CN1448141A - Medicine with total dogwood glycosides as main component for treating chronic nephritis and its production process - Google Patents
Medicine with total dogwood glycosides as main component for treating chronic nephritis and its production process Download PDFInfo
- Publication number
- CN1448141A CN1448141A CN 03114630 CN03114630A CN1448141A CN 1448141 A CN1448141 A CN 1448141A CN 03114630 CN03114630 CN 03114630 CN 03114630 A CN03114630 A CN 03114630A CN 1448141 A CN1448141 A CN 1448141A
- Authority
- CN
- China
- Prior art keywords
- fructus corni
- total glycosides
- medicine
- amount
- hours
- 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.)
- Granted
Links
- 150000002338 glycosides Chemical class 0.000 title claims abstract description 95
- 229930182470 glycoside Natural products 0.000 title claims abstract description 93
- 239000003814 drug Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 206010018367 Glomerulonephritis chronic Diseases 0.000 title abstract description 18
- 229940079593 drug Drugs 0.000 title description 11
- 240000006766 Cornus mas Species 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 131
- 238000005251 capillar electrophoresis Methods 0.000 claims abstract description 55
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 238000012544 monitoring process Methods 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000000857 drug effect Effects 0.000 claims abstract description 5
- 239000003480 eluent Substances 0.000 claims description 40
- 238000007639 printing Methods 0.000 claims description 29
- 238000010828 elution Methods 0.000 claims description 23
- 239000000284 extract Substances 0.000 claims description 22
- 238000005515 capillary zone electrophoresis Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 20
- 238000004244 micellar electrokinetic capillary chromatography Methods 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000007853 buffer solution Substances 0.000 claims description 13
- 239000000546 pharmaceutical excipient Substances 0.000 claims description 11
- 230000006837 decompression Effects 0.000 claims description 10
- 238000011010 flushing procedure Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000006210 lotion Substances 0.000 claims description 10
- 239000002075 main ingredient Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000825 ultraviolet detection Methods 0.000 claims description 8
- 239000002775 capsule Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 241000203998 [Candida] fructus Species 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000002552 dosage form Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 231100000419 toxicity Toxicity 0.000 claims description 4
- 230000001988 toxicity Effects 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 12
- 241001465754 Metazoa Species 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 4
- 208000024891 symptom Diseases 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 241000209020 Cornus Species 0.000 abstract 2
- 238000002474 experimental method Methods 0.000 abstract 2
- 239000012467 final product Substances 0.000 abstract 2
- 231100000053 low toxicity Toxicity 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 230000002110 toxicologic effect Effects 0.000 abstract 1
- 231100000027 toxicology Toxicity 0.000 abstract 1
- 229920002472 Starch Polymers 0.000 description 7
- 230000005012 migration Effects 0.000 description 7
- 238000013508 migration Methods 0.000 description 7
- 235000019698 starch Nutrition 0.000 description 7
- 239000008107 starch Substances 0.000 description 7
- 210000002700 urine Anatomy 0.000 description 7
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 6
- 241000699670 Mus sp. Species 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 239000000872 buffer Substances 0.000 description 4
- 201000010099 disease Diseases 0.000 description 4
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 4
- 238000002651 drug therapy Methods 0.000 description 4
- 210000003734 kidney Anatomy 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229920002307 Dextran Polymers 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 206010030113 Oedema Diseases 0.000 description 3
- 230000003110 anti-inflammatory effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229940109239 creatinine Drugs 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 210000002966 serum Anatomy 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 206010020772 Hypertension Diseases 0.000 description 2
- 241000699666 Mus <mouse, genus> Species 0.000 description 2
- PNNCWTXUWKENPE-UHFFFAOYSA-N [N].NC(N)=O Chemical compound [N].NC(N)=O PNNCWTXUWKENPE-UHFFFAOYSA-N 0.000 description 2
- 239000000427 antigen Substances 0.000 description 2
- 102000036639 antigens Human genes 0.000 description 2
- 108091007433 antigens Proteins 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 229940088597 hormone Drugs 0.000 description 2
- 239000005556 hormone Substances 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 230000003053 immunization Effects 0.000 description 2
- 238000002649 immunization Methods 0.000 description 2
- 230000001506 immunosuppresive effect Effects 0.000 description 2
- 229960003444 immunosuppressant agent Drugs 0.000 description 2
- 230000001861 immunosuppressant effect Effects 0.000 description 2
- 239000003018 immunosuppressive agent Substances 0.000 description 2
- 230000002757 inflammatory effect Effects 0.000 description 2
