare Ramulus et folium taxi cuspidatae raw material, branch of Ramulus et folium taxi cuspidatae and leaf are dried, are pulverized, and cross 80 mesh sieves, siftage is Ramulus et folium taxi cuspidatae raw material, for subsequent use.
(2) ultrasonication process, extracting screen underflow, i.e. Ramulus et folium taxi cuspidatae raw material 10kg, drop in ultrasonication pot for solvent extraction, add soaking agent---the water of Ramulus et folium taxi cuspidatae raw material weight 15 times, stirs and soak 1h at 50 DEG C; Adopt supersonic generator to carry out ultrasonication process, the power of ultrasonic generator is 15 ~ 30KW, such as 30KW, and frequency is 20 ~ 25KHz, such as 25KHz, and the sound intensity is 3W/cm
2, ultrasonication process 30min, obtains feed liquid.
(3) enzymolysis, feed liquid is gone to reaction vessel---namely stir in extraction pot, add the neutral protease accounting for Ramulus et folium taxi cuspidatae raw material weight 0.8%, obtain mixed liquor, regulate pH to 6.8 ~ 7.0 of mixed liquor, such as 7.0, enzymolysis 90 minutes, makes the free protein in glycoprotein and polysaccharide be hydrolyzed, is warming up to 90 DEG C, enzyme denaturing 10 minutes, obtains serosity;
(4) serosity is proceeded in reflux, extract, tank, reflux, extract, 5 hours at 90 DEG C, the extracting solution of acquisition is by plate-and-frame filtration (also can adopt microporous filter), and filtering order number is 150 orders, filter pressure is 0.3 ~ 0.6MPa, such as 0.5MPa, filters the filtering residue obtained and separately use it for anything else, and the supernatant that filtration obtains pumps in concentrating under reduced pressure tank, be evaporated to concentration 18% ~ 20%, such as 20%, obtain concentrated solution, concentrated solution filters;
(5), after the concentrated solution that step (4) obtains filters, filtrate Direct spraying is dry, obtains Ramulus et folium taxi cuspidatae Extract 1.45kg.
Ramulus et folium taxi cuspidatae Extract prepared by the present embodiment contains the multiple water soluble ingredients with biological function such as flavone, polysaccharide, oligosaccharide, small molecular protein, peptide, aminoacid, the medicine of antitumor, diabetes, raising immunity, adjusting blood lipid level, blood pressure lowering, treatment rheumatism, prevention coronary heart disease can be used for preparing with this Ramulus et folium taxi cuspidatae Extract, as medicine or health product, the form of medicine is tablet, capsule or granule.
Embodiment 4
The present embodiment difference from Example 3 is:
Step (4a) is also comprised before step (5), after concentrated solution filters, with diluent after step (4)---it is 12% ~ 18% that filtrate is adjusted to concentration by water, such as 15%, obtain fluid extract, and then spraying dry, also can obtain Ramulus et folium taxi cuspidatae Extract.
Other preparation process are as embodiment 3, and its concrete process chart is shown in Fig. 1.
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.