CN1460684A - Epimedium extract and its production method - Google Patents
Epimedium extract and its production method Download PDFInfo
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- 235000020696 epimedium extract Nutrition 0.000 title abstract 2
- 238000004519 manufacturing process Methods 0.000 title description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 212
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011347 resin Substances 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- 235000018905 epimedium Nutrition 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000003814 drug Substances 0.000 claims abstract description 16
- 239000003480 eluent Substances 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- 241000893536 Epimedium Species 0.000 claims abstract description 10
- 208000001132 Osteoporosis Diseases 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 70
- 239000000284 extract Substances 0.000 claims description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- 229930003944 flavone Natural products 0.000 claims description 35
- 235000011949 flavones Nutrition 0.000 claims description 35
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims description 35
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims description 34
- TZJALUIVHRYQQB-XFDQAQKOSA-N Icariin Natural products O(C)c1ccc(C2=C(O[C@H]3[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)C(=O)c3c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O4)c(C/C=C(\C)/C)c3O2)cc1 TZJALUIVHRYQQB-XFDQAQKOSA-N 0.000 claims description 33
- TZJALUIVHRYQQB-XLRXWWTNSA-N icariin Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-XLRXWWTNSA-N 0.000 claims description 33
- TZJALUIVHRYQQB-UHFFFAOYSA-N icariine Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(C)O2)O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-UHFFFAOYSA-N 0.000 claims description 33
- 150000002212 flavone derivatives Chemical class 0.000 claims description 31
- 238000012360 testing method Methods 0.000 claims description 31
- 239000013558 reference substance Substances 0.000 claims description 22
- 241001016310 Epimedium grandiflorum Species 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 239000012467 final product Substances 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 239000002775 capsule Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
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- 238000003556 assay Methods 0.000 claims description 6
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- 238000004587 chromatography analysis Methods 0.000 claims description 5
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- 239000007921 spray Substances 0.000 claims description 5
- YEZWWUMWIFKEQM-UHFFFAOYSA-N O.OC.ClC(Cl)Cl.CCOC(C)=O Chemical compound O.OC.ClC(Cl)Cl.CCOC(C)=O YEZWWUMWIFKEQM-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
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- 238000004064 recycling Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
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- 229910002027 silica gel Inorganic materials 0.000 claims description 4
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- 239000003826 tablet Substances 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 238000012850 discrimination method Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 description 16
- -1 flavone compound Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
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- 238000009472 formulation Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000006187 pill Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229920000858 Cyclodextrin Polymers 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000424773 Epimedium alpinum Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 235000010419 agar Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 210000002805 bone matrix Anatomy 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
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- 229920001436 collagen Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000008298 dragée Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000002662 enteric coated tablet Substances 0.000 description 1
- 230000001076 estrogenic effect Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 239000007941 film coated tablet Substances 0.000 description 1
- 150000002213 flavones Chemical group 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000007902 hard capsule Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- 229920001282 polysaccharide Polymers 0.000 description 1
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The epimedium extract which can be used for preparing medicine for curing osteoporosis is obtained by using Chinese medicinal materials epimedium through the processes of decocting in water, alcohol precipitation, macroporous resin adsorption, collecting eluent and concentrating eluent.
Description
Technical field:
The invention belongs to technical field of traditional Chinese medicine pharmacy. Particularly relate to Shorthorned Epimedium P.E and preparation technology thereof.
Background technology:
Osteoporosis be in, common complaint among the elderly, frequently-occurring disease, very good medicine is not yet arranged at present. Barrenwort is domestic traditional kidney-replenishing Chinese medicine, has history in thousand among the people continuing to use, and its main chemical compositions is flavone compound, polysaccharide, lignanoid, alkaloid and grease etc. Studies show that at present wherein active principle is flavones ingredient, carry out at compound and simple level the research of barrenwort protect against osteoporosis is many at present, in recent years, the state scholars such as U.S., day, moral pay attention to extracting natural disease-resistant medicine especially from plant, and they have successively extracted flavone compound or the derivative with function of resisting osteoporosis from legume. These compounds have estrogen-like action, thereby also are known as phytoestrogen. The mechanism of their protect against osteoporosis is got clear substantially, mainly comprises: (1) promotes osteoblastic propagation, increases the bone formation volume; (2) suppress the activity of raising of osteoclast, reduce bone and absorb level; (3) act on the bone matrix cell, promotion collagen synthesizes the mineralising with matrix.