- 210000000629 knee joint Anatomy 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000002398 materia medica Substances 0.000 description 2
- 210000004914 menses Anatomy 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 201000008383 nephritis Diseases 0.000 description 2
- 230000001575 pathological effect Effects 0.000 description 2
- 239000008194 pharmaceutical composition Substances 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 206010001580 Albuminuria Diseases 0.000 description 1
- 208000037157 Azotemia Diseases 0.000 description 1
- 102000004506 Blood Proteins Human genes 0.000 description 1
- 108010017384 Blood Proteins Proteins 0.000 description 1
- 241000759833 Cornus officinalis Species 0.000 description 1
- CMSMOCZEIVJLDB-UHFFFAOYSA-N Cyclophosphamide Chemical compound ClCCN(CCCl)P1(=O)NCCCO1 CMSMOCZEIVJLDB-UHFFFAOYSA-N 0.000 description 1
- 102000004127 Cytokines Human genes 0.000 description 1
- 108090000695 Cytokines Proteins 0.000 description 1
- 208000008967 Enuresis Diseases 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 208000022461 Glomerular disease Diseases 0.000 description 1
- 206010018364 Glomerulonephritis Diseases 0.000 description 1
- 239000009636 Huang Qi Substances 0.000 description 1
- 108060003951 Immunoglobulin Proteins 0.000 description 1
- 206010062016 Immunosuppression Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000013901 Nephropathies and tubular disease Diseases 0.000 description 1
- 206010030302 Oliguria Diseases 0.000 description 1
- 208000009205 Tinnitus Diseases 0.000 description 1
- 241000545405 Tripterygium Species 0.000 description 1
- HLXRWTJXGMHOFN-XJSNKYLASA-N Verbenalin Chemical class O([C@@H]1OC=C([C@H]2C(=O)C[C@H](C)[C@H]21)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HLXRWTJXGMHOFN-XJSNKYLASA-N 0.000 description 1
- 208000012886 Vertigo Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 208000019790 abdominal distention Diseases 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 231100000215 acute (single dose) toxicity testing Toxicity 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003178 anti-diabetic effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 230000002917 arthritic effect Effects 0.000 description 1
- 230000002146 bilateral effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 229960004397 cyclophosphamide Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- UREBDLICKHMUKA-CXSFZGCWSA-N dexamethasone Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@]2(F)[C@@H]1[C@@H]1C[C@@H](C)[C@@](C(=O)CO)(O)[C@@]1(C)C[C@@H]2O UREBDLICKHMUKA-CXSFZGCWSA-N 0.000 description 1
- 229960003957 dexamethasone Drugs 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000003118 histopathologic effect Effects 0.000 description 1
- 208000026278 immune system disease Diseases 0.000 description 1
- 102000018358 immunoglobulin Human genes 0.000 description 1
- 230000007233 immunological mechanism Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 238000009592 kidney function test Methods 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 206010025135 lupus erythematosus Diseases 0.000 description 1
- 231100000682 maximum tolerated dose Toxicity 0.000 description 1
- 201000008350 membranous glomerulonephritis Diseases 0.000 description 1
- 230000027939 micturition Effects 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000010172 mouse model Methods 0.000 description 1
- 230000002560 nonimmunologic effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008506 pathogenesis Effects 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 230000007170 pathology Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 231100000886 tinnitus Toxicity 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 210000003556 vascular endothelial cell Anatomy 0.000 description 1
- 231100000889 vertigo Toxicity 0.000 description 1
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a Chinese patent medicine for treating chronic nephritis, which is prepared by extracting total glycoside effective parts from a single traditional Chinese medicine dogwood and adding auxiliary materials. In particular to a medicine for treating chronic nephritis by taking the effective part of the total glycosides of the dogwood as the main component, an extraction method, a preparation method and a monitoring method thereof, and the toxicological and efficacy and clinical test results of the medicine. The preparation method comprises pulverizing Corni fructus, soaking in 70% ethanol, reflux-extracting, enriching total glycosides with macroporous resin, vacuum drying, and making into final product. The capillary electrophoresis Corni fructus fingerprint chromatogram is used for monitoring the production process of Corni fructus total glycoside extraction, preparation and final product. Animal experiments and drug effect experiments show that the medicine has low toxicity and has obvious treatment effect on chronic nephritis model animals; clinical observation shows that the medicine has obvious curative effect on chronic nephritis, the effective rate of clinical symptoms reaches 90 percent, and no toxic or side effect is seen. The invention has obvious social benefit and economic benefit.
Description
One. technical field
The present invention relates to Fructus Corni total glycosides is the Drug therapy chronic nephritis and the production technology thereof of Main Ingredients and Appearance, is specifically related to a kind of Chinese patent medicine for the treatment of chronic nephritis.
