CN100412545C - Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease - Google Patents
Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease Download PDFInfo
- Publication number
- CN100412545C CN100412545C CNB021573794A CN02157379A CN100412545C CN 100412545 C CN100412545 C CN 100412545C CN B021573794 A CNB021573794 A CN B021573794A CN 02157379 A CN02157379 A CN 02157379A CN 100412545 C CN100412545 C CN 100412545C
- Authority
- CN
- China
- Prior art keywords
- extract
- water
- red sage
- less
- sage root
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 150000001875 compounds Chemical class 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 21
- 240000007164 Salvia officinalis Species 0.000 title abstract description 202
- 235000005412 red sage Nutrition 0.000 title abstract description 136
- 238000002360 preparation method Methods 0.000 title abstract description 41
- 201000010099 disease Diseases 0.000 title description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 title description 3
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 claims abstract description 101
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 claims abstract description 100
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 claims abstract description 99
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 claims abstract description 99
- 229940116229 borneol Drugs 0.000 claims abstract description 99
- IBGBGRVKPALMCQ-UHFFFAOYSA-N 3,4-dihydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1O IBGBGRVKPALMCQ-UHFFFAOYSA-N 0.000 claims abstract description 34
- AIGAZQPHXLWMOJ-UHFFFAOYSA-N tanshinone IIA Natural products C1=CC2=C(C)C=CC=C2C(C(=O)C2=O)=C1C1=C2C(C)=CO1 AIGAZQPHXLWMOJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- PAFLSMZLRSPALU-MRVPVSSYSA-N (2R)-3-(3,4-dihydroxyphenyl)lactic acid Chemical compound OC(=O)[C@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-MRVPVSSYSA-N 0.000 claims abstract description 21
- PAFLSMZLRSPALU-QMMMGPOBSA-N Danshensu Natural products OC(=O)[C@@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-QMMMGPOBSA-N 0.000 claims abstract description 21
- PAFLSMZLRSPALU-UHFFFAOYSA-N Salvianic acid A Natural products OC(=O)C(O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229960003371 protocatechualdehyde Drugs 0.000 claims abstract description 17
- GVKKJJOMQCNPGB-UHFFFAOYSA-N Cryptotanshinone Natural products O=C1C(=O)C2=C3CCCC(C)(C)C3=CC=C2C2=C1C(C)CO2 GVKKJJOMQCNPGB-UHFFFAOYSA-N 0.000 claims abstract description 16
- GVKKJJOMQCNPGB-JTQLQIEISA-N Cryptotanshinone Chemical compound O=C1C(=O)C2=C3CCCC(C)(C)C3=CC=C2C2=C1[C@@H](C)CO2 GVKKJJOMQCNPGB-JTQLQIEISA-N 0.000 claims abstract description 16
- 238000003556 assay Methods 0.000 claims abstract description 15
- HYXITZLLTYIPOF-UHFFFAOYSA-N Tanshinone II Natural products O=C1C(=O)C2=C3CCCC(C)(C)C3=CC=C2C2=C1C(C)=CO2 HYXITZLLTYIPOF-UHFFFAOYSA-N 0.000 claims abstract description 12
- AZEZEAABTDXEHR-UHFFFAOYSA-M sodium;1,6,6-trimethyl-10,11-dioxo-8,9-dihydro-7h-naphtho[1,2-g][1]benzofuran-2-sulfonate Chemical compound [Na+].C12=CC=C(C(CCC3)(C)C)C3=C2C(=O)C(=O)C2=C1OC(S([O-])(=O)=O)=C2C AZEZEAABTDXEHR-UHFFFAOYSA-M 0.000 claims abstract description 12
- YURJSTAIMNSZAE-HHNZYBFYSA-N ginsenoside Rg1 Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YURJSTAIMNSZAE-HHNZYBFYSA-N 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 163
- 244000131316 Panax pseudoginseng Species 0.000 claims description 114
- 235000003181 Panax pseudoginseng Nutrition 0.000 claims description 114
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 96
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 45
- 229940089161 ginsenoside Drugs 0.000 claims description 44
- 229930182494 ginsenoside Natural products 0.000 claims description 44
- 239000006210 lotion Substances 0.000 claims description 44
- 238000005406 washing Methods 0.000 claims description 44
- 239000006187 pill Substances 0.000 claims description 40
- 239000000706 filtrate Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000003908 quality control method Methods 0.000 claims description 14
- 239000009524 danshen dripping Substances 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000945 filler Substances 0.000 claims description 9
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 229930183118 Tanshinone Natural products 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 claims description 6
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- ZMMKVDBZTXUHFO-DDWIOCJRSA-M sodium;(2r)-3-(3,4-dihydroxyphenyl)-2-hydroxypropanoate Chemical compound [Na+].[O-]C(=O)[C@H](O)CC1=CC=C(O)C(O)=C1 ZMMKVDBZTXUHFO-DDWIOCJRSA-M 0.000 claims description 3
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical class O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 26
- 229940079593 drug Drugs 0.000 abstract description 2
- YURJSTAIMNSZAE-UHFFFAOYSA-N UNPD89172 Natural products C1CC(C2(CC(C3C(C)(C)C(O)CCC3(C)C2CC2O)OC3C(C(O)C(O)C(CO)O3)O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O YURJSTAIMNSZAE-UHFFFAOYSA-N 0.000 abstract 3
- CBEHEBUBNAGGKC-UHFFFAOYSA-N ginsenoside Rg1 Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5CC(OC6OC(CO)C(O)C(O)C6O)C34C)C CBEHEBUBNAGGKC-UHFFFAOYSA-N 0.000 abstract 3
- UFNDONGOJKNAES-UHFFFAOYSA-N Ginsenoside Rb1 Natural products CC(=CCCC(C)(OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CC(O)C45C)C UFNDONGOJKNAES-UHFFFAOYSA-N 0.000 abstract 2
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 abstract 2
- TXEWRVNOAJOINC-UHFFFAOYSA-N ginsenoside Rb2 Natural products CC(=CCCC(OC1OC(COC2OCC(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CCC45C)C TXEWRVNOAJOINC-UHFFFAOYSA-N 0.000 abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 345
- 239000000284 extract Substances 0.000 description 169
- 239000012141 concentrate Substances 0.000 description 71
- 235000017276 Salvia Nutrition 0.000 description 65
- 239000000843 powder Substances 0.000 description 57
- 238000001035 drying Methods 0.000 description 56
- 239000007788 liquid Substances 0.000 description 53
- 239000011347 resin Substances 0.000 description 42
- 229920005989 resin Polymers 0.000 description 42
- 238000010828 elution Methods 0.000 description 41
- 239000000203 mixture Substances 0.000 description 41
- 239000006228 supernatant Substances 0.000 description 40
- 239000000243 solution Substances 0.000 description 35
- 239000000463 material Substances 0.000 description 30
- 239000002775 capsule Substances 0.000 description 25
- 238000007670 refining Methods 0.000 description 23
- 239000002245 particle Substances 0.000 description 21
- 238000000605 extraction Methods 0.000 description 20
- 239000011159 matrix material Substances 0.000 description 18
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 18
- 244000132619 red sage Species 0.000 description 18
- 238000001556 precipitation Methods 0.000 description 17
- 239000007921 spray Substances 0.000 description 17
- 239000012071 phase Substances 0.000 description 15
- 238000010992 reflux Methods 0.000 description 15
- WTPPRJKFRFIQKT-UHFFFAOYSA-N 1,6-dimethyl-8,9-dihydronaphtho[1,2-g][1]benzofuran-10,11-dione;1-methyl-6-methylidene-8,9-dihydro-7h-naphtho[1,2-g][1]benzofuran-10,11-dione Chemical compound O=C1C(=O)C2=C3CCCC(=C)C3=CC=C2C2=C1C(C)=CO2.O=C1C(=O)C2=C3CCC=C(C)C3=CC=C2C2=C1C(C)=CO2 WTPPRJKFRFIQKT-UHFFFAOYSA-N 0.000 description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 210000004369 blood Anatomy 0.000 description 12
- 239000008280 blood Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 102000011759 adducin Human genes 0.000 description 9
- 108010076723 adducin Proteins 0.000 description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
- 208000031225 myocardial ischemia Diseases 0.000 description 9
- 230000003203 everyday effect Effects 0.000 description 8
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 8
- 229920000053 polysorbate 80 Polymers 0.000 description 8
- 229920002545 silicone oil Polymers 0.000 description 8
- 239000004338 Dichlorodifluoromethane Substances 0.000 description 7
- 239000000443 aerosol Substances 0.000 description 7
- 239000002826 coolant Substances 0.000 description 7
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 7
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 7
- 230000004927 fusion Effects 0.000 description 7
- 210000004907 gland Anatomy 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 238000002347 injection Methods 0.000 description 7
- 238000009413 insulation Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000011122 softwood Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 241000700159 Rattus Species 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 230000002354 daily effect Effects 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 229930189533 tanshinol Natural products 0.000 description 6
- 102000004420 Creatine Kinase Human genes 0.000 description 5
- 108010042126 Creatine kinase Proteins 0.000 description 5
- 229920001353 Dextrin Polymers 0.000 description 5
- 239000004375 Dextrin Substances 0.000 description 5
- 241000699666 Mus <mouse, genus> Species 0.000 description 5