Because barrenwort is rich in flavone compound, a kind of effective population with pharmacological action, effect by this effective population, the treatment osteoporosis had very significantly effect, but because the content of general flavone is lower in the epimedium herb, the extracting mode of barrenwort mostly is the water boiling and precipitation with ethanol method, the present invention is in conjunction with the technological means of modern pharmaceutical industry, adopted the method for macroreticular resin wash-out, improved the yield of barrenwort total extract, for the more effective treatment osteoporosis of barrenwort provides necessary assurance.
This test draws the conclusion that the technique that adopts water boiling and precipitation with ethanol and macroreticular resin wash-out to combine can improve barren wort total chromocor purity by the different process method is compared. This technique can either be adapted to suitability for industrialized production, can play the effect of giving full play to curative effect of medication again.
Summary of the invention:
The invention provides a kind of Shorthorned Epimedium P.E, make by following process, it is characterized in that, barrenwort Chinese medicine process poach, alcohol precipitation, macroporous resin adsorption is collected eluent, and concentrate eluant obtains.
Extract of the present invention, in the poach process amount of water be the medicinal material amount 10-30 doubly, decoct 2-4 time altogether, decocted 1-3 hour at every turn.
Extract of the present invention, in the alcohol precipitation process, adding be ethanol, addition makes the alcohol amount of containing of solution reach 70%, add ethanol after, left standstill 24 hours, filter, filtrate recycling ethanol is also concentrated.
Extract of the present invention, in the macroporous resin adsorption process, use be D101Type macroreticular resin (internal diameter 10cm, long 100cm), first with distilled water (3 times of amount bed volumes) wash-out, flow velocity is that 40ml/ divides, and discards water elution liquid, again with 85% ethanol (4 times of amount bed volumes) wash-out, collect eluent, Recycled ethanol also is concentrated into thick paste (relative density is 1.30-1.35,50 ℃ of surveys), drying under reduced pressure (control vacuum: 0.08Mpa; Temperature: 75-8050 ℃), be ground into fine powder, sieve, make.
The invention still further relates to the discrimination method of extract of the present invention, extract of the present invention has following feature
A. be the yellowish-brown powder; Gas is little, bitter;
B. easily molten in glacial acetic acid, 60-85% ethanol, almost insoluble in acetone and ethyl acetate;
C. get extract 0.1g, add 60% ethanol 10ml, ultrasonic processing makes dissolving, gets solution as need testing solution. Other gets barrenwort control medicinal material 1.0g, adds ethanol 15ml, and refluxing extraction 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml makes dissolving, passes through D101Type macroreticular resin (internal diameter 1.5cm, long 10cm, dress D101Type macroreticular resin 5ml, flow velocity are that 1ml/ divides), with water 15ml wash-out, discard water lotion, use again 85% ethanol 20ml wash-out, collect eluent, evaporate to dryness, residue add 85% ethanol 5ml dissolving, in contrast medicinal material solution. Get again the icariin reference substance, add methyl alcohol and make the solution that every 1ml contains 0.5mg, in contrast product solution. According to thin-layered chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VIB) test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10, lower floor's solution of placing about 4 ℃) be solvent, launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the alchlor test solution. In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color. With the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
D. extract contains the amount of general flavone with icariin (C33H
40O
15) meter, be no less than 50%.
The invention still further relates to the assay method of general flavone in the extract of the present invention, this assay method is through following steps, get the about 30mg of extract, accurately weighed, put in the 25ml measuring bottle, add 60% ethanol 20ml, ultrasonic processing makes dissolving, adds 60% ethanol to scale, shakes up, filter with miillpore filter, get solution. Accurate draw solution 0.5ml puts in the volumetric flask of 50ml, adds methyl alcohol to scale, shakes up, as need testing solution. Other gets the icariin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 10 μ g, in contrast product solution. Get respectively need testing solution and reference substance solution, take reagent as blank, (one one of Chinese Pharmacopoeia version in 2000, appendix VA) measures trap at 270nm wavelength place according to AAS, calculates, and get final product.