Two. background technology
Chronic glomerulonephritis means that the bilateral glomerule diffusivity of the different pathological types that a variety of causes causes or focal inflammation change, clinical onset concealment, and the course of disease is tediously long, and PD is the general name of one group of primary glomerulopathy slowly.Most scholars think that this disease may cause by immunologic mechanism, the inflammatory mediator factor and non-immunologic mechanism etc. owing to infection such as various antibacterials, virus or protozoons.This disease pathogeny can be summarized as: circulating immune complex deposition, the formation of original position immune complex, cellular immunization and glomerular injury, inflammatory mediator and effect of cytokines etc.Basic therapeutic scheme is: 1) general treatment: as lie up, restriction Sal is taken in, and regulates diet etc.; 2) hormone, immunosuppressant treatment etc.; 3) azotemia is handled.If now the drug main hormones that adopts clinically, cyclophosphamide, tripterygium glycosides etc., these medicine life-time service all produce serious toxic and side effects, and some patients can not use these medicines because of contraindication.Therefore, develop the natural Chinese medicine for the treatment of chronic nephritis safely, effectively and have its important society and economic worth.
Fructus Corni (Cornus officinalis Sieb.et Zucc.), another name another name for Sichuan Province Fructus Jujubae, Mus arrow, chicken foot, Fructus Corni, real Fructus Jujubae, Fructus Corni and Fructus Corni etc. are one of Chinese medicine common first names precious medicinal materials.All there are distribution and cultivation in ground such as China Zhejiang, Henan, Shandong, Anhui, Jiangsu, Shanxi, Shaanxi, Sichuan.Its sour in the mouth of Fructus Corni, puckery, slightly warm in nature is returned the Liver and kidney warp, and the effect of liver and kidney tonifying, essence astringing and desertion stemming is arranged.Cure mainly vertigo and tinnitus, soreness of waist and knee joint, impotence and seminal emission, enuresis frequent micturition, bleeding not during menses, profuse sweating collapse, interior-heat is quenched one's thirst.The medicinal record the earliest of Fructus Corni sees Shennong's Herbal, classifies middle product as; The Pharmacopoeia of the People's Republic of China (version in 2000) also records.In chief editors such as chief editors' such as Chen Keji " newly organized delay aging drug " and Zhou Jinhuang " Pharmacology and Clinics of Chinese Materia Medica progress " the Chinese materia medica to Fructus Corni carried out elaboration.Fructus Corni often becomes compound recipe with other drug matching clinically.
Modern pharmacology studies show that, Fructus Corni has effects such as regulating immune, antibiotic, shock, anticoagulant, anti-diabetic, anti-hepatic injury, and clinical effectiveness is good, and safety, toxic and side effects are low.Zhao Shiping etc. (China-Japan Friendship Hospital's journal, 1996,10 (4), 294-298) early studied anti inflammatory immunity inhibitory action in the body of Fructus Corni general glycoside; Zhao Wushu etc. (Chinese microbiology and Journal of Immunology, 1995,15 (5), 325-327) studied the Fructus Corni general glycoside to immunity in the mice body with to the influence of heart transplant survival; Guo Lili etc. (Chinese Journal of Immunology, 2002,18 (3), 197-199) preliminary study the arthritic immunization mechanism of Fructus Corni total glycosides resisting rheumatoid disease; (Shanghai Journal of Immunology such as Li Jianmin, 2001,21 (5), 298-299) reported the Fructus Corni general glycoside to HUVEC express alpha 4 and the plain influence of β 7 integration, think that it may be one of the main antiinflammatory of Fructus Corni total glycosides and immunosuppression mechanism that inhibition vascular endothelial cell express alpha 4 and β 7 integrate elements; (Chinese patent database CN:1310011) has been announced a kind of medicine that immune disease kidney that lupus erythematosus causes decreases for the treatment of to Ding Congli etc., wherein is made up of 16 flavor medicines such as Cortex Moutan, the Radix Astragali, Fructus Corni.
Zhao Shiping etc. (CN_1148968) introduce a kind of extraction process with Fructus Corni extract of immunosuppressive action and antiinflammatory action, use polarity or nonpolar macroporous adsorption resin, ethanol elution, vacuum drying.But the not mentioned composition that extracts is a Fructus Corni total glycosides, and the isolating sample of macroporous adsorbent resin that this patent adopts is the water decoction extract of Fructus Corni.
At present, Fructus Corni total glycosides yet there are no report as the Drug therapy chronic nephritis of Main Ingredients and Appearance and production technology thereof and economy quality-monitoring research efficiently.