- 241000699670 Mus sp. Species 0.000 description 5
- 239000008118 PEG 6000 Substances 0.000 description 5
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 5
- 208000007536 Thrombosis Diseases 0.000 description 5
- 208000026106 cerebrovascular disease Diseases 0.000 description 5
- 235000019425 dextrin Nutrition 0.000 description 5
- 239000007901 soft capsule Substances 0.000 description 5
- 208000024172 Cardiovascular disease Diseases 0.000 description 4
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 description 4
- 235000011135 Salvia miltiorrhiza Nutrition 0.000 description 4
- 206010041956 Stasis syndrome Diseases 0.000 description 4
- 230000002785 anti-thrombosis Effects 0.000 description 4
- 208000005634 blind loop syndrome Diseases 0.000 description 4
- 230000017531 blood circulation Effects 0.000 description 4
- 229930004069 diterpene Natural products 0.000 description 4
- 125000000567 diterpene group Chemical group 0.000 description 4
- 230000002526 effect on cardiovascular system Effects 0.000 description 4
- 230000000144 pharmacologic effect Effects 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 210000002966 serum Anatomy 0.000 description 4
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 3
- DOUMFZQKYFQNTF-WUTVXBCWSA-N (R)-rosmarinic acid Chemical compound C([C@H](C(=O)O)OC(=O)\C=C\C=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-WUTVXBCWSA-N 0.000 description 3
- 241000723346 Cinnamomum camphora Species 0.000 description 3
- 235000003143 Panax notoginseng Nutrition 0.000 description 3
- 241000180649 Panax notoginseng Species 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000037396 body weight Effects 0.000 description 3
- 229930008380 camphor Natural products 0.000 description 3
- 229960000846 camphor Drugs 0.000 description 3
- 230000000747 cardiac effect Effects 0.000 description 3
- 208000029078 coronary artery disease Diseases 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 230000002496 gastric effect Effects 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000001802 infusion Methods 0.000 description 3
- 230000003387 muscular Effects 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 2
- XYKZSUXWBGUGQV-UHFFFAOYSA-N 4,8-dimethylnaphtho[2,1-f][1]benzofuran-7,11-dione Chemical compound CC1=CC=CC2=C(C(C=3OC=C(C=3C3=O)C)=O)C3=CC=C21 XYKZSUXWBGUGQV-UHFFFAOYSA-N 0.000 description 2
- 208000037260 Atherosclerotic Plaque Diseases 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 206010008190 Cerebrovascular accident Diseases 0.000 description 2
- 229920000858 Cyclodextrin Polymers 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 2
- ZZAFFYPNLYCDEP-HNNXBMFYSA-N Rosmarinsaeure Natural products OC(=O)[C@H](Cc1cccc(O)c1O)OC(=O)C=Cc2ccc(O)c(O)c2 ZZAFFYPNLYCDEP-HNNXBMFYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 208000006011 Stroke Diseases 0.000 description 2
- 230000000702 anti-platelet effect Effects 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 239000003146 anticoagulant agent Substances 0.000 description 2
- 210000000709 aorta Anatomy 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000007884 disintegrant Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000008899 fufang danshen Substances 0.000 description 2
- GVBFBKODLPVQOA-UHFFFAOYSA-N heptane-1-sulfonic acid;sodium Chemical compound [Na].CCCCCCCS(O)(=O)=O GVBFBKODLPVQOA-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 2
- 239000008108 microcrystalline cellulose Substances 0.000 description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 2
- 230000003285 pharmacodynamic effect Effects 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011552 rat model Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- DOUMFZQKYFQNTF-MRXNPFEDSA-N rosemarinic acid Natural products C([C@H](C(=O)O)OC(=O)C=CC=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-MRXNPFEDSA-N 0.000 description 2
- TVHVQJFBWRLYOD-UHFFFAOYSA-N rosmarinic acid Natural products OC(=O)C(Cc1ccc(O)c(O)c1)OC(=Cc2ccc(O)c(O)c2)C=O TVHVQJFBWRLYOD-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 description 1
- ATADHKWKHYVBTJ-FVGYRXGTSA-N (R)-adrenaline hydrochloride Chemical compound [H+].[Cl-].CNC[C@H](O)C1=CC=C(O)C(O)=C1 ATADHKWKHYVBTJ-FVGYRXGTSA-N 0.000 description 1
- HARGZZNYNSYSGJ-UHFFFAOYSA-N 1,2 dihydrotanshinquinone Natural products C1=CC2=C(C)C=CC=C2C(C(=O)C2=O)=C1C1=C2C(C)CO1 HARGZZNYNSYSGJ-UHFFFAOYSA-N 0.000 description 1
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 208000034657 Convalescence Diseases 0.000 description 1
- 101710088194 Dehydrogenase Proteins 0.000 description 1
- HARGZZNYNSYSGJ-JTQLQIEISA-N Dihydrotanshinone I Chemical compound C1=CC2=C(C)C=CC=C2C(C(=O)C2=O)=C1C1=C2[C@@H](C)CO1 HARGZZNYNSYSGJ-JTQLQIEISA-N 0.000 description 1
- 206010061216 Infarction Diseases 0.000 description 1
- 201000001429 Intracranial Thrombosis Diseases 0.000 description 1
- 208000007201 Myocardial reperfusion injury Diseases 0.000 description 1
- 206010028851 Necrosis Diseases 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- -1 Rosmarinic acid methyl esters Chemical class 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 241000256856 Vespidae Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000006502 antiplatelets effects Effects 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000003143 atherosclerotic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940074360 caffeic acid Drugs 0.000 description 1
- 235000004883 caffeic acid Nutrition 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 206010008118 cerebral infarction Diseases 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- YTJJRAWFHJBAMT-UHFFFAOYSA-N depside Natural products OC(=O)CC1=C(O)C=C(O)C=C1OC(=O)C1=CC=C(O)C(O)=C1 YTJJRAWFHJBAMT-UHFFFAOYSA-N 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 230000007831 electrophysiology Effects 0.000 description 1
- 238000002001 electrophysiology Methods 0.000 description 1
- 210000003743 erythrocyte Anatomy 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000001076 estrogenic effect Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 230000007574 infarction Effects 0.000 description 1
- 208000028867 ischemia Diseases 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001114 myogenic effect Effects 0.000 description 1
- 230000017074 necrotic cell death Effects 0.000 description 1
- 239000003182 parenteral nutrition solution Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention discloses a method for controlling the quality of a compound red sage root preparation. The present invention comprises one or some in the following assays: each preparation adopts the dosage of a finished product of daily taken crude drugs as the unitage; in the assay of danshensu and protocatechuic aldehyde, each unitage comprises not less than 2.0 to 4.40 mg of the danshensu and not less than 0.13 to 1.44 mg of the protocatechuic aldehyde, in the assay of tanshinone IIA and cryptotanshinone, each unitage comprises not less than 3.5 to 7.2 mg of the tanshinone IIA and not less than 3.5 to 7.2 mg of the cryptotanshinone; in the assay of borneol, each unitage comprises not less than 20 to 50 mg of the borneol; in the assay of ginsenoside RB1 and ginsenoside Rg1, each unitage comprises not less than 6.67 to 21.43 mg of ginsenoside Rg1, and the total amount of the ginsenoside Rg1 and the ginsenoside Rb1 is not less than 13.3 to 42.86 mg.
Description
Invention field
The present invention relates to a kind of pharmaceutical preparation and method of quality control thereof, particularly relate to the compound red sage root preparation and the method for quality control thereof for the treatment of cardiovascular and cerebrovascular disease.
Background of invention
Cardiovascular and cerebrovascular disease is to cause human first dead sick the kind, and along with the raising of social life level and the aging of population, the research of cardiovascular and cerebrovascular diseases medicament becomes the focus of drug development.Coronary atherosclerotic heart disease, be called for short coronary heart disease, its cause of disease is because some can not infilter blood-lipoids material such as cholesterol, the triglyceride etc. of arterial wall, be deposited on and form " atheromatous plaque " back on the endarterium because of calmness calcareous in the liquid, make original whippy artery hardening, along with the atheromatous plaque scope on the endarterium strengthens, cause lumen of vessels to narrow down even block, cause myocardial ischemia, anoxic or necrosis.Ischemia apoplexy (cerebral infarction) all is important opportunitys of its prevention and treatment at acute attack stage and in apoplexy early stage and convalescence.Traditional Chinese medicine plays an important role in above-mentioned prevention and treatment of diseases, especially is that the folk prescription or the compound preparation of primary raw material all has definite curative effect with the red sage root, as Fufang Danshen Pian, compound injection of red sage root, treating coronary heart disease particle, happy amylan capsule etc.The red sage root is being brought into play main effect in these preparations.