The invention still further relates to the pharmaceutical composition of extract of the present invention, formed by extract and the 0.1-99.9% medicine acceptable carrier of 0.1-99.9%.
Composition of the present invention, can add the medicine acceptable carrier when being prepared into medicament, described medicine acceptable carrier can be: starch, sucrose, lactose, mannitol, silicon derivative, cellulose and derivative thereof, alginates, gelatin, polyvinylpyrrolidone, glycerine, POLYSORBATE 80, agar, calcium carbonate, calcium bicarbonate, surfactant, polyethylene glycol, cyclodextrin, beta-schardinger dextrin-, phospholipid material, kaolin, talcum powder, calcium stearate, dolomol etc.
Composition of the present invention can be any pharmaceutically useful formulation, and these formulations comprise: tablet, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, oral liquid, suck agent, granule, electuary, pill, powder, paste, sublimed preparation, supensoid agent, pulvis, solution, injection, suppository, ointment, emplastrum, creme, spray, drops, patch. Preparation of the present invention, peroral dosage form preferably, as: capsule, tablet, oral liquid, granule, pill, powder, sublimed preparation, paste etc., preferably capsule.
Pharmaceutical composition of the present invention is tablet, capsule, granule, oral liquid. Composition of the present invention is determined usage and dosage according to patient's situation in use, but takes every day three times, each 1-20 agent, as: 1-20 bag or grain or sheet.
The invention still further relates to extract of the present invention or composition and prepare a kind of medicine for the treatment of osteoporosis.
Composition of the present invention is capsule, and per 1000 capsules contain the extract 100-250g of claim, and all the other are the medicine acceptable carrier.
Extract of the present invention can prepare with following methods: get epimedium herb 100kg, decoct three times, add water at every turn and be 20 times of medicinal material amount, the each decoction 2 hours merges decoction liquor, filters, filtrate is concentrated into the thick paste that relative density is 1.10-1.13 (50 ℃ of survey), let cool, add ethanol, make to contain the alcohol amount and reach 70%, left standstill 24 hours, filter, filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.18-1.20 (50 ℃ of survey), lets cool, adding distil water (identical with the medicinal material amount) makes dissolving, room temperature left standstill about 4 hours, drew supernatant, passed through D101Type macroreticular resin (internal diameter 10cm, long 100cm), with distilled water (3 times of amount bed volumes) wash-out, flow velocity is that 40ml/ divides, and discards water elution liquid, again with 85% ethanol (4 times of amount bed volumes) wash-out, collect eluent, Recycled ethanol also is concentrated into thick paste (relative density is 1.30-1.35,50 ℃ of surveys), drying under reduced pressure (control vacuum: 0.08Mpa; Temperature: 75-80 ℃), be ground into fine powder, sieve, make.