Three, summary of the invention
The object of the invention is to provide a kind of medicine for the treatment of chronic nephritis.
Another object of the present invention provides the production technology of a kind of Fructus Corni total glycosides as the Drug therapy chronic nephritis of Main Ingredients and Appearance.
The technical scheme that realizes the object of the invention comprises following step: 1) extract Fructus Corni total glycosides effective site; 2) preparation; The capillary electrophoresis fingerprint monitoring of 3) Fructus Corni total glycosides extraction, preparation and finished product; 4) toxicity and drug effect; 5) clinical observation.A. extract Fructus Corni total glycosides effective site
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening is first with 8 times of soak with ethanol 6-12 hours of measuring 70% concentration, heated 65 ℃～75 ℃ reflux, extract, 2～4 hours, and filtered, medicinal residues continue to add the alcohol reflux 2～4 hours of 6 times of amount 70% concentration, filter, merge extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.05～1.10 (60 ℃) for 45 ℃～60 ℃ in temperature;
4). with concentrated solution stand at low temperature (4～10 ℃) 24 hours, get supernatant, cross macroporous resin D
101, the diameter 40cm of pillar and height 200cm, earlier with 5～7 times of amount pure water rinsing, eluent flow rate 20～25ml/min, the water lotion reject is used the alcohol flushing of 10～30% concentration instead, and eluent becomes clear by mixing, and eluent discards; Continue to collect 50%～80% ethanol elution with 5～6 times of amount 50～80% ethanol elutions; Each step of capillary electrophoresis (CE) the finger printing monitoring elution process that provides with the present invention.
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 60～90 parts of Fructus Corni total glycosides, 10～40 parts of mixing and stirring of yellow starch gum (or other excipient), be divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.Capillary zone electrophoresis (CZE) optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm (internal diameter 50 μ m, effectively separation length 50cm); The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV (+) → (-), 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography (MECC): 30mM SDS, 50mM borate buffer solution, pH9.5, the same CZE of other condition.D. toxicity and drug effect
1). toxicity
Acute toxicity testing studies show that, gives mouse stomach with 4 parts of Fructus Corni total glycosides effective sites and 3 parts of yellow starch gum preparations, measures maximum tolerated dose, LD
50＞30g/kg (in Fructus Corni crude drug amount) illustrates that this poison of drug is less.
2). drug effect
The present invention is based on the immunology pathogenesis of chronic glomerulonephritis and Fructus Corni general glycoside pathology pharmacological research conclusion as immunosuppressant, can infer at first theoretically that the Fructus Corni general glycoside has good curative effect to chronic glomerulonephritis, this is a theoretical basis of the present invention.
Fructus Corni total glycosides is to the effect research of rat Heymann nephritis model.Press document (Zhang Jingbo etc., Chinese Journal of Nephrology, 1999,15 (3), 158-161) duplicate rat Heymann glomerulonephritis model, animal pattern is divided into model group, Fructus Corni total glycosides group, positive controls at random (selects dexamethasone for use, 0.1mg/kg), other establishes the blank group, and every treated animal is no less than 15.Gastric infusion 15 days is determined dosage by the frequency or the drug level of administration every day.Observation index comprises qualitative, quantitative urine protein, serum creatinine and blood urea nitrogen, immune globulin Pseudobulbus Bletillae (Rhizoma Bletillae) complement and pathological examination etc.Press t significance test deal with data, the result shows: the Fructus Corni total glycosides preparation can reduce serum creatinine content and the twenty-four-hour urine protein content of animal pattern and alleviate the glomerule lesion degree.