The red sage root is the root of Labiatae salvia red sage root Salvia miltiorrhiza Bge..Bitter, cold nature, have promoting blood circulation and removing blood stasis, nourishing blood and tranquilization, the effect of cool blood row's carbuncle and toxin expelling myogenic is a Chinese medicine common drug promoting blood circulation and removing blood stasis.The red rooted salvia master contains fat-soluble Diterpenes composition and water miscible liposoluble ingredient, still contains other compositions such as flavonoids, triterpenes, sterol.What belong to quinone, ketone type structure in the Diterpenes composition has Tanshinone I, an II
A, II
B, V, VI, Cryptotanshinone, isotanshinone I, II, II
B, dihydrotanshinone I etc.Water miscible liposoluble ingredient has depside that danshensu, protocatechualdehyde, protocatechuic acid, caffeic acid and danshensu and caffeinic derivant or dipolymer esterification form such as salviandic acid A, B, C, D, E, G, alkannic acid B, Rosmarinic acid, Rosmarinic acid methyl esters etc.Tanshinone I I
AIt is one of red sage root Diterpenes representative composition promoting blood circulation and removing blood stasis.Modern pharmacological research shows Tanshinone I I
AThe pharmacological action of monomer mainly contains: expeirmental myocardial ischemia and reperfusion injury are had the improvement effect; Influence experiment to cardiac electrophysiology shows calcium antagonism; The antiplatelet aggregative activity anti thrombotic action.On behalf of the composition Cryptotanshinone, red sage root Diterpenes another have the antibacterial and estrogen-like action of anti-inflammatory.The pharmacological action of water-soluble phenolic acids monomeric compound mainly contains in the red sage root: anti thrombotic action comprises antiplatelet effects, anticoagulation, anti-thrombosis function; Improve the blood circulation effect; The anti-oxidative damage effect.The limitation of existing red sage formulation technology shows as: 1, the instability of tanshinone, concentrate, in the dry run loss more, cause the low and content poor reproducibility of tanshinone retention rate in preparation; Tanshinone poorly soluble, dissolution rate is low in the preparation.Existing preparation does not screen suitable auxiliary material and technology, to improve the tanshinone dissolution rate; 2, the extraction of water-soluble danshinolic acid class is index with the danshensu, and loss of active ingredients such as danshensu is bigger in the alcohol precipitation process for refining, and retention rate is low in preparation; Absorb in the danshensu body, metabolism is fast, ordinary preparation is difficult to keep the stability of oral administration blood concentration.Therefore when the exploitation red sage formulation, not only should cure mainly, extract its active component of reservation according to the prescription function; And should in moulding process, impose the preparation factor, improve the release of effective constituent and making with extra care of preparation.
Summary of the invention
The object of the invention is to provide a kind of compound red sage root preparation; The object of the invention also is to provide a kind of preparation method of compound red sage root preparation; The object of the invention also is to provide a kind of method of quality control of compound red sage root preparation.
The present invention seeks to be achieved through the following technical solutions:
Preparation of the present invention is made by following raw material:
Salvia root P.E 4-60 weight portion, Notogineng Extract 2-18 weight portion, borneol 1-10 weight portion.
The above-mentioned raw materials optimum ratio is: Salvia root P.E 36-54 weight portion, Notogineng Extract 8.46-16.92 weight portion, borneol 2-8 weight portion; The above-mentioned raw materials optimum ratio is: Salvia root P.E 18-27 weight portion, Notogineng Extract 4.23-8.46 weight portion, borneol 1-2 weight portion; The above-mentioned raw materials optimum ratio is: Salvia root P.E 4.5-9 weight portion, Notogineng Extract 2.82-5.64 weight portion, borneol 4-6 weight portion.
Salvia root P.E of the present invention can be that red sage root super critical extract, tanshinol extract, red sage root water extract-alcohol precipitation extract, red sage root water extract or red sage root water were carried the refining thing of post; Salvia root P.E of the present invention can also be that red sage root water extract-alcohol precipitation extract or red sage root water were carried refining thing of post and red sage root super critical extract or tanshinol extract in 1-99: the composition of 99-1 ratio; Described red sage root water extract-alcohol precipitation extract or red sage root water were carried refining thing of post and red sage root super critical extract or tanshinol extractive composition percentage: 80-20: 20-80,70-30: 30-70,60-40: 40-60 or 50: 50.
Notogineng Extract of the present invention is pseudo-ginseng water extract or pseudo-ginseng alcohol extract; Borneol of the present invention can replace with camphor.
Red sage root super critical extract of the present invention or tanshinol extract contain tanshinone IIA and are no less than 5-10%; Red sage root water extract-alcohol precipitation extract or red sage root water were carried the refining thing of post and are contained danshensu and be no less than 0.5-1.5%, and protocatechualdehyde is no less than 0.16-0.48%; Pseudo-ginseng water extract or pseudo-ginseng alcohol extract contain the ginsenoside Rg
1Be no less than 15.83-30%, contain the ginsenoside Rg
1And Rb
1Be no less than 31-40%.
Preparation of the present invention can add auxiliary material and make clinical acceptable forms such as tablet, capsule, oral liquid, dripping pill, spray, granule; Described auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
Preparation of the present invention is as follows
A, compound danshen dripping pills
Press recipe quantity, with Salvia root P.E, Notogineng Extract and borneol are pulverized, and mix stand-by; Press medicinal powder: matrix 1: 1-2 with matrix PEG6000 or PEG4000 fusion after, add medicine and mix, 60-90 ℃ of insulation dripped/minute added in the methyl-silicone oil with 20-70, collects dripping pill, absorbs liquid coolant with filter paper, the heavy 20-80mg of every ball.
B, compound capsule of red sage root:
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix, and add auxiliary material 1-3 doubly, make capsule.
C, compound Danshen Root particle
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix, and add the auxiliary material that suitable medicine 2-5 doubly measures, and make softwood with the ethanol of 60-90% concentration, make particle.
D, compound red sage root spray
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by, add 10～20% Tween-80 ethanolic solutions, 30～300 parts by volume, add 1,2-propylene glycol 100～500 parts by volume, mixing, ethanol is fixed molten to 200～1000 parts by volume g/ml, be sub-packed in the aerosol pressure bottle by 20-100ml (specification), in every bottle, be pressed into dichlorodifluoromethane 1～10 weight portion behind the gland, make spray.
E, compound Danshen Root oral liquid
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol mix, and add 1-3 and doubly measure (g/ml) Tween-80, add the injection water again and make oral liquid.
The preparation of Salvia root P.E of the present invention can be but be not limited in the following method any one:
1, gets red rooted salvia, supercritical CO
2Extraction adds 10-40% medicinal material amount 75-95% ethanol and makes entrainer, extracting pressure 20-40Mpa, temperature 30-60 ℃, gets the red sage root super critical extract.
2, get red rooted salvia, behind the supercritical extract, medicinal powder is taken out, decocting boils 1-2 time, add 6-8 times of water gaging respectively, decocted 0.5-1 hour, merge decocting liquid, concentrate, add 75-95% ethanol and make and contain alcohol amount and reach 60-80%, left standstill 12-24 hour, filter, the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract.
3, get red rooted salvia, behind the supercritical extract, medicinal powder is taken out, decocting boils 1-2 time, adds 4-8 times of water gaging respectively, decocts 1-2 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, the 30-80% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing of post.
4, get red rooted salvia, decocting boils 2-3 time, adds 4-8 times of water gaging respectively, decocted 1-2 hour, and merged decocting liquid, being concentrated into relative density is 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, the 30-80% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing of post.
5, red rooted salvia, 95% alcohol reflux 1-3 time, each 1-2 hour, reclaim ethanol, concentrate drying gets the tanshinol extract.
The preparation of Notogineng Extract of the present invention can be but be not limited in the following method any one:
1, get pseudo-ginseng, pulverize, decocting boils 2-3 time, adds water 4-6 respectively doubly, decocts 1-2 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, the 30-80% ethanol elution reclaims ethanol, and concentrate drying gets the pseudo-ginseng water extract.
2, get pseudo-ginseng, pulverize, add 60-70% alcohol reflux 2-3 time, each 1-2 hour, extract reclaimed ethanol, and being concentrated into relative density is 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, the 30-80% ethanol elution, reclaim ethanol, concentrate drying gets the pseudo-ginseng alcohol extract.
Preparation of the present invention is except that being raw material directly feeds intake from extract, can also be the raw material preparation that directly feeds intake by raw medicinal material:
Get red rooted salvia 130-450 weight portion and pseudo-ginseng 25-145 weight portion, be ground into coarse grain, decocting boils 2-3 time, adds water 4-6 respectively and doubly measures, and decocts 1-2 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, the 30-80% ethanol elution reclaims ethanol, concentrate drying, Salvia miltiorrhiza and Panax notoginseng is closed and is carried thing, add borneol fine powder 1-8 weight portion, add auxiliary material and make tablet, capsule, oral liquid, dripping pill, spray, granule, described auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
The raw medicinal material proportioning can also be to get red rooted salvia 130-240 weight portion, pseudo-ginseng 28-60 weight portion, borneol or camphor 1.5-5 weight portion.
The described macroporous resin column model of this instructions can be: D101, DA201, DM130, WLD-3, YPR-II, X5, AB-8, HPD-100, Dx-5, NKA-9.