Composite preparation of the present invention can prepare by the following method
Shorthorned Epimedium P.E 200-400g
Starch is an amount of
Make 1000
Method for making: get barrenwort total extract 170g, adding starch is an amount of, and mixing incapsulates, and makes 1000, and get final product. Carried out the comparison of different process route in carrying out the technical study process, the concrete technology method is compared as follows:
| Water extraction | Ethanol (70%) is carried | Water extraction, resin elution | Ethanol (70%) is carried resin elution | Water boiling and precipitation with ethanol | The water boiling and precipitation with ethanol resin elution | |
| Medicinal material amount (g) | 200 (general flavone content 5.145 %, Icariin contents 0.5321%) | 200 (general flavone content 5.145 %, Icariin contents 0.5321%) | 200 (general flavone content 5.145 %, Icariin contents 0.5321%) | 200 (general flavone content 5.145 %, Icariin contents 0.5321%) | 500 (general flavone content 5.375 %, Icariin contents 0.5416%) | 500 (general flavone content 5.375 %, Icariin contents 0.5416%) |
| The preparation method | Extract 3 times, each 2 hours, make dry extract | Extract 3 times, each 2 hours, make dry extract | Extract 3 times, each 2 hours, make medicinal extract, again by macroreticular resin, with ethanol (90 %) wash-out, make dry extract | Extract 3 times, each 2 hours, make medicinal extract, again by macroreticular resin, with ethanol (90 %) wash-out, make dry extract | Water extracts 3 times, and each 2 hours, merging filtrate with 70 % ethanol static 24 hours, was made dry extract again | Water extracts 3 times, and each 2 hours, merging filtrate, with 70 % ethanol static 24 hours, Recycled ethanol was done the resin column pre-treatment, and by macroreticular resin, usefulness ethanol (85 %) wash-out is made dry extract |
| Dry extract must be measured (g) | 40.2 | 28.8 | 6.76 | 6.356 | 64.833 | 15.667 |
| Dry extract yield (%) | 20.1 | 14.4 | 3.38 | 3.18 | 12.97 | 3.13 |
| General flavone content (mg/g) | 179.2 | 296.3 | 532.5 | 553.5 | 229.01 | 549.72 |
| The general flavone rate of transform (%) | 70.0 | 82.9 | 34.98 | 33.06 | 55.25 | 32.05 |
| In the dry extract | 17.9 | 29.6 | 53.3 | 55.4 | 22.90 | 54.97 |
| General flavone purity (%) | ||||||
| General flavone yield (%) | 3.6 | 4.3 | 1.80 | 1.76 | 2.97 | 1.72 |
| Icariin content (mg/g) | 20.9 | 29.8 | 90.39 | 94.19 | 29.05 | 90.80 |
| The icariin rate of transform (%) | 78.8 | 80.8 | 57.42 | 56.26 | 69.55 | 52.53 |
| Icariin purity (%) in the dry extract | 2.09 | 2.98 | 9.04 | 9.42 | 2.91 | 9.08 |
| Icariin yield (%) | 0.42 | 0.43 | 031 | 0.30 | 0.38 | 0.28 |
| Characteristics | Simple process, the general flavone rate of transform is high, but general flavone purity is lower, is unfavorable for clinical use. | Technique is simple, and the general flavone rate of transform is high, but general flavone purity is lower, is unfavorable for clinical use, and the ethanol consumption is excessive, is not easy to industrial production. | General flavone purity is higher, meets the clinical application requirement, but owing to contain more impurity in the water extraction liquid, if water extraction liquid is directly passed through macroporous resin column, makes resin stain serious, and resin regeneration is difficulty very, is unfavorable for suitability for industrialized production. | General flavone purity is higher, meets the clinical application requirement, but the ethanol consumption is excessive, is unfavorable for suitability for industrialized production. | Meet the requirement of suitability for industrialized production, but general flavone purity is lower, is unfavorable for clinical use. | General flavone purity is higher, meets the clinical application requirement, can reduce impurity to the pollution of resin by alcohol precipitation, is conducive to the regeneration of resin, is fit to the requirement of industrialized production. |
In addition, the kind of eluant, eluent is investigated in the technique that poach alcohol precipitation and macroreticular resin wash-out are combined, and the result is as follows:
| Strippant | Water | 10% ethanol | 20% ethanol | 30% ethanol | 85% ethanol | 95% ethanol |
| General flavone content (mg/ml) | 1.946 | 0.363 | 0.379 | 0.399 | 2.2433 | 0.143 |
Observe by thin-layered chromatography, although water lotion has stronger absorption at the 270nm place, in thin-layer chromatography, almost without the spot (test of pesticide effectiveness proves, water elution thing parmacodynamics-less activity) of icariin, and the icariin spot is arranged all in other eluent. And by to the comparison of general flavone content under the different ethanol concentration, barrenwort general flavone content be described with the improving constantly and increase of ethanol concentration, in the scope of 80-90% ethanol concentration for the highest, progressively decline under 90-100 % ethanol concentration.
In order to guarantee that the barrenwort general flavone has high level, reduce production costs again, be conducive to ethanol and reclaim, when wash-out, selecting first water is the strippant wash-out, to remove impurity; Again with 85% ethanol as the strippant wash-out, collect eluent, Recycled ethanol is made dry extract.