The laboratory observation Fructus Corni total glycosides is to the therapeutical effect of mice IgA nephritis.Press document (Mo Rong etc., Chinese Journal of Nephrology, 1989,5 (2), 123-127) use dextran (Dextran) as antigen, bring out mice IgA nephritis, the treatment of experimentizing property of medication, the content of observation urine protein content, serum urea nitrogen (BUN), creatinine (SCr).Get kidney and carry out perusal and histopathologic examination's discovery, behind the injected in mice antigen, albuminuria occurs, serum BUN raises.After the Fructus Corni total glycosides treatment, the mice body weight there is reduction trend, may be gently relevant with the model mice edema, and can significantly reduce urine protein (P＜0.01); Fructus Corni total glycosides 10g/kg group can obviously reduce the content (P＜0.05) of BUN in the blood; Fructus Corni total glycosides has certain mitigation to the glomerule pathological changes that Dextran causes.E. clinical observation
The medicine (capsule) that with the Fructus Corni total glycosides is Main Ingredients and Appearance is used for the treatment of chronic nephritis, Preliminary Clinical Observation 50 examples.Select case by chronic nephritis diagnostic criteria (new Chinese medicine clinical research guideline, version in 2002), wherein plain edition (30 example), hypertension type (10 example), acute attack type (10 example).Continuous oral 3 months, every day 3 times, each 4 (every amount that is equivalent to 2g Fructus Corni crude drug) is parameters for observation on effect with urine protein, renal function, edema, hypertension etc.The result shows, total effective rate 80%; Tcm symptom (soreness of waist and knee joint, abdominal distention, the tired power of body, oliguria, edema etc.) remission rate 95%, urine protein correction rate 30%.Menses, urine, just conventional, liver function (ALT, AST) and kidney function test, patient's no abnormal change in back of taking medicine; Do not see untoward reaction.This show this medicine can within a short period of time relieve chronic nephritis symptom, improve patient's whole body functional condition, delay nephridial tissue and effect such as further damage.And take nontoxic, safety and economy for a long time.
Four. description of drawings
Fig. 1 Fructus Corni alcohol extraction thing CZE characteristic fingerprint pattern;
Fig. 2 Fructus Corni alcohol extraction thing MECC characteristic fingerprint pattern;
Fig. 3 Fructus Corni total glycosides effective site CZE finger printing;
Fig. 4 Fructus Corni total glycosides effective site MECC finger printing.
Five. the specific embodiment
Below in conjunction with the embodiment that accompanying drawing and inventor provide, the present invention is described in further detail.
By optimization to conditions such as buffer kind, concentration, pH value, micellar concentration and column temperatures, same for test agent under same instrument, capillary column and close buffer conditions, two kinds of finger printing that separating mechanism is different of acquisition.Optimum Fructus Corni extract finger printing condition is seen (three c).
Shown in Figure 1, Fructus Corni alcohol extraction thing CZE characteristic fingerprint pattern, deposition condition comprises buffer: Borax 50mM, pH9.5; Voltage: 22kV (+) → (-); 30 ℃ of capillary tube column temperatures; Pressure sample introduction 5psi * sec; The 200nm ultraviolet detection;
Shown in Figure 2, Fructus Corni alcohol extraction thing MECC characteristic fingerprint pattern, the Borax 50mM of deposition condition buffer: pH9.5, SDS:30mM; Voltage: 22kV (+) → (-); 30 ℃ of capillary tube column temperatures; Pressure sample introduction 5psi * sec; The 200nm ultraviolet detection;
Shown in Figure 3, Fructus Corni total glycosides effective site CZE finger printing (the same Fig. 1 of deposition condition);
Shown in Figure 4, Fructus Corni total glycosides effective site MECC finger printing (the same Fig. 2 of deposition condition).
In sum, Fig. 1～4 are respectively Fructus Corni alcohol extraction thing and CZE and the MECC chemical feature finger printing of Fructus Corni total glycosides effective site under optimal conditions.And obtain the basic parameters such as migration time, peak area, relative migration time and area percentage of Fructus Corni CZE and each characteristic peak of MECC characteristic fingerprint pattern simultaneously.These finger printing data are the bases of formulating the Fructus Corni quality control standard.
Fructus Corni alcohol extraction thing is through ether defatting, water-saturated n-butanol extraction, and dehydration, obtains Fructus Corni total glycosides effective site.Fructus Corni total glycosides effective site is compared with Fructus Corni alcohol extraction thing, and its saponin content enlarges markedly, and other composition significantly reduces or disappear (as polysaccharide, esters etc.).The peak number of optimal conditions CZE and MECC Fructus Corni alcohol extraction thing characteristic fingerprint pattern (Fig. 1 and Fig. 2) is respectively 39 and 41, and Fructus Corni total glycosides finger printing (Fig. 3 and Fig. 4) peak number is 13 and 20.The CZE finger printing of contrast Fructus Corni alcohol extraction thing (Fig. 1) and Fructus Corni total glycosides effective site (Fig. 3) just can be found, the component of Fig. 1 migration time 19.63min (No. 1 peak), the component of migration time 19.66min in the corresponding diagram 3 (No. 1 peak), its relative peak area rises to 50.66% of Fig. 3 from 8.97% of Fig. 1.In MECC, the component of Fig. 2 migration time 20.48min (No. 7 peaks), the component of migration time 20.58min in the corresponding diagram 4 (No. 8 peaks), its relative peak area rises to 51.16% of Fig. 4 from 9.56% of Fig. 2.This and Fructus Corni alcohol extraction thing obtain Fructus Corni total glycosides effective site through n-butanol extraction, and it is consistent supplying the fact of the chemical compound proportion increase of test agent glycoside structure.In addition, borate buffer solution CE collection of illustrative plates migration time lags behind and supports from another point of view that also this peak is this inference of chemical compound of cornin class formation.