Contain in the following assay one or more in the method for quality control of the present invention:
A, danshensu, protocatechualdehyde (according to high performance liquid chromatography)
It is an amount of to get each preparation, puts in the tool plug triangular flask, adds methyl alcohol 25ml, sonicated 2 hours, put coldly, add methyl alcohol and supply weight, shake up, filter, get filtrate 10ml, water-bath is concentrated into dried, adds water 10ml, and ether 20ml is transferred in the separating funnel, divide and get ether layer, water layer is used 10ml extracted with diethyl ether 2 times more respectively, merge ether solution, ether solution is washed with 5ml, and washing lotion is incorporated above-mentioned water layer into, volatilizes ether, steam to a small amount of, add methanol constant volume to the 10ml volumetric flask, be need testing solution; Methanol solution with Sodium Danshensu is contrast; The chromatographic column octadecylsilane chemically bonded silica is a filling agent, 2-5: 4-1: 95-99=methyl alcohol: the heptanesulfonic acid sodium solution: water or 75-85: 22-16: 0.5-2=water: methyl alcohol: glacial acetic acid is a moving phase, and the detection wavelength is 280nm; Each preparation is a unit quantity to take output suitable every day, and the per unit amount contains danshensu and is no less than 2.0mg or is no less than 4.40mg, and protocatechualdehyde is no less than 0.13mg or is no less than 1.44mg;
B, tanshinone IIA, Cryptotanshinone (according to high performance liquid chromatography)
Get ether solution under a item, evaporate to dryness, methanol constant volume is contrast to 10ml with the methanol solution of tanshinone and the methanol solution of Cryptotanshinone, is filling agent with octadecylsilane chemically bonded silica, and 70-80: 30-20=methyl alcohol: water is moving phase, and the detection wavelength is 270nm; Each preparation is a unit quantity to take output suitable every day, and the per unit amount contains Tanshinone I I A and is no less than 3.5mg or is no less than 7.2mg, and Cryptotanshinone is no less than 3.5mg or is no less than 7.2mg;
C, borneol (according to vapor-phase chromatography)
It is an amount of to get n-pentadecane, and it is fixed molten to add ethyl acetate, as inner mark solution; It is an amount of to get each preparation finished product, adds inner mark solution, and sonicated 2 hours filters, and gets filtrate, is contrast with the inner mark solution of borneol, is stationary phase with polyglycol-20M, and coating concentration is 10%, and column temperature is 140 ℃; Each preparation is a unit quantity to take output suitable every day, and the per unit amount contains borneol and is no less than 20mg or is no less than 50mg;
D, ginsenoside Rb
1And ginsenoside Rg
1(according to high performance liquid chromatography)
Get test sample under a item, with ginsenoside Rb
1And ginsenoside Rg
1Methanol solution for the contrast; With octadecylsilane chemically bonded silica is filling agent, 55-65: 45-35=methyl alcohol: water or 90-110: 410-390=second cyanogen: 0.05% phosphoric acid solution or 1-4: 9-6=second cyanogen: water is moving phase, and the detection wavelength is 203nm; Perhaps use amino normal phase column, with 85-90: 15-10=second cyanogen: 1% phosphoric acid is moving phase, and the detection wavelength is 203nm; Each preparation is a unit quantity to take output suitable every day, and the per unit amount contains the ginsenoside Rg
1Be no less than 6.67mg or be no less than 21.43mg, contain the ginsenoside Rg
1And Rb
1Total amount is no less than 13.3mg or is no less than 42.86mg.
Per unit amount content can also be in the above-mentioned method of quality control: tanshinone IIA is no less than 3.53mg or is no less than 7.06mg, Cryptotanshinone is no less than 3.53mg or is no less than 7.06mg, danshensu is no less than 2.1mg or is no less than 4.2mg, protocatechualdehyde is no less than 0.13mg or is no less than 0.26mg, contains the ginsenoside Rg
1Be no less than 6.67mg or be no less than 13.3mg, contain the ginsenoside Rg
1And Rb
1Total amount is no less than 13.3mg or is no less than 26.6mg.
The moving phase of the assay of danshensu, protocatechualdehyde can also be 80: 19 in the above-mentioned method of quality control: 1=water: methyl alcohol: glacial acetic acid; The ginsenoside Rg
1With ginsenoside Rb
1The moving phase of assay can also be 3: 7=second cyanogen: water or 87: 13=second cyanogen: 1% phosphoric acid or 99: 400=second cyanogen: 0.05% phosphoric acid solution.
Described each preparation finished product amount of regularlying sample and deciding in right amount of getting.
Compound red sage root preparation of the present invention, compare technology advanced person, few, the determined curative effect of dose with official preparation, Pharmacodynamic test of active extract result shows: have and resist myocardial ischemia and effects such as anti-platelet aggregation, treatment coronary heart disease, angina pectoris, miocardial infarction, cerebral thrombus.These pharmacological actions are confirmed by following pharmacodynamic experiment example.Following experimental example is used to further specify the present invention.
Experimental example 1The anti thrombotic action of compound Danshen Root tablet of the present invention
Get 40 of rats, be divided into 4 groups at random, press 6 of human dosage, 12 times of amounts are established the dosage group, every day gastric infusion once, successive administration 7 days, after the administration in the 4th day behind the 30min, except that the blank group, all the other animal hypodermic injection adrenalin hydrochloride parenteral solution Adr (0.1%) 0.1ml/, 30min is placed on the 5min that swims in 1.5 degrees centigrade of water, repeated swimming on the 5th day under the same conditions once, 30min after the administration in the 6th day injects Adr one time, 30min after the last administration again, in animal lumbar injection yellow Jackets 35mg/kg, anesthetized rat is got blood from rat aorta then, surveys thrombosis.The result shows: compound red sage root preparation can obviously suppress the formation of blood stasis rats in vitro thrombus, reduces the weight of thrombus, shortens the length of thrombus.See Table 1.
The influence that table 1 compound red sage root preparation forms stasis syndrome rat model external thrombus
Compare * P＜0.05, * * P＜0.01, * * * P＜0.001 with model control group
Experimental example 2The influence that compound danshen dripping pills of the present invention is learned stasis syndrome model mouse hemorheology
Grouping, administration, modeling and processing are with experimental example 1.Get blood from rat aorta and survey its whole blood contrast viscosity, plasma viscosity, packed cell volume and erythrocyte sedimentation rate, the results are shown in Table 2.
Table 2 red sage formulation is to the hemorheology influence of stasis syndrome rat model
Compare * P＜0.05 with model control group, * * P＜0.01,
As seen from Table 2, compound red sage root preparation can reduce the whole blood contrast viscosity of stasis syndrome rat, and other index is not had obvious influence.
Experimental example 3 compound Danshen Root particles are to the influence of MDA content in LDH, CPK and the cardiac muscular tissue in the myocardial ischemia mice serum due to the isoprel
Get 50 of mouse, female, body weight 20 ± 2g, divide equally 5 groups by body weight, in the 7th day, press 5 of human dosage, 10,15 times of amounts are established the dosage group, every day gastric infusion once, the 1st, give consubstantiality ponding 10ml/kg for 2 groups, after administration 4-6 days, the 1st group of hypodermic injection physiological saline 10ml/kg, 2-8 group hypodermic injection isoprel 4mg/kg, 24h after last is given isoprel is after the socket of the eye vein is got blood, measure lactic dehydrogenase (LDH) and creatine phosphokinase (CPK) content in the mice serum, the muscular tissue of coring is surveyed MDA (MDA) content, and the result shows, compound red sage root preparation can obviously reduce because the activity of LDH and CPK in the myocardial ischemia mice serum due to the isoprel, and mda content in the cardiac muscular tissue, and there were significant differences; See Table 3.
Table 3 compound red sage root preparation is to the influence of LDH and CPK in the myocardial ischemia mice serum due to the isoprel
Compare * P＜0.05, * * P＜0.01, * * * P＜0.001 with model control group
Experimental example 4Compound capsule of red sage root is to the influence of myocardial ischemia mouse
Get 50 of male mices, divide equally 5 groups, establish the dosage group by 5,10,15 times of amounts of human dosage by body weight, gastric infusion, be administered once every day, after the last administration 30 minutes, hypodermic injection (except first group) isoprel 5ml/kg does anti-weary oxygen experiment after 15 minutes.The result shows, compound red sage root preparation can obviously prolong myocardial ischemia mouse diing time due to the isoprel, and significant difference is arranged, and sees Table 4.
Table 4 compound red sage root preparation is to the influence of the weary oxygen of myocardial ischemia mouse anti due to the isoprel
Compare * P＜0.05, * * P＜0.01, * * * P＜0.001 with model control group
Following embodiment all can realize above-mentioned effect.
Embodiment 1: Fufang Danshen Pian
Red sage root water was carried post thing 36g Notogineng Extract 8.46g borneol 2g, made 400 in tablet, and each 2,2 times/day.
Embodiment 2: compound capsule of red sage root
Tanshinol extract 18g, pseudo-ginseng alcohol extract 4.23g, borneol 3g makes 270 of capsules, one time 1,2-3 time/day.
Embodiment 3: the compound Danshen Root particle
Red sage root water extract-alcohol precipitation extract 54g, pseudo-ginseng water extract 16.92g, camphor 8g makes granule 800 grams, and 4g/ time, 2-3 time/day.
Embodiment 4:
Red sage root water was carried column extract 27g, red sage root super critical extract 4.5g, pseudo-ginseng alcohol extract 8.46g, borneol 2g makes spray 1000ml, every day 10-15ml.
Embodiment 5:
Red sage root super critical extract 4.5g, red sage root water extract 36g, pseudo-ginseng water extract 2.82g, borneol 1.5g makes 500 of capsules, each 1-2 grain, 2-3 time/day.