The invention still further relates to detection and the discrimination method of Shorthorned Epimedium P.E,
Proterties: be the yellowish-brown powder; Gas is little, bitter.
Easily molten in glacial acetic acid, 60-85% ethanol, almost insoluble in acetone and ethyl acetate.
Differentiate: get 0.1g, add 60% ethanol 10ml, ultrasonic processing makes dissolving, gets solution as need testing solution. Other gets barrenwort control medicinal material 1.0g, adds ethanol 15ml, and refluxing extraction 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml makes dissolving, passes through D101Type macroreticular resin (internal diameter 1.5cm, long 10cm, dress D101Type macroreticular resin 5ml, flow velocity are that 1ml/ divides), with water 15ml wash-out, discard water lotion, use again 85% ethanol 20ml wash-out, collect eluent, evaporate to dryness, residue add 85% ethanol 5ml dissolving, in contrast medicinal material solution. Get again the icariin reference substance, add methyl alcohol and make the solution that every 1ml contains 0.5mg, in contrast product solution. According to thin-layered chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VIB) test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10, lower floor's solution of placing about 4 ℃) be solvent, launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the alchlor test solution. In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious identical color. With the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious identical color.
Check: moisture, ash content should meet the every regulation of Chinese Pharmacopoeia standard;
The resin residue thing is measured according to Determination of Residual Organic Solvents (two ones of Chinese Pharmacopoeia versions in 2000, appendix VIIIP).
The divinylbenzene of chromatographic condition and system suitability test take diameter as 0.25-0.18mm-EST type porous polymer beads is as fixing phase, and column temperature is 80-170 ℃.
The preparation precision of standard liquid take by weighing the organic solvent benzene,toluene,xylene and styrene an amount of, adding respectively becomes 30,16,20,30 μ g/ml standard liquids without organic water-soluble solution and preparation. Precision is measured each 5ml of above-mentioned standard liquid, adds without organic water to be diluted to 50ml, and mixing, and get final product.
The preparation precision of need testing solution takes by weighing this product 1.0g, puts in the 10ml measuring bottle, adds without organic water, and ultrasonic processing makes dissolving and adds without organic water to scale, mixing, and get final product.
The determination method precision is measured standard liquid and each 10ml of need testing solution, and placing respectively volume is the empty sampling bottle of item of 25ml, band spiral shell fastener port lid. Bottleneck band barrier film pad, with should have poly tetrafluoroethylene to make with rubber blanket on the barrier film pad of top contact with air to separate, each bottle heated 30 minutes in 60 ℃ water-bath, be used in the syringe that heats in the empty test tube in the same water-bath and extract static headspace gas an amount of (being generally 1ml), sample introduction, record corresponding peak area, calculate, and get final product.
Benzene is residual must not to be surpassed 2ppm, Residual Toluene and must not surpass that 20ppm, dimethylbenzene residually must not surpass 20ppm, styrene is residual must not surpass 20ppm.
Assay:
Need testing solution 0.5ml under the accurate absorption of the general flavone Determination of Content of Icariin item puts in the volumetric flask of 50ml, adds methyl alcohol to scale, shakes up, as need testing solution. Other gets the icariin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 10 μ g, in contrast product solution. Get respectively need testing solution and reference substance solution, take reagent as blank, (one one of Chinese Pharmacopoeia version in 2000, appendix VA) measures trap at 270nm wavelength place according to AAS, calculates, and get final product.
Contain general flavone with icariin (C33H
40O
15) meter, must not be less than 50%.
Icariin is measured according to high performance liquid chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VID).
Chromatographic condition and system suitability test are filler with octadecyl silane; Second is fine-and water (30: 70) is mobile phase; The detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, makes the solution that every 1ml contains 0.1mg with methyl alcohol, and get final product.
The about 30mg of this product is got in the preparation of need testing solution, and is accurately weighed, puts in the 25ml measuring bottle, adds 60% ethanol 20ml, and ultrasonic processing makes dissolving, adds 60% ethanol to scale, shakes up, and filters with miillpore filter, gets subsequent filtrate, and get final product.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures, and get final product.
This product contains icariin (C33H
40O
15), must not be less than 7.8%. For the capsule of the preparation take extract of the present invention as active ingredient, the present invention also provides discriminating and assay method
Proterties: be capsule, content is that yellowish-brown powder, gas are little, bitter.
Differentiate: get this product 0.1g, add 60% ethanol 10ml, ultrasonic processing makes dissolving, gets solution as need testing solution. Other gets barrenwort control medicinal material 1.0g, adds ethanol 15ml, and refluxing extraction 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml makes dissolving, passes through D101Type macroreticular resin (internal diameter 1.5cm, long 10cm, dress D101Type macroreticular resin 5ml, flow velocity are that 1ml/ divides), with water 15ml wash-out, discard water lotion, use again 85% ethanol 20ml wash-out, collect eluent, evaporate to dryness, residue add 85% ethanol 5ml dissolving, in contrast medicinal material solution. Get again the icariin reference substance, add methyl alcohol and make the solution that every 1ml contains 0.5mg, in contrast product solution. According to thin-layered chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VIB) test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10, lower floor's solution of placing about 4 ℃) be solvent, launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the alchlor test solution. In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious identical color. With the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious identical color.
Check: this product should meet the every regulation of Chinese Pharmacopoeia standard rubber wafer;
Assay:
Need testing solution 0.5ml under the accurate absorption of the general flavone Determination of Content of Icariin item puts in the volumetric flask of 50ml, adds methyl alcohol to scale, shakes up, as need testing solution. Other gets the icariin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 10 μ g, in contrast product solution. Get respectively need testing solution and reference substance solution, take reagent as blank, (one one of Chinese Pharmacopoeia version in 2000, appendix VA) measures trap at 270nm wavelength place according to AAS, calculates, and get final product.
This product contains the 85-115% that general flavone should be labelled amount.
Icariin is measured according to high performance liquid chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VID).
Chromatographic condition and system suitability test are filler with octadecyl silane; Second is fine-and water (30: 70) is mobile phase; The detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, makes the solution that every 1ml contains 0.1mg with methyl alcohol, and get final product.
The about 30mg of this product is got in the preparation of need testing solution, and is accurately weighed, puts in the 25ml measuring bottle, adds 60% ethanol 20ml, and ultrasonic processing makes dissolving, adds 60% ethanol to scale, shakes up, and filters with miillpore filter, gets subsequent filtrate, and get final product.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures, and get final product.
Every of this product contains icariin (C33H
40O
15), must not be less than 23.5mg.
Function with cure mainly: this product has kidney-replenishing, the effect of strengthening the bones and muscles. Cure mainly osteoporosis.
Usage and consumption: oral, one time 3,3 times on the one.
Specification: 0.35g/ grain
Storage: airtight, put shady and cool dry place and preserve.
The specific embodiment:
Further specify by the following examples the present invention.
The preparation of embodiment 1 extract
Get barrenwort medicinal material 100kg, decoct three times, add water at every turn and be 20 times of medicinal material amount, the each decoction 2 hours merges decoction liquor, filters, filtrate is concentrated into the thick paste that relative density is 1.10-1.13 (50 ℃ of survey), let cool, add ethanol, make to contain the alcohol amount and reach 70%, left standstill 24 hours, filter, filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.18-1.20 (50 ℃ of survey), lets cool, adding distil water (identical with the medicinal material amount) makes dissolving, room temperature left standstill about 4 hours, drew supernatant, passed through D101Type macroreticular resin (internal diameter 10cm, long 100cm), with distilled water (3 times of amount bed volumes) wash-out, flow velocity is that 40ml/ divides, and discards water elution liquid, again with 85% ethanol (4 times of amount bed volumes) wash-out, collect eluent, Recycled ethanol also is concentrated into thick paste (relative density is 1.30-1.35,50 ℃ of surveys), drying under reduced pressure (control vacuum: 0.08Mpa; Temperature: 75-8050 ℃), be ground into fine powder, sieve, make.
The preparation of embodiment 2 capsules
Shorthorned Epimedium P.E 309g
Starch 41g
Make 1000
Method for making: get the total extract 309g of barrenwort, add starch, mixing incapsulates, and makes 1000, and get final product.
Claims (10)
1. a Shorthorned Epimedium P.E makes by following process, it is characterized in that, and barrenwort Chinese medicine process poach, alcohol precipitation, macroporous resin adsorption is collected eluent, and concentrate eluant obtains.
2. the extract of claim 1 is characterized in that, in the poach process amount of water be the medicinal material amount 10-30 doubly, decoct 2-4 time altogether, decocted 1-3 hour at every turn.
3. the extract of claim 1 is characterized in that, in the alcohol precipitation process, adding be ethanol, addition makes the alcohol amount of containing of solution reach 70%, add ethanol after, left standstill 24 hours, filter, filtrate recycling ethanol is also concentrated.
4. the extract of claim 1 is characterized in that, in the macroporous resin adsorption process, use be D101Type macroreticular resin (internal diameter 10cm, long 100cm), first with distilled water (3 times of amount bed volumes) wash-out, flow velocity is that 40ml/ divides, and discards water elution liquid, again with 85% ethanol (4 times of amount bed volumes) wash-out, collect eluent, Recycled ethanol also is concentrated into thick paste (relative density is 1.30-1.35,50 ℃ of surveys), drying under reduced pressure (control vacuum: 0.08Mpa; Temperature: 75-80 ℃), be ground into fine powder, sieve, make.
5. the discrimination method of the extract of claim 1 is characterized in that, this extract has following feature
A. be the yellowish-brown powder; Gas is little, bitter;
B. easily molten in glacial acetic acid, 60-85% ethanol, almost insoluble in acetone and ethyl acetate;
C. get extract 0.1g, add 60% ethanol 10ml, ultrasonic processing makes dissolving, gets solution as need testing solution. Other gets barrenwort control medicinal material 1.0g, adds ethanol 15ml, and refluxing extraction 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml makes dissolving, passes through D101Type macroreticular resin (internal diameter 1.5cm, long 10cm, dress D101Type macroreticular resin 5ml, flow velocity are that 1ml/ divides), with water 15ml wash-out, discard water lotion, use again 85% ethanol 20ml wash-out, collect eluent, evaporate to dryness, residue add 85% ethanol 5ml dissolving, in contrast medicinal material solution. Get again the icariin reference substance, add methyl alcohol and make the solution that every 1ml contains 0.5mg, in contrast product solution. According to thin-layered chromatography (one one of Chinese Pharmacopoeia version in 2000, appendix VIB) test, draw each 1 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10, lower floor's solution of placing about 4 ℃) be solvent, launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with the alchlor test solution. In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious identical color. With the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious identical color;
D. extract contains the amount of general flavone with icariin (C33H
40O
15) meter, be no less than 50%.
6. the assay method of general flavone in the extract of claim 1 is characterized in that, through following steps, gets the about 30mg of extract, accurately weighed, put in the 25ml measuring bottle, add 60% ethanol 20ml, ultrasonic processing makes dissolving, add 60% ethanol to scale, shake up, filter with miillpore filter, get solution. The accurate solution 0.5ml that draws puts in the volumetric flask of 50ml, adds methyl alcohol to scale, shakes up, as need testing solution. Other gets the icariin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 10 μ g, in contrast product solution. Get respectively need testing solution and reference substance solution, take reagent as blank, (one one of Chinese Pharmacopoeia version in 2000, appendix VA) measures trap at 270nm wavelength place according to AAS, calculates, and get final product.
7. contain the pharmaceutical composition of the extract of claim 1, it is characterized in that, formed by extract and the 0.1-99.9% medicine acceptable carrier of 0.1-99.9%.
8. the pharmaceutical composition of claim 7 is tablet, capsule, granule, oral liquid.
9. prepare a kind of medicine for the treatment of osteoporosis with claim 1,2,3,4,7,8 extract or composition.
10. the composition of claim 8 is capsules, and per 1000 capsules contain the extract 200-400g of claim, and all the other are starch.
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| CN1295224C (en) * | 2004-11-11 | 2007-01-17 | 中国药科大学 | Process for preparing epimedium total flavone for injection |
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