Two kinds of pattern finger printing of the CZE of Fructus Corni ethanol extract and Fructus Corni total glycosides effective site and MECC are stable under optimal conditions, meet the correlation technique requirement of finger printing.
Below be pharmaceutical composition, the Fructus Corni total glycosides effective site extracting method embodiment that the inventor provides.
1. pharmaceutical composition embodiment
Embodiment 1: contain 60～90 parts of Fructus Corni total glycosides in the medicine, 10～40 parts of yellow starch gums.
Embodiment 2: contain 65～85 parts of Fructus Corni total glycosides in the medicine, 15～35 parts of yellow starch gums.
Embodiment 3: contain 70～80 parts of Fructus Corni total glycosides in the medicine, 20～30 parts of yellow starch gums.
Embodiment 4: contain 65～70 parts of Fructus Corni total glycosides in the medicine, 25～35 parts of yellow starch gums.
Embodiment 5: contain 60～90 parts of Fructus Corni alcohol extraction things in the medicine, 10～40 parts of yellow starch gums.
2. Fructus Corni total glycosides effective site extracting method
Method 1:
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 6 hours, heat 70 ℃ of reflux, extract, 2 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.05 (60 ℃) for 50 ℃ in temperature;
4). concentrated solution low temperature (4 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 20% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 50% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.
Method 2:
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 8 hours, heat 70 ℃ of reflux, extract, 3 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.08 (60 ℃) for 50 ℃ in temperature;
4). concentrated solution low temperature (5 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 30% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 60% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.
Method 3:
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 10 hours, heat 70 ℃ of reflux, extract, 4 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.07 (60 ℃) for 60 ℃ in temperature;
4). concentrated solution low temperature (8 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 10% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 70% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.
Method 4:
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 8 hours, heat 72 ℃ of reflux, extract, 2 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.06 (60 ℃) for 55 ℃ in temperature;
4). with concentrated solution stand at low temperature (4 ℃) 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 20% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 80% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.
Claims (10)
1. one kind is the medicine of Main Ingredients and Appearance with the Fructus Corni total glycosides, comprises following step: 1) extract Fructus Corni total glycosides effective site; 2) preparation; The capillary electrophoresis fingerprint monitoring of 3) Fructus Corni total glycosides extraction, preparation and finished product; 4) toxicity and drug effect; 5) clinical observation is characterized in that containing in this medicine 60～90 parts of Fructus Corni total glycosides effective sites, 10～40 parts of excipient.
2. according to claim 1 is the medicine of Main Ingredients and Appearance with the Fructus Corni total glycosides, it is characterized in that containing in this medicine 65～85 parts of Fructus Corni total glycosides effective sites, 25～35 parts of excipient.
3. according to claim 1 is the medicine of Main Ingredients and Appearance with the Fructus Corni total glycosides, it is characterized in that containing in this medicine 70～80 parts of Fructus Corni total glycosides effective sites, 20～30 parts of excipient.
4. according to claim 1 is the medicine of Main Ingredients and Appearance with the Fructus Corni total glycosides, it is characterized in that containing in this medicine 75～85 parts of Fructus Corni total glycosides effective sites, 25～35 parts of excipient.
5. according to claim 1 is the medicine of Main Ingredients and Appearance with the Fructus Corni total glycosides, it is characterized in that containing in this medicine 80～90 parts of Fructus Corni total glycosides effective sites, 10～20 parts of excipient.
6. one kind is used the described medicine production technology of claim 1, and it is characterized in that production technology undertaken by following step: a. extracts Fructus Corni total glycosides effective site 1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved; 2). the powder of Fructus Corni of crushing screening is first with 8 times of soak with ethanol 6-12 hours of measuring 70% concentration, add
65 ℃～75 ℃ reflux, extract, of heat 2～4 hours filter, and medicinal residues continue to add 6 times of amount 70% concentration
Alcohol reflux 2～4 hours, filter, merge extracted twice liquid; 3). decompression and solvent recovery, be concentrated into the alcohol amount 20% that contains for 45 ℃～60 ℃ in temperature, relative density 1.05～
1.10, in the time of 60 ℃, measure; 4). concentrated solution 4～10 ℃ of stand at low temperature 24 hours, is got supernatant, cross macroporous resin D
101, post
The diameter 40cm of son and height 200cm are earlier with 5～7 times of amount pure water rinsing, eluent flow rate
20～25ml/min, the water lotion reject is used the alcohol flushing of 10～30% concentration instead, eluent by
It is clear to mix change, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, collection 50%～
80% ethanol elution; Each step with capillary electrophoresis fingerprint monitoring elution process.5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol,
The thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 60～90 parts of Fructus Corni total glycosides, 10～40 parts of mixing and stirring of excipient, be divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.The capillary zone electrophoresis optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm: internal diameter 50 μ m, effectively separation length 50cm; The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV+ →-, 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography: 30mM SDS, 50mM borate buffer solution, pH9.5, the same capillary zone electrophoresis of other condition.