Embodiment 6:
Red sage root super critical extract 8g, pseudo-ginseng alcohol extract 5.64g, borneol 3g makes 260 of capsules, and each 1,1-2 time/day.
Embodiment 7:
Red sage root super critical extract 9g, pseudo-ginseng water extract 8.46g, borneol 2.54g makes 180 of capsules, and each 1,1-2 time/day.
Embodiment 8:
Red sage root super critical extract 18g, red sage root water was carried column extract 27g, pseudo-ginseng water extract 15g, borneol 3g makes 400 of soft capsules, and each 1,1-2 time/day.
Embodiment 9: compound danshen dripping pills
Red sage root 133g, pseudo-ginseng 26.3g, borneol 1.5g gets red rooted salvia and pseudo-ginseng, be ground into coarse grain, decocting boils three times, adds 6 times in water respectively, 5 times, 5 times, decocted 1,1,1 hour, merge decocting liquid, be concentrated into relative density and be 1.04, centrifugal, supernatant is crossed the D101 macroporous resin column, washing is abandoned water lotion, 60% ethanol elution, reclaim ethanol, concentrate drying, Salvia miltiorrhiza and Panax notoginseng is closed and is carried thing 7.97g; Borneol 1.5g is ground into fine powder, closes with Salvia miltiorrhiza and Panax notoginseng and carries thing and mix; By medicine: matrix adds matrix PEG6000 14.21g at 1: 1.5, mixes, and splashes in the methyl-silicone oil, makes dripping pill, totally 960 balls, every ball weight 25mg, consumption per day 30 balls.One time 10 ball, 2-3 time/day.
Embodiment 10: the compound Danshen Root particle
Red sage root 140g, pseudo-ginseng 28g, borneol 2g, get red rooted salvia and pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6 times in water respectively, 5 times, decocted 1,1 hour, merge decocting liquid, being concentrated into relative density is 1.04, leaves standstill, the DA201 macroporous resin column is crossed in ultrafiltration, filtrate, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying, must make with extra care thing 7.97g, borneol 2g is ground into fine powder, mixes, press medicinal powder: auxiliary material adds dextrin 40g at 1: 4, make particle 50g, a 1g, 2-3 time/day.
Embodiment 11: compound danshen dripping pills
Get red sage root 450g, pseudo-ginseng 141g, borneol 8g gets red rooted salvia and pulverizes (20 order), supercritical CO
2Extraction adds 30% medicinal material amount, 90% ethanol and makes entrainer, 50 ℃ of extracting pressure 28MPa, temperature, get extract 8g, behind the supercritical extract, medicinal powder is taken out, decocting boils secondary, adds 8,6 times of water gagings respectively, decocts 1,1 hour, merge decocting liquid, concentrate, add 95% ethanol and make and contain the alcohol amount and reach 70%, left standstill 12-24 hour, filter, the filtrate concentrate drying, 54g gets dry extract; Get pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6,4 times in water respectively, decocted 1,1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 7.5g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol are pulverized (80 order) and are mixed stand-by; Press medicinal powder: matrix with matrix PEG6000 fusion after adds medicine mixes at 1: 1.5, and 70 ℃ of insulations in 30 droplets/minute adding methyl-silicone oils, are collected dripping pill, absorb liquid coolant with filter paper, make 2800 balls, the heavy 70mg of every ball, day clothes 25 balls.
The dripping pill method of quality control
Assay:
A, danshensu, protocatechualdehyde (according to high performance liquid chromatography)
Get dripping pill 25 balls, put in the tool plug triangular flask, add methyl alcohol 25ml, sonicated 2 hours is put coldly, adds methyl alcohol and supplies weight, shake up, filter, get filtrate 10ml, water-bath is concentrated into dried, add water 10ml, ether 20ml is transferred in the separating funnel, divides and gets ether layer, and water layer is used 10ml extracted with diethyl ether 2 times more respectively, merge ether solution, ether solution is washed with 5ml, and washing lotion is incorporated above-mentioned water layer into, volatilizes ether, steam to a small amount of, adding methanol constant volume to the 10ml volumetric flask, be need testing solution, is contrast with the methanol solution of Sodium Danshensu; The chromatographic column octadecylsilane chemically bonded silica is a filling agent, 3: 2.5: 97=methyl alcohol: the heptanesulfonic acid sodium solution: water is moving phase, and the detection wavelength is 280nm;
B, tanshinone IIA, Cryptotanshinone (according to high performance liquid chromatography)
Get ether solution under a item, evaporate to dryness, methanol constant volume is contrast to 10ml with the methanol solution of tanshinone and the methanol solution of Cryptotanshinone; With octadecylsilane chemically bonded silica is filling agent, and 73: 27=methyl alcohol: water is moving phase, and the detection wavelength is 270nm;
C, borneol (according to vapor-phase chromatography)
It is an amount of to get n-pentadecane, and it is fixed molten to add ethyl acetate, as inner mark solution; Get dripping pill 25 balls, add inner mark solution, sonicated 2 hours filters, and gets filtrate, is contrast with the inner mark solution of borneol, is stationary phase with polyglycol-20M, and coating concentration is 10%, and column temperature is 140 ℃;
D, ginsenoside Rb
1And ginsenoside Rg
1(according to high performance liquid chromatography)
Get test sample under a item, with ginsenoside Rb
1And ginsenoside Rg
1Methanol solution for the contrast; With octadecylsilane chemically bonded silica is filling agent, and 58: 42=methyl alcohol: water is moving phase, and the detection wavelength is 203nm.
The contained danshensu of every dripping pill of present embodiment is no less than 0.096mg, and protocatechualdehyde is no less than 0.031mg.Every contained tanshinone IIA of dripping pill is no less than 0.16mg, and Cryptotanshinone is no less than 0.16mg.Every contained borneol of dripping pill is no less than 1.57mg in borneol.Every contained pseudo-ginseng of dripping pill is with the ginsenoside Rg
1Meter is no less than 0.42mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 0.84mg.
Embodiment 12 compound Danshen Root particles
Get red sage root 450g, pseudo-ginseng 141g, borneol 8g gets red rooted salvia and pulverizes (20 order), supercritical CO
2Extraction adds 30% medicinal material amount, 90% ethanol and makes entrainer, 50 ℃ of extracting pressure 28MPa, temperature, get extract 8g, behind the supercritical extract, medicinal powder is taken out, decocting boils secondary, adds 8,6 times of water gagings respectively, decocts 1,1 hour, merge decocting liquid, concentrate, add 95% ethanol and make and contain the alcohol amount and reach 70%, left standstill 12-24 hour, filter, the filtrate concentrate drying, 54g gets dry extract; Get pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6,4 times in water respectively, decocted 1,1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 7.5g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add the dextrin of 3 times of amounts of suitable medicine, make softwood, make particle 300g, each 3g, day clothes 1-2 time with the ethanol of 80% concentration.
Embodiment 13 compound capsule of red sage root
Get red sage root 450g, pseudo-ginseng 141g, borneol 8g gets red rooted salvia and pulverizes (20 order), supercritical CO
2Extraction adds 30% medicinal material amount, 90% ethanol and makes entrainer, 50 ℃ of extracting pressure 28MPa, temperature, get extract 8g, behind the supercritical extract, medicinal powder is taken out, decocting boils secondary, adds 8,6 times of water gagings respectively, decocts 1,1 hour, merge decocting liquid, concentrate, add 95% ethanol and make and contain the alcohol amount and reach 70%, left standstill 12-24 hour, filter, the filtrate concentrate drying, 54g gets dry extract; Get pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6,4 times in water respectively, decocted 1,1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 7.5g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; The dextrin that adds 2 times of amounts of suitable medicine is made 900 of capsules, and each 3, day clothes 3 times.
Embodiment 14 compound Danshen Root soft capsules
Get red sage root 450g, pseudo-ginseng 141g, borneol 8g gets red rooted salvia and pulverizes (20 order), supercritical CO
2Extraction adds 30% medicinal material amount, 90% ethanol and makes entrainer, 50 ℃ of extracting pressure 28MPa, temperature, get extract 8g, behind the supercritical extract, medicinal powder is taken out, decocting boils secondary, adds 8,6 times of water gagings respectively, decocts 1,1 hour, merge decocting liquid, concentrate, add 95% ethanol and make and contain the alcohol amount and reach 70%, left standstill 12-24 hour, filter, the filtrate concentrate drying, 54g gets dry extract; Get pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6,4 times in water respectively, decocted 1,1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 7.5g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix; The vegetable oil that adds 1 times of amount of suitable medicine, even with the colloid mill mill, make 500 of soft capsules, each 2, day clothes 2 times.
Embodiment 15 compound red sage root sprays
Get red sage root 450g, pseudo-ginseng 141g, borneol 8g gets red rooted salvia and pulverizes (20 order), supercritical CO
2Extraction adds 30% medicinal material amount, 90% ethanol and makes entrainer, 50 ℃ of extracting pressure 28MPa, temperature, get extract 8g, behind the supercritical extract, medicinal powder is taken out, decocting boils secondary, adds 8,6 times of water gagings respectively, decocts 1,1 hour, merge decocting liquid, concentrate, add 95% ethanol and make and contain the alcohol amount and reach 70%, left standstill 12-24 hour, filter, the filtrate concentrate drying, 54g gets dry extract; Get pseudo-ginseng, be ground into coarse grain, decocting boils 2 times, add 6,4 times in water respectively, decocted 1,1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 7.5g;
The red sage root is extracted, thing Notogineng Extract and borneol fine powder mix stand-by, and 20% Tween-80 ethanolic solution 100ml adds 1,2-propylene glycol 200ml, mixing, ethanol is fixed molten to 1000ml, and ethanol is fixed molten to 1000ml, the 50ml/ bottle is sub-packed in the aerosol pressure bottle, in every bottle, be pressed into dichlorodifluoromethane 2g behind the gland, make spray, daily 10-15ml.
Embodiment 16: compound danshen dripping pills
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g,
Get red rooted salvia and pulverize (20 order), supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 1 time, adds 6 times of water gagings, decocts 0.5 hour, merges decocting liquid, concentrates, and adds 95% ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 12 hours, filters, and the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 70% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 4.23g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol are pulverized (80 order) and are mixed stand-by; Press medicinal powder: matrix with matrix PEG4000 fusion after adds medicine mixes at 1: 1.3, and 80 ℃ of insulations in 40 droplets/minute adding methyl-silicone oils, are collected dripping pill, absorb liquid coolant with filter paper, and the heavy 60mg of every ball makes 1944 balls, day clothes 18 balls.
Embodiment 17: the compound Danshen Root particle
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g,
Get red rooted salvia and pulverize (20 order), supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 1 time, adds 6 times of water gagings, decocts 0.5 hour, merges decocting liquid, concentrates, and adds 95% ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 12 hours, filters, and the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 70% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 4.23g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add the microcrystalline cellulose of 4 times of amounts of suitable medicine, make softwood, make particle 250g, each 3g, day clothes 1-2 time with the ethanol of 70% concentration.
Press embodiment 11 method of quality control and measure, the moving phase of the assay of danshensu, protocatechualdehyde is 80: 19: 1=water: methyl alcohol: glacial acetic acid, and the contained danshensu of every g is no less than 1.08mg, and protocatechualdehyde is no less than 0.36mg.The contained tanshinone IIA of every g is no less than 1.8mg, and Cryptotanshinone is no less than 1.8mg.The contained borneol of every g is no less than 13.2mg in borneol.The contained pseudo-ginseng of every g is with the ginsenoside Rg
1Meter is no less than 4.28mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 8.56mg.
Embodiment 18: compound capsule of red sage root
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g,
Get red rooted salvia and pulverize (20 order), supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 1 time, adds 6 times of water gagings, decocts 0.5 hour, merges decocting liquid, concentrates, and adds 95% ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 12 hours, filters, and the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 70% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 4.23g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; The microcrystalline cellulose that adds 2 times of amounts of suitable medicine is made 600 of capsules, and each 2, day clothes 3 times.
Embodiment 19: compound red sage root spray
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g,
Get red rooted salvia and pulverize (20 order), supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 1 time, adds 6 times of water gagings, decocts 0.5 hour, merges decocting liquid, concentrates, and adds 95% ethanol and makes and contain the alcohol amount and reach 70%, leaves standstill 12 hours, filters, and the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 70% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 4.23g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by, 10% Tween-80 ethanolic solution 120ml adds 1,2-propylene glycol 80ml, mixing, ethanol is fixed molten to 1000ml, and the 50ml/ bottle is sub-packed in the aerosol pressure bottle, is pressed into dichlorodifluoromethane 7g behind the gland in every bottle, make spray, daily 10-15ml.
Embodiment 20: compound danshen dripping pills
Get red sage root 400g, pseudo-ginseng 120g, borneol 6g gets red rooted salvia and pulverizes supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 50 ℃ of extracting pressure 30MPa, temperature get red sage root super critical extract red sage root super critical extract 6.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 2 times, add 4 times of water gagings respectively, decocted 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 75% ethanol elution reclaims ethanol, concentrate drying gets red sage root water and carried the refining thing 18g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 4.23g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol pulverizing mix stand-by; Press medicinal powder: matrix with matrix PEG6000 or PEG400 fusion after adds medicine mixes 70 ℃ insulations at 1: 1.8, with inside/outside directly is to add in the methyl-silicone oil with 50 droplets/minute, collects dripping pill, absorbs liquid coolant with filter paper, make 2431 balls, the heavy 40mg of every ball, day clothes 25 balls.
Embodiment 21: the compound Danshen Root particle
Get red sage root 400g, pseudo-ginseng 120g, borneol 6g gets red rooted salvia and pulverizes supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 50 ℃ of extracting pressure 30MPa, temperature get red sage root super critical extract red sage root super critical extract 6.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 2 times, add 4 times of water gagings respectively, decocted 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 750% ethanol elution reclaims ethanol, concentrate drying gets red sage root water and carried the refining thing 18g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 4.23g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add the carboxymethyl cellulose of 4 times of amounts of suitable medicine, make softwood, make particle 180g, each 2g, day clothes 1-2 time with the ethanol of 60% concentration.
Embodiment 22: compound capsule of red sage root
Get red sage root 400g, pseudo-ginseng 120g, borneol 6g gets red rooted salvia and pulverizes supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 50 ℃ of extracting pressure 30MPa, temperature get red sage root super critical extract red sage root super critical extract 6.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 2 times, add 4 times of water gagings respectively, decocted 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 750% ethanol elution reclaims ethanol, concentrate drying gets red sage root water and carried the refining thing 18g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 4.23g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; The carboxymethyl cellulose that adds 2 times of amounts of suitable medicine is made 400 of capsules, and each 2, day clothes 4 times.
Press embodiment 11 method of quality control and measure the ginsenoside Rg
1With ginsenoside Rb
1The moving phase of assay be 99: 400=second cyanogen: 0.05% phosphoric acid solution, the contained danshensu of every capsules is no less than 0.48mg, protocatechualdehyde is no less than 0.16mg, the contained tanshinone IIA of every capsules is no less than 1mg, Cryptotanshinone is no less than 1mg, the contained borneol of every capsules is no less than 8.25mg in borneol, and the contained pseudo-ginseng of every capsules is with the ginsenoside Rg
1Meter is no less than 2.28mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 4.56mg.
Embodiment 23: compound red sage root spray
Get red sage root 400g, pseudo-ginseng 120g, borneol 6g gets red rooted salvia and pulverizes supercritical CO
2Extraction adds 40% medicinal material amount, 90% ethanol and makes entrainer, and 50 ℃ of extracting pressure 30MPa, temperature get red sage root super critical extract red sage root super critical extract 6.5g; Behind the supercritical extract, medicinal powder is taken out, decocting boils 2 times, add 4 times of water gagings respectively, decocted 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 750% ethanol elution reclaims ethanol, concentrate drying gets red sage root water and carried the refining thing 18g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 4.23g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by, 10% Tween-80 ethanolic solution 200ml adds 1,2-propylene glycol 100ml, mixing, ethanol is fixed molten to 1000ml, and the 50ml/ bottle is sub-packed in the aerosol pressure bottle, is pressed into dichlorodifluoromethane 6g behind the gland in every bottle, make spray, daily 10-15ml.
Embodiment 24: compound danshen dripping pills
Get red sage root 140g, pseudo-ginseng 28g, borneol 2g, behind the supercritical extract, medicinal powder is taken out, the medicinal powder decocting boils 2 times, add 6,5,5 times of water gagings, decocted 1.5,1,1 hours, merge decocting liquid, concentrate, add 95% ethanol and make and contain alcohol amount and reach 60%, left standstill 12 hours, filter, the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 1.68g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol pulverizing mix stand-by; Press medicinal powder: matrix with matrix PEG6000 or PEG400 fusion after adds medicine mixes at 1: 1.8, and 70 ℃ of insulations in 50 droplets/minute adding methyl-silicone oils, are collected dripping pill, absorb liquid coolant with filter paper, make 2222 balls, the heavy 50mg of every ball, day clothes 70 balls.
Embodiment 25: the compound Danshen Root particle
Red sage root water extract-alcohol precipitation extract 36g, the refining thing 1.68g of post, borneol 2g are crossed in the pseudo-ginseng alcohol extracting.
Get red sage root 140g, pseudo-ginseng 28g, borneol 2g, behind the supercritical extract, medicinal powder is taken out, the medicinal powder decocting boils 2 times, add 6,5,5 times of water gagings, decocted 1.5,1,1 hours, merge decocting liquid, concentrate, add 95% ethanol and make and contain alcohol amount and reach 60%, left standstill 12 hours, filter, the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 1.68g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add the sodium carboxymethyl starch of 3 times of amounts of suitable medicine, make softwood, make particle 160g, each 5g, day clothes 1-2 time with the ethanol of 80% concentration.
Embodiment 26: compound capsule of red sage root
Red sage root water extract-alcohol precipitation extract 36g, the refining thing 1.68g of post, borneol 2g are crossed in the pseudo-ginseng alcohol extracting.
Get red sage root 140g, pseudo-ginseng 28g, borneol 2g, behind the supercritical extract, medicinal powder is taken out, the medicinal powder decocting boils 2 times, add 6,5,5 times of water gagings, decocted 1.5,1,1 hours, merge decocting liquid, concentrate, add 95% ethanol and make and contain alcohol amount and reach 60%, left standstill 12 hours, filter, the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 1.68g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; The sodium carboxymethyl starch that adds 1 times of amount of suitable medicine is made 300 of capsules, and each 3, day clothes 3 times.
Embodiment 27: compound red sage root spray
Get red sage root 140g, pseudo-ginseng 28g, borneol 2g, behind the supercritical extract, medicinal powder is taken out, the medicinal powder decocting boils 2 times, add 6,5,5 times of water gagings, decocted 1.5,1,1 hours, merge decocting liquid, concentrate, add 95% ethanol and make and contain alcohol amount and reach 60%, left standstill 12 hours, filter, the filtrate concentrate drying gets red sage root water extract-alcohol precipitation extract 36g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 1.68g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by; 15% Tween-80 ethanolic solution 100ml, ethanol is fixed molten to 300ml, adds 1,2-propylene glycol 30ml, mixing, ethanol is fixed molten to 300ml, and the 60ml/ bottle is sub-packed in the aerosol pressure bottle, in every bottle, be pressed into dichlorodifluoromethane 1g behind the gland, make spray, daily 15ml.
Measure by embodiment 11 method of quality control: every milliliter of contained danshensu is no less than 0.28mg, and protocatechualdehyde is no less than 0.09mg.Every milliliter of contained borneol is no less than 3.6mg in borneol.Every milliliter of contained pseudo-ginseng is with the ginsenoside Rg
1Meter is no less than 0.71mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 0.76mg.
Embodiment 28: compound danshen dripping pills
Get red sage root 133g, pseudo-ginseng 26g, borneol 1.5g, red sage root decocting boils 2 times, adds 4 times of water gagings respectively, decocts 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 75% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing 8g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 1.56g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol pulverizing mix stand-by; Press medicinal powder: the adding medicine mixed matrix with after the matrix PEG4000 fusion in 1: 1.5, and 80 ℃ of insulations in 60 droplets/minute adding methyl-silicone oils, are collected dripping pill, absorb liquid coolant with filter paper, get dripping pill 922 balls, the heavy 30mg of every ball, and day is obeyed 31 balls.
Pressing embodiment 11 method of quality control measures: the ginsenoside Rg
1With ginsenoside Rb
1The moving phase of assay be 3: 7=second cyanogen: water, every contained danshensu of dripping pill is no less than 0.07mg, protocatechualdehyde is no less than 0.023mg.Every contained borneol of dripping pill is no less than 0.89mg in borneol.Every contained pseudo-ginseng of dripping pill is with the ginsenoside Rg
1Meter is no less than 0.21mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 0.42mg.
Embodiment 29: the compound Danshen Root particle
Get red sage root 133g, pseudo-ginseng 26g, borneol 1.5g, red sage root decocting boils 2 times, adds 4 times of water gagings respectively, decocts 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 75% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing 8g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 1.56g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add 4 times of amounts of suitable medicine-cyclodextrin, make softwood with the ethanol of 60% concentration, make particle 55g, each 2g, day clothes 1-2 time.
Embodiment 30: compound capsule of red sage root
Get red sage root 133g, pseudo-ginseng 26g, borneol 1.5g, red sage root decocting boils 2 times, adds 4 times of water gagings respectively, decocts 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 75% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing 8g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 1.56g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add 2 times of amounts of suitable medicine-cyclodextrin, make 120 of particles, each 2, day clothes 2 times.
Embodiment 31: compound red sage root spray
Get red sage root 133g, pseudo-ginseng 26g, borneol 1.5g, red sage root decocting boils 2 times, adds 4 times of water gagings respectively, decocts 1 hour, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 75% ethanol elution, reclaim ethanol, concentrate drying gets red sage root water and carried the refining thing 8g of post; Get pseudo-ginseng, be ground into coarse grain, decocting boils 3 times, add 6,5,4 times in water respectively, decocted 1.5,1,1 hours, merge decocting liquid, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, washing, abandon water lotion, 70% ethanol elution reclaims ethanol, concentrate drying gets pseudo-ginseng water extract 1.56g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by; Add 15% Tween-80 ethanolic solution 100ml, ethanol is fixed molten to 300ml, adds 1,2-propylene glycol 30ml, mixing, ethanol is fixed molten to 300ml, and the 100ml/ bottle is sub-packed in the aerosol pressure bottle, in every bottle, be pressed into dichlorodifluoromethane 1g behind the gland, make spray, daily 10-15ml.
Embodiment 32: compound danshen dripping pills
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g
Get red rooted salvia and pulverize supercritical CO
2Extraction adds 40% medicinal material amount, 95% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 2.82g;
With Salvia root P.E, refining thing of pseudo-ginseng and borneol pulverizing mix stand-by; Press medicinal powder: matrix with matrix PEG4000 fusion after adds medicine mixes at 1: 1.5, and 80 ℃ of insulations in 30 droplets/minute adding methyl-silicone oils, are collected dripping pill, absorb liquid coolant with filter paper, make 1332 balls, the heavy 25mg of every ball, day clothes 12 balls.
Embodiment 33: the compound Danshen Root particle
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g
Get red rooted salvia and pulverize supercritical CO
2Extraction adds 40% medicinal material amount, 95% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 2.82g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; Add the dextrin of 4 times of amounts of suitable medicine, make softwood, make particle 70g, each 0.7g, day clothes 1-2 time with the ethanol of 60% concentration.
Embodiment 34: compound capsule of red sage root
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g
Get red rooted salvia and pulverize supercritical CO
2Extraction adds 40% medicinal material amount, 95% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 2.82g;
Press recipe quantity with Salvia root P.E, Notogineng Extract and borneol fine powder mix; The dextrin that adds 2 times of amounts of suitable medicine is made 150 of particles, each 1-2 grain, day clothes 3 times.
Embodiment 35: the compound Danshen Root soft capsule
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g
Get red rooted salvia and pulverize supercritical CO
2Extraction adds 40% medicinal material amount, 95% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 2.82g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix; The vegetable oil that adds 1.5 times of amounts of suitable medicine, even with the colloid mill mill, make 200 of soft capsules, each 1, day clothes 2 times.
Press embodiment 11 method of quality control and measure the ginsenoside Rg
1With ginsenoside Rb
1The amino normal phase column of assay, moving phase is 87: 13=second cyanogen: 1% phosphoric acid, every contained tanshinone IIA of dripping pill is no less than 2.25mg, every contained borneol of dripping pill is no less than 16.5mg in borneol.Every contained pseudo-ginseng of dripping pill is with the ginsenoside Rg
1Meter is no less than 5.35mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 10.7mg.
Embodiment 36: compound red sage root spray
Get red sage root 450g, pseudo-ginseng 141g, borneol 6g
Get red rooted salvia and pulverize supercritical CO
2Extraction adds 40% medicinal material amount, 95% ethanol and makes entrainer, and 35 ℃ of extracting pressure 23MPa, temperature get red sage root super critical extract 4.5g; Get pseudo-ginseng, be ground into coarse grain, add 60% alcohol reflux 3 times, each 1 hour, extract reclaimed ethanol, be concentrated into relative density and be 1-1.1, centrifugal, supernatant is crossed macroporous resin column, and water lotion is abandoned in washing, 60% ethanol elution reclaims ethanol, and concentrate drying gets pseudo-ginseng alcohol extract 2.82g;
With Salvia root P.E, Notogineng Extract and borneol fine powder mix stand-by; Add 15% Tween-80 ethanolic solution 120ml, add 1,2-propylene glycol 80ml, mixing, it is fixed molten to 800ml to add ethanol again, and the 100ml/ bottle is sub-packed in the aerosol pressure bottle, is pressed into dichlorodifluoromethane 4g behind the gland in every bottle, makes spray, daily 8-10ml.
Claims (1)
1. the method for quality control of a compound danshen dripping pills is characterized in that its content assaying method comprises the steps:
A, danshensu, protocatechualdehyde assay:
Get dripping pill 25 balls, put in the tool plug triangular flask, add methyl alcohol 25ml, sonicated 2 hours, put coldly, add methyl alcohol and supply weight, shake up, filter, get filtrate 10ml, water-bath is concentrated into dried, adds water 10ml, ether 20ml is transferred in the separating funnel, divide and get ether layer, water layer is used 10ml extracted with diethyl ether 2 times more respectively, merge ether solution, ether solution is washed with 5ml, washing lotion is incorporated above-mentioned water layer into, volatilizes ether, steams to a small amount of, add methanol constant volume to the 10ml volumetric flask, being need testing solution, is contrast with the methanol solution of Sodium Danshensu, and the chromatographic column octadecylsilane chemically bonded silica is a filling agent, 3: 2.5: 97 methyl alcohol-heptanesulfonic acid sodium solution-water is moving phase, and the detection wavelength is 280nm;
B, tanshinone IIA, Cryptotanshinone assay
Get A item ether solution, evaporate to dryness, methanol constant volume is contrast to 10ml with the methanol solution of tanshinone and the methanol solution of Cryptotanshinone, is filling agent with octadecylsilane chemically bonded silica, and 73: 27 methanol-waters are moving phase, and the detection wavelength is 270nm;
C, content of bornyl alcohol are measured
It is an amount of to get n-pentadecane, and it is fixed molten to add ethyl acetate, as inner mark solution; Get dripping pill 25 balls, add inner mark solution, sonicated 2 hours filters, and gets filtrate, is contrast with the inner mark solution of borneol, is stationary phase with polyglycol-20M, and coating concentration is 10%, and column temperature is 140 ℃;
D, ginsenoside Rb
1And ginsenoside Rg
1
Get test sample under the A item, with ginsenoside Rb
1And ginsenoside Rg
1Methanol solution for the contrast, be filling agent with octadecylsilane chemically bonded silica, 58: 42 methanol-waters are moving phase, the detection wavelength is 203nm;
Every contained danshensu of dripping pill is no less than 0.096mg, and protocatechualdehyde is no less than 0.031mg; Every contained tanshinone IIA of dripping pill is no less than 0.16mg, and Cryptotanshinone is no less than 0.16mg; Every contained borneol of dripping pill is no less than 1.57mg in borneol; Every contained pseudo-ginseng of dripping pill is with the ginsenoside Rg
1Meter is no less than 0.42mg, with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter is no less than 0.84mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021573794A CN100412545C (en) | 2002-12-23 | 2002-12-23 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021573794A CN100412545C (en) | 2002-12-23 | 2002-12-23 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1419124A CN1419124A (en) | 2003-05-21 |
| CN100412545C true CN100412545C (en) | 2008-08-20 |
Family
ID=4752955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021573794A Expired - Lifetime CN100412545C (en) | 2002-12-23 | 2002-12-23 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100412545C (en) |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339706C (en) * | 2003-06-19 | 2007-09-26 | 北京中医药大学 | Quality control method of injection agent for treating apoplexia |
| CN1333248C (en) * | 2003-07-14 | 2007-08-22 | 北京中医药大学 | Chinese medicine quality control method |
| CN100381813C (en) * | 2004-03-16 | 2008-04-16 | 天津天士力制药股份有限公司 | Quality control of compound Danshen root drops |
| WO2005088295A1 (en) * | 2004-03-17 | 2005-09-22 | Tianjin Tasly Pharmaceutical Co., Ltd. | A quality controlling method for the compound danshen dropping pills |
| CN100381817C (en) * | 2004-03-17 | 2008-04-16 | 天津天士力制药股份有限公司 | Quality control of compound Danshen root drops |
| CN1327217C (en) * | 2004-05-26 | 2007-07-18 | 江西江中药业股份有限公司 | Quality control of Jianweixiaoshi tablets for promotnig digest |
| CN100390538C (en) * | 2005-06-20 | 2008-05-28 | 中国医学科学院药用植物研究所 | Detection method for dammarane type four-ring triterpenoid saponin |
| CN1919243B (en) * | 2005-08-24 | 2011-03-23 | 天津天士力制药股份有限公司 | Traditional medicine composition for treating cardiovascular and cerebrovascular diseases |
| CN1919251B (en) * | 2005-08-24 | 2010-11-03 | 天津天士力制药股份有限公司 | Traditional Chinese medicine composition for treating cardiac vascular disease |
| CN1919240B (en) * | 2005-08-24 | 2011-02-16 | 天津天士力制药股份有限公司 | Traditional Chinese medicine for treating cardiovascular and cerebrovascular diseases |
| CN100458421C (en) * | 2005-09-28 | 2009-02-04 | 沈百华 | Microchemical identifying method for wild ginseng and cultivated gineeng |
| CN101574359B (en) * | 2008-05-09 | 2011-09-14 | 昆明制药集团股份有限公司 | Pharmaceutical composition for treating cardiovascular and cerebrovascular disease |
| CN101607954B (en) * | 2008-06-18 | 2012-10-24 | 复旦大学 | Danshensu derivative, preparation method thereof, and application thereof in pharmacy |
| CN102309543B (en) * | 2010-06-30 | 2014-01-01 | 广东环球制药有限公司 | Compound salvia miltiorrhiza concentrated preparation and preparation and detection method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074121A (en) * | 1992-10-24 | 1993-07-14 | 广西卫生学校附属药厂 | A kind of production method for the treatment of the coronary heart disease Chinese medicinal tablet |
| CN1144673A (en) * | 1995-09-04 | 1997-03-12 | 张相国 | Red sage root and its composite compound red sage root powder injection and preparation method |
| CN1322951A (en) * | 2001-06-29 | 2001-11-21 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
-
2002
- 2002-12-23 CN CNB021573794A patent/CN100412545C/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1074121A (en) * | 1992-10-24 | 1993-07-14 | 广西卫生学校附属药厂 | A kind of production method for the treatment of the coronary heart disease Chinese medicinal tablet |
| CN1144673A (en) * | 1995-09-04 | 1997-03-12 | 张相国 | Red sage root and its composite compound red sage root powder injection and preparation method |
| CN1322951A (en) * | 2001-06-29 | 2001-11-21 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1419124A (en) | 2003-05-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100412545C (en) | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease | |
| CN101612362B (en) | Complex preparation for regulating lipid and preventing and curing heart cerebrovascular diseases and preparation method thereof | |
| CN101116722A (en) | Pharmaceutical formulations with the raw material containing panax, ophiopogon root and schisandra fruit, processes for their preparation, the raw material and the quality control method for the prepa | |
| CN102228506A (en) | Composition of malaytea scurfpea extract as well as preparation method and use thereof | |
| JP2001508777A (en) | Pine needle extract and its use | |
| CN1421241A (en) | Compound red sage drip pill for treating cardiac and cerebral vascular diseases and its prepn process | |
| CN1296063C (en) | Compound red sage prepn for treating cardiac and cerebral vascular diseases and its prepn process | |
| CN107913277A (en) | The purposes of the anti-uric acid nephropathy of tanshinone | |
| CN100421683C (en) | Composite red sage root micro-capsules for cardio-cerebral diseases and its preparing method | |
| CN1923228B (en) | Pharmaceutical composition comprising notoginseng extract, Danshen extract and ligustrazine | |
| CN1872099B (en) | Medication for treating cardiovascular diseases, and cerebrovascular disease | |
| CN101766699B (en) | Medicinal combination containing musk | |
| CN101732409B (en) | Salvia miltiorrhiza soft capsule and preparation method thereof | |
| CN1422664A (en) | Compound preparation of root of red-rooted salvia for treating cerebrovascular and cardiovascular diseases and preparation method thereof | |
| CN1421242A (en) | Compound red sage capsule for treating cardiac and cerebral vascular diseases and its prepn process | |
| CN1424088A (en) | Composite red sage root granules for cardio-cerebral diseases and its preparing method | |
| CN1319519C (en) | Composite red sage root spray for cardio-cerebral diseases and its preparing method | |
| CN100584357C (en) | Medicine composition containing borneol and musk | |
| CN101766703B (en) | Medicinal combination containing borneol and musk | |
| CN101766702B (en) | Medicinal combination containing borneol and musk | |
| CN100584356C (en) | Musk containing medicine composition | |
| CN101664452A (en) | Drug combination containing musk | |
| KR20140114398A (en) | Uses of danshen or danshen preparation in preparation of drugs for treating diseases related to hepatic fibrosis | |
| CN101766705B (en) | Medicinal combination containing borneol and musk | |
| CN103784504B (en) | A kind of Chinese medicine composition and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: TIANJIN TASLY PHARMACY CO., LTD. Free format text: FORMER OWNER: BEIJING CAIRUI MEDICAL TECHNOLOGY CO., LTD. Effective date: 20100420 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C56 | Change in the name or address of the patentee |
Owner name: BEIJING CAIRUI MEDICAL TECHNOLOGY CO., LTD. Free format text: FORMER NAME: BEIJING CAIRUI MEDICINE CO., LTD. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100029 ROOM 601, WEITE OFFICE BUILDING, NO.A11,NORTH 3RD RING EAST ROAD, CHAOYANG DISTRICT, BEIJING CITY TO: 300410 TIANSHILI MODERM CHINESE MEDICINE CITY, NO.2, PUJIHE EAST ROAD, BEICHEN DISTRICT, TIANJIN CITY |
|
| CP03 | Change of name, title or address |
Address after: 100029, Witt, office building 11, 601 North Third Ring Road, Beijing, Chaoyang District Patentee after: BEIJING CAIRUI MEDICAL TECHNOLOGY Co.,Ltd. Address before: 100029, Beijing, Chaoyang District cherry garden, 19 floor, 507 Patentee before: BEIJING CAIRUI MEDICINE Co.,Ltd. |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20100420 Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee after: TIANJIN TASLY PHARMACEUTICAL Co.,Ltd. Address before: 100029, Witt, office building 11, 601 North Third Ring Road, Beijing, Chaoyang District Patentee before: BEIJING CAIRUI MEDICAL TECHNOLOGY Co.,Ltd. |
|
| C56 | Change in the name or address of the patentee |
Owner name: TASLY PHARMACEUTICAL GROUP CO., LTD. Free format text: FORMER NAME: TIANJIN TASLY PHARMACEUTICAL CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee after: TASLY PHARMACEUTICAL GROUP Co.,Ltd. Address before: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee before: TIANJIN TASLY PHARMACEUTICAL Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee after: TASLY PHARMACEUTICAL GROUP Co.,Ltd. Address before: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee before: TASLY PHARMACEUTICAL GROUP Co.,Ltd. |
|
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20080820 |