7. one kind is used the described medicine production technology of claim 1, and it is characterized in that production technology undertaken by following step: a. extracts Fructus Corni total glycosides effective site
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 6 hours, heat 70 ℃ of reflux, extract, 2 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.05 (60 ℃) for 50 ℃ in temperature;
4). concentrated solution low temperature (4 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 20% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 50% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 65～85 parts of Fructus Corni total glycosides effective sites, 25～35 parts of mixing and stirring of excipient are divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.The capillary zone electrophoresis optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm: internal diameter 50 μ m, effectively separation length 50cm; The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV+ →-, 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography: 30mM SDS, 50mM borate buffer solution, pH9.5, the same capillary zone electrophoresis of other condition.
8. one kind is used the described medicine production technology of claim 1, and it is characterized in that production technology undertaken by following step: a. extracts Fructus Corni total glycosides effective site
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 8 hours, heat 70 ℃ of reflux, extract, 3 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.08 (60 ℃) for 50 ℃ in temperature;
4). concentrated solution low temperature (5 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 30% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 60% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 70～80 parts of Fructus Corni total glycosides effective sites, 20～30 parts of mixing and stirring of excipient are divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.The capillary zone electrophoresis optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm: internal diameter 50 μ m, effectively separation length 50cm; The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV+ →-, 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography: 30mM SDS, 50mM borate buffer solution, pH9.5, the same capillary zone electrophoresis of other condition.
9. one kind is used the described production technology of claim 6, and it is characterized in that production technology undertaken by following step: a. extracts Fructus Corni total glycosides effective site
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 10 hours, heat 70 ℃ of reflux, extract, 4 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.07 (60 ℃) for 60 ℃ in temperature;
4). concentrated solution low temperature (8 ℃) was left standstill 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 10% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 70% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 75～85 parts of Fructus Corni total glycosides effective sites, 25～35 parts of mixing and stirring of excipient are divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.The capillary zone electrophoresis optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm: internal diameter 50 μ m, effectively separation length 50cm; The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV+ →-, 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography: 30mM SDS, 50mM borate buffer solution, pH9.5, the same capillary zone electrophoresis of other condition.
10. one kind is used the described medicine production technology of claim 1, and it is characterized in that production technology undertaken by following step: a. extracts Fructus Corni total glycosides effective site
1). at first Fructus Corni sarcocarp is cleaned, dries, pulverizes, sieved;
2). the powder of Fructus Corni of crushing screening earlier with the soak with ethanol of 8 times of amount 70% concentration 8 hours, heat 72 ℃ of reflux, extract, 2 hours, filter, medicinal residues continue to add the alcohol reflux 2 hours of 6 times of amount 70% concentration, filtration, merging extracted twice liquid;
3). decompression and solvent recovery is concentrated into the alcohol amount of containing 20%, relative density 1.06 (60 ℃) for 55 ℃ in temperature;
4). with concentrated solution stand at low temperature (4 ℃) 24 hours, get supernatant, cross macroporous resin D
101Earlier with 5～7 times of amount pure water rinsing, diameter of pillar (40cm) and height 200cm), eluent flow rate 20～25ml/min, capillary electrophoresis (CE) the finger printing monitoring total glycosides index that provides with the present invention refers to the water lotion reject, use the alcohol flushing of 20% concentration instead, eluent becomes clear by mixing, and monitors relevant index with CE, and eluent discards; Continue with 5～6 times of amount 50～80% ethanol elutions, flow velocity 20～25ml/min, 80% ethanol elution is collected in the monitoring of CE finger printing;
5). collect eluent, 50 ℃～60 ℃ distilling under reduced pressure, vacuum is 0.088Mpa, reclaims ethanol, the thick paste of gained promptly gets Fructus Corni total glycosides behind vacuum drying.B. preparation
With 80～90 parts of Fructus Corni total glycosides effective sites, 10～20 parts of mixing and stirring of excipient are divided in the capsule or make tablet or make the pharmaceutically any dosage form of acceptable.The capillary zone electrophoresis optimal conditions of the capillary electrophoresis fingerprint monitoring Fructus Corni alcohol extraction thing chemistry characteristic fingerprint pattern of c. Fructus Corni total glycosides extraction, preparation and finished product is: coating elasticity is not melted silicon capillary 54cm: internal diameter 50 μ m, effectively separation length 50cm; The 50mM borate buffer solution, pH9.5; Pressure sample introduction 5psi * sec, operating voltage 22kV+ →-, 200nm ultraviolet detection on the post, 30 ℃ of column temperatures.The optimal conditions of micellar electrokinetic capillary chromatography: 30mM SDS, 50mM borate buffer solution, pH9.5, the same capillary zone electrophoresis of other condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03114630 CN1224397C (en) | 2003-04-11 | 2003-04-11 | Medicine for treating chronic nephritis and production process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03114630 CN1224397C (en) | 2003-04-11 | 2003-04-11 | Medicine for treating chronic nephritis and production process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1448141A true CN1448141A (en) | 2003-10-15 |
| CN1224397C CN1224397C (en) | 2005-10-26 |
Family
ID=28684130
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03114630 Expired - Fee Related CN1224397C (en) | 2003-04-11 | 2003-04-11 | Medicine for treating chronic nephritis and production process thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1224397C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389162A (en) * | 2011-08-04 | 2012-03-28 | 深圳烟草工业有限责任公司 | Method for preparing cornus officinalis extract, application in cigarettes and cigarette |
-
2003
- 2003-04-11 CN CN 03114630 patent/CN1224397C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389162A (en) * | 2011-08-04 | 2012-03-28 | 深圳烟草工业有限责任公司 | Method for preparing cornus officinalis extract, application in cigarettes and cigarette |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1224397C (en) | 2005-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1515286A (en) | Chinese medicinal herb extractive | |
| CN102058673B (en) | Chinese medicine composition for expelling wind and removing dampness and preparation method thereof | |
| CN101062074A (en) | Compound of sphaeria sinensis and panax notoginseng extract and the application thereof in the preventing and treating of pulmonary fibrosis | |
| CN102872015B (en) | Stephanotis total alkaloid extract as well as preparation method and application thereof | |
| CN1775261A (en) | Mingmu-Dihuang preparation and new preparing method | |
| CN1923263A (en) | Traditional Chinese medicine composition, its preparing method and quality controlling means | |
| EP1825860A1 (en) | A panaxatriol saponins composition and its preparing method and the use | |
| CN1067901C (en) | Drug for curing migraine and its preparing method | |
| CN100479837C (en) | Weinakang for treating ischemic cerebrovascular disease and senile dementia and preparation method thereof | |
| CN1224397C (en) | Medicine for treating chronic nephritis and production process thereof | |
| CN101023979A (en) | Lamiophlomis-rotata leaf-stem distract and its preparing process and use | |
| CN1762359A (en) | Lindera root alkaloid, its preparation method and application in medicine preparation | |
| CN1853688A (en) | Chinese medicinal preparation for treating heart cerebrovascular disease and ischemic apoplexia and making method thereof | |
| CN1712060A (en) | Preparation of Chinese medicinal mixture for treating gynecologic menstrual disease | |
| CN109674747B (en) | Preparation method for reducing toxic and side effects of girald daphne bark injection | |
| CN103239618A (en) | Traditional Chinese medicine composition for treating chronic hepatitis and cirrhosis and preparation method thereof | |
| CN1241586C (en) | Chinese medicine composition and preparing method thereof | |
| CN1296087C (en) | Compound capsule for treating apoplexy involving the meridians of wind phlegm stasis blockage syndrome type and preparation process thereof | |
| CN113368209B (en) | New use of QIZHI Capsule in preparing medicine for treating essential hypertension | |
| CN104173413B (en) | Application of centella asiatica leaf total terpenoids in preparation of anti-rheumatoid arthritis drugs | |
| CN110215474B (en) | Traditional Chinese medicine composition for promoting blood circulation to remove blood stasis and application thereof | |
| CN1333044A (en) | Wasting-thirst hypoglycemic preparation | |
| CN1442165A (en) | Chinese medicine for treating chronic nephritis and its preparation method | |
| CN1242755C (en) | Chinese traditional medicine extracts and its preparation and application in pharmacy | |
| CN1276760C (en) | Chinese medicine composition and its preparing method |
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 | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |