CN1840050A - Quality control method of 'Jia Wei Huo Xiang' soft capsule - Google Patents
Quality control method of 'Jia Wei Huo Xiang' soft capsule Download PDFInfo
- Publication number
- CN1840050A CN1840050A CN 200610001043 CN200610001043A CN1840050A CN 1840050 A CN1840050 A CN 1840050A CN 200610001043 CN200610001043 CN 200610001043 CN 200610001043 A CN200610001043 A CN 200610001043A CN 1840050 A CN1840050 A CN 1840050A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- weight portion
- jiawei
- adds
- 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
- 239000007901 soft capsule Substances 0.000 title claims abstract description 58
- 238000003908 quality control method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000000341 volatile oil Substances 0.000 claims abstract description 23
- 244000303040 Glycyrrhiza glabra Species 0.000 claims abstract description 5
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 3
- 235000004347 Perilla Nutrition 0.000 claims abstract 2
- 244000124853 Perilla frutescens Species 0.000 claims abstract 2
- 239000002994 raw material Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 74
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 70
- VVOAZFWZEDHOOU-UHFFFAOYSA-N magnolol Chemical compound OC1=CC=C(CC=C)C=C1C1=CC(CC=C)=CC=C1O VVOAZFWZEDHOOU-UHFFFAOYSA-N 0.000 claims description 62
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- 238000012360 testing method Methods 0.000 claims description 53
- 239000013558 reference substance Substances 0.000 claims description 36
- 239000000047 product Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000009711 Huoxiang-zhengqi Substances 0.000 claims description 25
- 239000003208 petroleum Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 20
- BYTORXDZJWWIKR-UHFFFAOYSA-N Hinokiol Natural products CC(C)c1cc2CCC3C(C)(CO)C(O)CCC3(C)c2cc1O BYTORXDZJWWIKR-UHFFFAOYSA-N 0.000 claims description 18
- FVYXIJYOAGAUQK-UHFFFAOYSA-N honokiol Chemical compound C1=C(CC=C)C(O)=CC=C1C1=CC(CC=C)=CC=C1O FVYXIJYOAGAUQK-UHFFFAOYSA-N 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 239000003814 drug Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000004809 thin layer chromatography Methods 0.000 claims description 12
- 241001619461 Poria <basidiomycete fungus> Species 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 238000003556 assay Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 8
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 239000012085 test solution Substances 0.000 claims description 8
- 229940079593 drug Drugs 0.000 claims description 6
- 238000004811 liquid chromatography Methods 0.000 claims description 6
- 239000001100 (2S)-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chroman-4-one Substances 0.000 claims description 4
- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 claims description 4
- APSNPMVGBGZYAJ-GLOOOPAXSA-N clematine Natural products COc1cc(ccc1O)[C@@H]2CC(=O)c3c(O)cc(O[C@@H]4O[C@H](CO[C@H]5O[C@@H](C)[C@H](O)[C@@H](O)[C@H]5O)[C@@H](O)[C@H](O)[C@H]4O)cc3O2 APSNPMVGBGZYAJ-GLOOOPAXSA-N 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims description 4
- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 claims description 4
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 claims description 4
- 229940025878 hesperidin Drugs 0.000 claims description 4
- 235000011477 liquorice Nutrition 0.000 claims description 4
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001738 pogostemon cablin oil Substances 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- 238000011003 system suitability test Methods 0.000 claims description 4
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 4
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 4
- 235000012141 vanillin Nutrition 0.000 claims description 4
- SRCZQMGIVIYBBJ-UHFFFAOYSA-N ethoxyethane;ethyl acetate Chemical compound CCOCC.CCOC(C)=O SRCZQMGIVIYBBJ-UHFFFAOYSA-N 0.000 claims description 2
- 241000202807 Glycyrrhiza Species 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 17
- 238000004821 distillation Methods 0.000 abstract description 10
- 241001529821 Agastache Species 0.000 abstract 1
- 241000213006 Angelica dahurica Species 0.000 abstract 1
- 244000080767 Areca catechu Species 0.000 abstract 1
- 241000132012 Atractylodes Species 0.000 abstract 1
- 235000017443 Hedysarum boreale Nutrition 0.000 abstract 1
- 235000007858 Hedysarum occidentale Nutrition 0.000 abstract 1
- 241001673966 Magnolia officinalis Species 0.000 abstract 1
- 241001522129 Pinellia Species 0.000 abstract 1
- 240000002505 Pogostemon cablin Species 0.000 abstract 1
- 235000011751 Pogostemon cablin Nutrition 0.000 abstract 1
- 244000197580 Poria cocos Species 0.000 abstract 1
- 235000008599 Poria cocos Nutrition 0.000 abstract 1
- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 abstract 1
- 238000004886 process control Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 27
- 241000238370 Sepia Species 0.000 description 15
- 239000003205 fragrance Substances 0.000 description 15
- 239000004519 grease Substances 0.000 description 15
- 239000007787 solid Substances 0.000 description 13
- 239000000284 extract Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 description 7
- MPDGHEJMBKOTSU-UHFFFAOYSA-N Glycyrrhetinsaeure Natural products C12C(=O)C=C3C4CC(C)(C(O)=O)CCC4(C)CCC3(C)C1(C)CCC1C2(C)CCC(O)C1(C)C MPDGHEJMBKOTSU-UHFFFAOYSA-N 0.000 description 7
- 229960003720 enoxolone Drugs 0.000 description 7
- WNIFXKPDILJURQ-UHFFFAOYSA-N stearyl glycyrrhizinate Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C)CCC(C(=O)OCCCCCCCCCCCCCCCCCC)(C)CC5C4=CC(=O)C3C21C WNIFXKPDILJURQ-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 241000699670 Mus sp. Species 0.000 description 5
- 229920001971 elastomer Polymers 0.000 description 5
- 238000002481 ethanol extraction Methods 0.000 description 5
- 206010047700 Vomiting Diseases 0.000 description 4
- 239000007766 cera flava Substances 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 238000000748 compression moulding Methods 0.000 description 4
- 239000006071 cream Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- -1 filter Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 230000008673 vomiting Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 238000000540 analysis of variance Methods 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000693 micelle Substances 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- SBNFWQZLDJGRLK-UHFFFAOYSA-N phenothrin Chemical compound CC1(C)C(C=C(C)C)C1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 SBNFWQZLDJGRLK-UHFFFAOYSA-N 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 102000003712 Complement factor B Human genes 0.000 description 2
- 108090000056 Complement factor B Proteins 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- 241000322338 Loeseliastrum Species 0.000 description 2
- 241000699666 Mus <mouse, genus> Species 0.000 description 2
- 239000005662 Paraffin oil Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000008991 intestinal motility Effects 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012567 medical material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000010773 plant oil Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229930003347 Atropine Natural products 0.000 description 1
- 241000272201 Columbiformes Species 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- RKUNBYITZUJHSG-UHFFFAOYSA-N Hyosciamin-hydrochlorid Natural products CN1C(C2)CCC1CC2OC(=O)C(CO)C1=CC=CC=C1 RKUNBYITZUJHSG-UHFFFAOYSA-N 0.000 description 1
- 206010061245 Internal injury Diseases 0.000 description 1
- 208000019790 abdominal distention Diseases 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000001142 anti-diarrhea Effects 0.000 description 1
- RKUNBYITZUJHSG-SPUOUPEWSA-N atropine Chemical compound O([C@H]1C[C@H]2CC[C@@H](C1)N2C)C(=O)C(CO)C1=CC=CC=C1 RKUNBYITZUJHSG-SPUOUPEWSA-N 0.000 description 1
- 229960000396 atropine Drugs 0.000 description 1
- 230000000741 diarrhetic effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- ALWKGYPQUAPLQC-UHFFFAOYSA-N neostigmine Chemical compound CN(C)C(=O)OC1=CC=CC([N+](C)(C)C)=C1 ALWKGYPQUAPLQC-UHFFFAOYSA-N 0.000 description 1
- 229960002362 neostigmine Drugs 0.000 description 1
- 239000002547 new drug Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 210000000813 small intestine Anatomy 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparing process and quality control method of agastache soft capsule, wherein patchouli, purple perilla, dahurian angelica root, white atractylodes rhizome, dried orange peel, pinellia tuber, magnolia bark, poria cocos, root of ballon flower, licorice root, areca catecha are used as the raw materials, and the preparing process consists of ethanol extracting, extracting volatile oil through vapor distillation, watering and boiling, decompressing and drying, disintegrating into fines, sieving, jevigating and pressing into soft capsules. The disclosed quality control method comprises an authentication method and a content determination method.
Description
Patent application of the present invention is for dividing an application, and the original bill application number is 200310122427.0, and the applying date is December in 2003 23 days, and denomination of invention is a kind of preparation method and method of quality control of 'Jia Wei Huo Xiang ' soft capsule.
Technical field
The present invention relates to a kind of preparation of soft capsule method and method of quality control, particularly relate to a kind of preparation method and method of quality control of 'Jia Wei Huo Xiang ' soft capsule.
Background technology
What use in the market is JIAWEI HUOXIANG ZHENGQI WAN, be mainly used in diseases such as affection of exogenous wind-cold, internal injury humidity hysteresis, the confused weight of headache, abdominal distention, vomiting diarrhea clinically, but said preparation is that conventional dosage forms and quality controllability are poor.The invention discloses a kind of 'Jia Wei Huo Xiang ' soft capsule, and to preparation of soft capsule technology, method of quality control is studied, made this dosage form have better controllability and stability.
Summary of the invention
The object of the invention is to provide a kind of preparation method and method of quality control of 'Jia Wei Huo Xiang ' soft capsule.
The present invention seeks to be achieved through the following technical solutions.
Prescription:
Herba Pogostemonis 300-350 weight portion Folium Perillae 90-110 weight portion
The Radix Angelicae Dahuricae 90-110 weight portion Rhizoma Atractylodis Macrocephalae (stir-fry) 180-220 weight portion
Pericarpium Citri Reticulatae 180-220 weight portion Rhizoma Pinelliae (processed) 180-220 weight portion
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 180-220 weight portion Poria 90-110 weight portion
Radix Platycodonis 180-220 weight portion Radix Glycyrrhizae 180-220 weight portion
Pericarpium Arecae 90-110 weight portion.
Method for making: above ten simply, Cortex Magnoliae Officinalis 50-80% ethanol extraction 2-3 time, and each 1-2 hour, filter, merging filtrate reclaims ethanol, and being concentrated into relative density is the clear paste A of 1.15 (80 ℃); Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Dahuricae vapor distillation extract volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The medicinal residues and the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Rhizoma Zingiberis Recens 30-35 weight portion and Fructus Jujubae 50-55 weight portion decoct with water 2-3 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned aqueous solution merge, be concentrated into 80 ℃ of following relative densities and be 1.12 clear paste, centrifugal, supernatant concentration to relative density is the clear paste B of 1.15 (80 ℃); Merge clear paste A and B, be concentrated into the thick paste of relative density for (80 ℃) 1.30-1.35, drying under reduced pressure is ground into fine powder, sieves; Other gets edible vegetable oil 340-380 weight portion, and it is an amount of to add Cera Flava etc., and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into soft capsule; Every heavy 0.6g of soft capsule content is equivalent to crude drug 2.157g.
The method for making of soft capsule of the present invention can also for: above ten simply, and Cortex Magnoliae Officinalis is with 50-80% ethanol extraction 2-3 time, each 1-2 hour, filter, merging filtrate, recovery ethanol, being concentrated into relative density is the clear paste A of 1.15 (80 ℃); Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Dahuricae vapor distillation extract volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The medicinal residues and the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Rhizoma Zingiberis Recens 30-35 weight portion and Fructus Jujubae 50-55 weight portion decoct with water 2-3 time, each 1-2 hour, collecting decoction, merge with above-mentioned aqueous solution, filter, filtrate is concentrated into the clear paste that relative density is 1.12 (80 ℃), and is centrifugal, and supernatant concentration to relative density is the clear paste B of 1.15 (80 ℃); With clear paste A drying under reduced pressure, be ground into fine powder, sieve.With clear paste B, being concentrated into relative density is the thick paste of 1.30-1.35 (80 ℃), and drying under reduced pressure is ground into fine powder, sieves.The above-mentioned extract powder of mixing adds volatile oil and refined plant oil, Cera Flava is an amount of, and is even through the colloid mill mill, is pressed into soft capsule.
Soft capsule preparation moulding process: the preparation of soft capsule rubber solution
Get certain 1～2: 0.01～0.05: 1～2 glycerol, Brown Ferric Oxide and water, be heated to 70-80 ℃, mix homogeneously adds 1～2 part of gelatin and stirs, fusion, insulation was left standstill 1-2 hour, made the foam come-up, scrape off the foam of come-up, filter heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, medicinal liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains medicine is compression moulding, the soft capsule micelle of compression moulding sent in the hothouse that dehydrating unit is housed under 25-30 ℃ of temperature, carry out drying, allow moisture slowly evaporates in the rubber, and stir micelle gently frequently, to prevent adhesion, be 4-6 hour drying time; Use the washing with alcohol soft capsule, the soft capsule after the washing is sent into hothouse once more, and drying is about 12-18 hour under 30-35 ℃ of temperature, promptly gets the soft capsule finished product.
Soft capsule quality control method of the present invention:
Differentiate: get soft capsule content 2g of the present invention, put in the 500ml round-bottomed flask, add water 200-300ml, mixing, connect volatile oil determination apparatus, add water to scale from the determinator upper end, and till overflow goes in the flask, add petroleum ether 1-3ml again, connect reflux condensing tube, be heated to and boil, and kept little 1-3 of boiling hour, put coldly, divide and to get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds petroleum ether and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with 0.5% sodium carboxymethyl cellulose, with 8-12: 0.8-1.2 petroleum ether-ethyl acetate is developing solvent, launch, take out, dry, spray is with 2% vanillin sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Get soft capsule content 2g of the present invention, the jolting that adds diethyl ether is extracted 2-3 time, each 20ml, discard ether solution, residue is waved most ether, adds water 40ml and makes dissolving, adds water saturated n-butanol extraction 2-3 time, each 30ml, merge n-butyl alcohol liquid, filter evaporate to dryness, residue adds methanol 5ml makes dissolving, as need testing solution; Other gets the hesperidin reference substance, adds methanol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to thin layer chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, with 0.8-1.2: the 0.8-1.2 acetone-water is developing solvent, launches, and takes out, and dries, and spray is put under the ultra-violet lamp and inspected with 1% aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show same color fluorescence speckle;
Get soft capsule content 2g of the present invention, add petroleum ether 20-40ml, supersound process 20-40 minute, discard petroleum ether, volatilize, residue adds chloroform 20-30ml and hydrochloric acid 1-3ml, put in the water-bath reflux 1-1.5 hour, and filtered the filtrate evaporate to dryness, residue adds methanol 1-3ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add methanol and make the solution that every 1ml contains 0.5mg, product solution according to the thin layer chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively in same be on the silica GF254 lamellae of binding agent with 0.5% sodium carboxymethyl cellulose, with 28-32: 12-16: 0.8-1.2 toluene-ethyl acetate-formic acid is developing solvent, launches, and takes out, dry, put under the uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; 72-76: 23-26 methanol-water is mobile phase; Flow velocity 1ml/min; Detect wavelength 294nm; Column temperature is a room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800;
The preparation of reference substance solution, precision take by weighing magnolol and the honokiol reference substance is an amount of, and add methanol and make the mixed solution that every 1ml contains magnolol 25-35ug, honokiol 20-30ug, mixing, promptly; The preparation of need testing solution, precision take by weighing the about 2g of soft capsule of the present invention, and precision adds 50-70% ethanol 15-25ml, weigh, supersound process 30-50 minute, weigh again, supply solvent and subtract the weight of mistake, shake well filters, discard filtrate just, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, uses the 50-60% ethanol dilution to scale, shake up, promptly;
Algoscopy, accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures, promptly; Soft capsule of the present invention contains Cortex Magnoliae Officinalis in the total amount of magnolol (C18H1802) with honokiol (C18H1802), must not be less than 0.9mg.
The JIAWEI HUOXIANG ZHENGQI RUANJIAONANG test of pesticide effectiveness proves, after JIAWEI HUOXIANG ZHENGQI RUANJIAONANG is oral, can increase the intestinal propulsion function of normal mouse; Atropine induced mice intestinal motility is suppressed model, after JIAWEI HUOXIANG ZHENGQI RUANJIAONANG is oral tangible excitation is arranged; To the excited model of neostigmine induced mice intestinal motility, JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has the obvious suppression effect.Show that motion has dual regulation to JIAWEI HUOXIANG ZHENGQI RUANJIAONANG to mouse small intestine.JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has significant analgesia role, and Dichlorodiphenyl Acetate induced mice writhing response has the obvious suppression effect.JIAWEI HUOXIANG ZHENGQI RUANJIAONANG has tangible anti-diarrhea effect, can obviously prolong Folium Sennae induced mice diarrheal incubation period, reduces mice diarrhoea number of times within a certain period of time.To pigeon vomiting model due to the CUS04, this medicine can prolong vomiting incubation period, reduces the vomiting number of times.
Experimental example 1 Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Dahuricae Study on extraction
The volatile oil extraction and application rate of Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, the Radix Angelicae Dahuricae as investigating index, is selected for use L9 (3
4) orthogonal scheme, investigate soak time, powder particle diameter, amount of water, extraction time four factors, in conjunction with producing reality, each factor is chosen 3 levels, sees Table 1.
Table 1 experimental factor water-glass
Experiment and data:
Taking by weighing Herba Pogostemonis 150g, Folium Perillae 50g, Pericarpium Citri Reticulatae 100g, Rhizoma Atractylodis Macrocephalae 100g, Radix Angelicae Dahuricae 50g five kinds of Chinese medicine extraction volatile oil, is index with the extraction and application rate, sees Table 2.
(L9 (3 for table 2 orthogonal experiment design table
4))
Attached: through check, Herba Pogostemonis Volatile oil content 2.11%, Folium Perillae volatile oil content 0.73%, Pericarpium Citri Reticulatae volatile oil content are 1.94%, and Rhizoma Atractylodis Macrocephalae volatile oil content is 0.52%, and Radix Angelicae Dahuricae volatile oil content is 0.4%.By the R value as can be known, factor A is very little to experimental result influence, thus with the sum of sguares of deviation from mean of factor A as error estimation.In order to other factors are carried out significance test, see Table 3.
Table 3 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean (S) | Degree of freedom (f) | Mean square (z) | The F value | P | Significance |
| B C D error e | 182.92 20.88 586.69 7.66 | 2 2 2 2 | 91.46 10.44 293.34 3.83 | 23.88 2.73 76.59 | ＜0.05 ＜0.05 | Significantly |
Conclusion: as shown in Table 3, factor B, D to the experimental result influence significantly can be known by inference by table 2,
B1D2 is an optimised process, is coarse powder about 0.5cm so the extraction process of five tastes medical material volatile oil is selected pulverizing medicinal materials is become particle diameter, and it is an amount of to add water, vapor distillation 8 hours.
Experimental example 2 Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) Study on extraction
With the content of magnolol, honokiol in the high effective liquid chromatography for measuring Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), select L9 (3 for use
4) be orthogonal scheme, investigate concentration of alcohol, soak time, extraction time, ethanol consumption, extraction time each factor, actual in conjunction with producing, each factor is chosen 3 levels, and extraction time, ethanol consumption, extraction time merged into a factor, testing program sees Table 4.
Table 4 experimental factor water-glass
Experiment and data: taking by weighing Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 200g by the requirement of experimental design scheme and extract, with the content of magnolol honokiol in the high effective liquid chromatography for measuring Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), serves as to investigate index with the extraction and application rate, sees Table 5.
Table 5 Orthogonal Experiment and Design table
Attached: through check, magnolol and honokiol total amount are 2.1% in the Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens).
D classifies blank column as, carries out significance test so be listed as test error with D, sees Table 6.
Table 6 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean S | Degree of freedom f | Mean square z | The F value | P | Significance |
| A B C error e | 894·89 304·27 348·45 17·31 | 2 2 2 2 2 | 447·44 152·14 174·22 8·66 | 51·67 17·57 20·12 | ＜0·05 ＜0·05 | Significantly |
Conclusion: as can be seen from Table 6, significantly sex to experimental result is A, next is factor C, and factor B is not remarkable to the experiment influence, shows according to table 5, the optimised process that Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) is extracted is A3C3, promptly use 60% ethanol extraction three times, for the first time 6 times of amount 60% ethanol, 4 times of amount 60% ethanol for the second time, for the third time with 4 times of amount 60% ethanol, each 1 hour.
The Study on extraction of experimental example 3 all the other flavour of a drug
To the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Fructus Jujubae, Rhizoma Zingiberis Recens and the Herba Pogostemonis after extracting volatile oil, Folium Perillae, Pericarpium Citri Reticulatae, the Radix Angelicae Dahuricae, the Rhizoma Atractylodis Macrocephalae totally ten two flavor medicines, select L9 (3 for use
4) orthogonal scheme, investigate decocting number of times, amount of water, decocting time, extractum density, centrifugation rate, each factor of centrifugation time is actual in conjunction with producing, each factor designs three levels, and decocting number of times, amount of water and decocting time are merged into a factor, and testing program sees Table 7.
Table 7 experimental factor water-glass
Test and data: the Herba Pogostemonis after taking by weighing the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Fructus Jujubae, the Rhizoma Zingiberis Recens in the prescription ratio and extract volatile oil by the experimental program requirement, Folium Perillae, Pericarpium Citri Reticulatae, the Radix Angelicae Dahuricae, the Rhizoma Atractylodis Macrocephalae 12 flavor medicines 890g altogether decoct, content and the dried cream rate of choosing enoxolone are to investigate index, carry out comprehensive grading.The content tlc scanning determination of enoxolone.See Table 8.The content of testing enoxolone in the used Radix Glycyrrhizae is 3.1%, and regulation enoxolone Y full marks are 70 minutes, and because of the total 890g of the medical material that decocts, wherein Radix Glycyrrhizae has 100g, so wherein contained enoxolone should be 100 * 3.1%/890=0.35%.So the yield 0.35% with enoxolone is full marks 70 minutes, per 1% is 200 minutes, score Y * 200, dried cream rate full marks are 30 minutes, it is predicted the mobility scale of testing out dried cream rate, stipulate that dried cream rate 20% is 0,10% is 30 minutes, every increase by 1% deducts 30/ (20-10)=3 minute, and overall score is counted Y * 200+[30-3 (X-10)].
Table 8 orthogonal experiment design table
By the R value as can be known, the R value of factor D is minimum, shows its very little or not influence to experimental result influence, thus with the D example as test error, carry out significance test, see Table 9.
Table 9 analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean s | Free | Mean square z | The F value | p | Significance |
| A B C error e | 64·41 36·54 111·06 0·49 | 2 2 2 2 | 32·20 18·27 55·53 0·24 | 134·17 76·12 231·38 | ＜0·01 ＜0·05 ＜0·01 | Extremely significantly extremely remarkable |
Conclusion: as shown in Table 9, the principal element that influences paste-forming rate and enoxolone yield is A, C, secondly be B, according to table 8, optimised process is A2B1C1, it is the decocting secondary, 8 times of water gagings were fried in shallow oil 2 hours for the first time, added 6 times of water gagings for the second time and fried in shallow oil 1 hour, and it is 1.12 (80 ℃) that decocting liquid is concentrated into clear paste density, carry out centrifugally, centrifugation rate is 7000 rev/mins.
Experimental example 4 concentrates, the research of drying process
Get Cortex Magnoliae Officinalis 536g, press optimised process and extract, collect extracting solution, therefrom get 3000ml, be divided into two parts, behind the recovery ethanol, under condition of different temperatures, be condensed into clear paste, measure the content of magnolol and honokiol again.We by the visible temperature of table 15 content of magnolol and honokiol are had certain influence, so when pilot scale, can be evaporated to extract relative density 1.15 (80 ℃ of surveys).
See Table 10;
Table 10 concentrates condition and investigates
| Method | Extracting solution | Concentrated solution | The content of magnolol and honokiol |
| Normal pressure reclaims (95～90 ℃) reclaim under reduced pressure (75～80 ℃) | 1500ml 1500ml | 85ml 85ml | 3.07mg/ml 4.19mg/ml |
The method of extract dry and temperature: owing to contain volatile material in this product, so we adopt the drying means of drying under reduced pressure, and drying under reduced pressure can shorten drying time, therefore consider produce actual, our drying under reduced pressure in technology.
Experimental example 5 stability tests
Method: " provisions for new drugs approval " of issuing execution according to Ministry of Public Health on May 1st, 1999 is about adnexa " specification requirement of new Chinese medicine steady quality Journal of Sex Research " in the revision of Chinese medicine part and the supplementary provisions, by the prepared JIAWEI HUOXIANG ZHENGQI RUANJIAONANG, the aluminium-plastic panel packing is observed (seeing the following form) by declaring clinical trial with drug quality draft standard (data numbering 11) requirement under the 10/plate room temperature.
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990227
Date of manufacture: on February 27th, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.2) | March (99.6.2) | June (99.9.2) | December (00.3.2) | 18 months (00.9.2) | |
| Character | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspension consubstantiality powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspension consubstantiality powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of Pericarpium Citri Reticulatae of Herba Pogostemonis | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration (minute) | 12 | 15 | 17 | 17 | 19 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.30 | 1.30 | 1.30 | 1.29 | 1.33 |
| Microbial limit | Antibacterial (individual/g) mycete is (individual/g) the escherichia coli demodicid mite that lives | ＜10＜10 do not detect | 10 20 do not detect | ＜10＜10 do not detect | ＜10＜10 do not detect | 10 20 do not detect |
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990306
Date of manufacture: on March 6th, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.8) | March (99.6.8) | June (99.9.8) | December (00.3.8) | 18 months (00.9.8) | |
| Character | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of Pericarpium Citri Reticulatae of Herba Pogostemonis | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration (minute) | 13 | 15 | 18 | 18 | 20 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.27 | 1.27 | 1.27 | 1.20 | 1.24 |
| Microbial limit | Antibacterial (individual/g) mycete is (individual/g) the escherichia coli demodicid mite that lives | 20＜10 do not detect | ＜10 10 do not detect | 10＜10 do not detect | 20 20 do not detect | 20 20 do not detect |
Sample title: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG (0.6 gram/grain) lot number: 990313
Date of manufacture: on March 13rd, 1999
| Standing time (experiment date) is project as a result | 0 month (99.3.15) | March (99.6.15) | June (99.9.15) | December (00.3.15) | 18 months (00.9.15) | |
| Character | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | This product is brown soft capsule, and content is the sepia grease that contains a small amount of suspended solid powder; Gas fragrance, bitter in the mouth. | |
| Differentiate | 1. 2. 3. Radix Glycyrrhizae of Pericarpium Citri Reticulatae of Herba Pogostemonis | Positive positive | Positive positive | Positive positive | Positive positive | Positive positive |
| Check | Disintegration (minute) | 15 | 18 | 19 | 18 | 22 |
| Assay | Magnolol, honokiol (mg/ grain) | 1.38 | 1.38 | 1.38 | 1.38 | 1.40 |
| Microbial limit | Antibacterial (individual/g) mycete is (individual/g) the escherichia coli demodicid mite that lives | 20＜10 do not detect | 20 10 do not detect | 10＜10 do not detect | 20 20 do not detect | 20 20 do not detect |
The result: observed through 18 months, every index (character, discriminating, inspection, assay) all meets the quality standard requirement, and health examination meets the health examination standard.
Conclusion: JIAWEI HUOXIANG ZHENGQI RUANJIAONANG was placed 18 months with the aluminium-plastic panel room temperature respectively, steady quality.
Embodiment 1:Preparation of soft capsule method one of the present invention
Herba Pogostemonis 326.8g Folium Perillae 108.9g Radix Angelicae Dahuricae 108.9g
Rhizoma Atractylodis macrocephalae's (stir-fry) 217.9g Pericarpium Citri Reticulatae 217.9g Rhizoma Pinelliae (processed) 217.9g
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 217.9g Poria 108.9g Radix Platycodonis 217.9g
Radix Glycyrrhizae 217.9g Pericarpium Arecae 108.9g
More than ten simply, Cortex Magnoliae Officinalis is with 60% ethanol extraction three times, each 1 hour, filter, merging filtrate reclaims ethanol, is concentrated into relative density and is 1.15 clear paste A; Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Dahuricae vapor distillation extract volatile oil, and the aqueous solution after the distillation filters other device and collects; The medicinal residues and the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Rhizoma Zingiberis Recens 32.7g and Fructus Jujubae 54.5g decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate and the merging of above-mentioned aqueous solution are concentrated into relative density and are 1.12 clear paste, centrifugal, supernatant concentration to relative density is 1.15 clear paste B; Merge clear paste A and B, be concentrated into relative density and be 1.30 thick paste, drying under reduced pressure is ground into fine powder, sieves.Other gets edible vegetable oil 360g, and it is an amount of to add Cera Flava etc., and temperature is treated in fusing, adds above-mentioned powder and volatile oil, and is even through the colloid mill mill, is pressed into 1000 of soft capsules, promptly.
Embodiment 2:Preparation of soft capsule method two of the present invention
Herba Pogostemonis 326.8g Folium Perillae 108.9g Radix Angelicae Dahuricae 108.9g
The Rhizoma Atractylodis Macrocephalae (stir-fry) 217.9g Pericarpium Citri Reticulatae 217.9g Rhizoma Pinelliae (processed) 217.9g
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 217.9g Poria 108.9g Radix Platycodonis 217.9g
Radix Glycyrrhizae 217.9g Pericarpium Arecae 108.9g
More than ten simply, Cortex Magnoliae Officinalis is with 60% ethanol extraction three times, each 1 hour, filter, merging filtrate reclaims ethanol, being concentrated into relative density is the clear paste A of 1.15 (80 ℃); Herba Pogostemonis, Folium Perillae, Pericarpium Citri Reticulatae, the Rhizoma Atractylodis Macrocephalae, Radix Angelicae Dahuricae vapor distillation extract volatile oil, and the aqueous solution after the distillation filters, and device is collected in addition; The medicinal residues and the Rhizoma Pinelliae, Poria, Radix Platycodonis, Radix Glycyrrhizae, Pericarpium Arecae, Rhizoma Zingiberis Recens 32.7g and Fructus Jujubae 54.5g decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, merge with above-mentioned aqueous solution, filter, filtrate is concentrated into the clear paste that relative density is 1.12 (80 ℃), centrifugal, supernatant concentration to relative density is the clear paste B of 1.15 (80 ℃); With clear paste A drying under reduced pressure, be ground into fine powder, sieve.With clear paste B, being concentrated into relative density is the thick paste of 1.30-1.35 (80 ℃), and drying under reduced pressure is ground into fine powder, sieves.The above-mentioned extract powder of mixing adds volatile oil and refined plant oil, Cera Flava is an amount of, and is even through the colloid mill mill, is pressed into 1000 of soft capsules, promptly.
Embodiment 3:The preparation of soft capsule rubber solution of the present invention
Get 1.5: 0.03: 1.5 glycerol, Brown Ferric Oxide and water, be heated to 75 ℃, mix homogeneously adds and adds the bloated 1.5 parts of gelatin stirring of water logging in advance, fusion, and insulation was left standstill 1.5 hours, made the foam come-up, scraped off the foam of come-up, filtered heat preservation for standby use with clean calico;
Start encapsulating machine, the rubber of arranging exhibits carries out the heavy debugging of ball with paraffin as content, debug qualified after, drain paraffin oil, medicinal liquid is added in the liquid reservoir of machine top, start the medicine inlet valve, the soft capsule that contains medicine is compression moulding; The soft capsule micelle of compression moulding sent in the hothouse that dehydrating unit is housed carried out drying 4 hours under 27 ℃ of temperature, use the washing with alcohol soft capsule, the soft capsule after the washing is sent into hothouse once more, under 35 ℃ of temperature dry 15 hours, promptly gets the soft capsule finished product.
Embodiment 4:The method of quality control of soft capsule of the present invention
Differentiate: get soft capsule content 2g of the present invention, put in the 500ml round-bottomed flask, add water 250ml, mixing, connect volatile oil determination apparatus, add water to scale from the determinator upper end, and till overflow goes in the flask, add petroleum ether (60-90 ℃) 1.5ml again, connect reflux condensing tube, be heated to and boil, and keep little and boiled 2 hours, put coldly, divide and to get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds petroleum ether and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with 0.5% sodium carboxymethyl cellulose, with 10: 1 petroleum ether (60-90 ℃)-ethyl acetates was developing solvent, launch, take out, dry, spray is with 2% vanillin sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Get soft capsule content 2g of the present invention, secondary is extracted in the jolting that adds diethyl ether, and each 20ml discards ether solution, residue is waved most ether factory and is added water 40ml and make dissolving, add water saturated n-butanol extraction secondary, each 30ml merges n-butyl alcohol liquid, filter, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the hesperidin reference substance, adds methanol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, be developing solvent with 1: 1 acetone-water, launch, take out, to dry, spray is put under the 365nm ultra-violet lamp and is inspected with 1% aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show same color fluorescence speckle;
Get soft capsule content 2g of the present invention, add petroleum ether (60 ℃-90 ℃) 30ml, supersound process 30 minutes discards petroleum ether, volatilize, residue adds chloroform 25ml and hydrochloric acid 2ml, puts in the water-bath reflux 1 hour, filters, filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add methanol and make the solution that every 1ml contains 0.5mg, product solution according to the thin layer chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively in same be on the silica GF254 lamellae of binding agent with 0.5% sodium carboxymethyl cellulose, with 30: 15: 1 toluene-ethyl acetate-formic acid was developing solvent, launched, and took out, dry, put under the 254nm uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; 75: 25 methanol-water is mobile phase; Flow velocity 1ml/min; Detect wavelength 294nm; Column temperature is a room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800;
The preparation of reference substance solution, precision take by weighing magnolol and the honokiol reference substance is an amount of, and add methanol and make into the mixed solution that every 1ml contains magnolol 30ug, honokiol 25ug, mixing, promptly;
The system of need testing solution each, precision takes by weighing the about 2g of soft capsule of the present invention, precision adds 60% ethanol 20ml, weigh, supersound process 45 minutes is weighed again, supply solvent and subtract the weight of mistake, shake well filters, discard filtrate just, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, with 60% ethanol dilution to scale, shake up, promptly;
Algoscopy, accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures, promptly.
Claims (3)
1, a kind of method of quality control of JIAWEI HUOXIANG ZHENGQI RUANJIAONANG, this soft capsule is that raw material is made with Herba Pogostemonis 300-350 weight portion, Folium Perillae 90-110 weight portion, Radix Angelicae Dahuricae 90-110 weight portion, Rhizoma Atractylodis Macrocephalae (parched) 180-220 weight portion, Pericarpium Citri Reticulatae 180-220 weight portion, Rhizoma Pinelliae Preparata 180-220 weight portion, Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 180-220 weight portion, Poria 90-110 weight portion, Radix Platycodonis 180-220 weight portion, Radix Glycyrrhizae 180-220 weight portion, Pericarpium Arecae 90-110 weight portion, it is characterized in that this method is:
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, put in the 500ml round-bottomed flask, add water 200-300ml, mixing, connect volatile oil determination apparatus, add water to scale from the determinator upper end, and till overflow goes in the flask, add petroleum ether 1-3ml again, connect reflux condensing tube, be heated to and boil, and kept little 1-3 of boiling hour, put coldly, divide and to get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds petroleum ether and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with 0.5% sodium carboxymethyl cellulose, with 8-12: 0.8-1.2 petroleum ether-ethyl acetate is developing solvent, launch, take out, dry, spray is with 2% vanillin sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, the jolting that adds diethyl ether is extracted 2-3 time, each 20ml, discard ether solution, residue is waved most ether, adds water 40ml and makes dissolving, adds water saturated n-butanol extraction 2-3 time, each 30ml, merge n-butyl alcohol liquid, filter evaporate to dryness, residue adds methanol 5ml makes dissolving, as need testing solution; Other gets the hesperidin reference substance, adds methanol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to thin layer chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, with 0.8-1.2: the 0.8-1.2 acetone-water is developing solvent, launches, and takes out, and dries, and spray is put under the ultra-violet lamp and inspected with 1% aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show same color fluorescence speckle;
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, add petroleum ether 20-40ml, supersound process 20-40 minute, discard petroleum ether, volatilize, residue adds chloroform 20-30ml and hydrochloric acid 1-3ml, put in the water-bath reflux 1-1.5 hour, and filtered the filtrate evaporate to dryness, residue adds methanol 1-3ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add methanol and make the solution that every 1ml contains 0.5mg, product solution according to the thin layer chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively in same be on the silica GF254 lamellae of binding agent with 0.5% sodium carboxymethyl cellulose, with 28-32: 12-16: 0.8-1.2 toluene-ethyl acetate-formic acid is developing solvent, launches, and takes out, dry, put under the uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay, according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; 72-76: the 23-26 methanol-water is a mobile phase; Flow velocity 1ml/min; Detect wavelength 294nm; Column temperature is a room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800; The preparation of reference substance solution, precision take by weighing magnolol and the honokiol reference substance is an amount of, and add methanol and make into the mixed solution that every 1ml contains magnolol 25-35ug, honokiol 20-30ug, mixing, promptly; The preparation of need testing solution, precision take by weighing JIAWEI HUOXIANG ZHENGQI RUANJIAONANG 2g, and precision adds 50-70% ethanol 15-25ml, weigh, supersound process 30-50 minute, weigh again, supply solvent and subtract the weight of mistake, shake well filters, discard filtrate just, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, uses the 50-60% ethanol dilution to scale, shake up, promptly;
Algoscopy, accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures, promptly.
2, the method for quality control of JIAWEI HUOXIANG ZHENGQI RUANJIAONANG as claimed in claim 1 is characterized in that this method is:
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, put in the 500ml round-bottomed flask, add water 250ml, mixing, connect volatile oil determination apparatus, add water to scale from the determinator upper end, and till overflow goes in the flask, add petroleum ether 1.5ml again, connect reflux condensing tube, be heated to and boil, and keep little and boiled 2 hours, put coldly, divide and to get petroleum ether layer as need testing solution; Other gets the patchouli oil reference substance and adds petroleum ether and make the solution that every 1ml contains 0.1ml, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 5ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with 0.5% sodium carboxymethyl cellulose, with 10: 1 petroleum ether-ethyl acetates was developing solvent, launch, take out, dry, spray is with 2% vanillin sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, secondary is extracted in the jolting that adds diethyl ether, and each 20ml discards ether solution, residue is waved most ether factory and is added water 40ml and make dissolving, add water saturated n-butanol extraction secondary, each 30ml merges n-butyl alcohol liquid, filter, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the hesperidin reference substance, adds methanol and makes every 1ml and contain 0.5mg solution, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned two kinds of each 2ul of solution, put respectively on same polyamide film, be developing solvent with 1: 1 acetone-water, launch, take out, to dry, spray is put under the 365nm ultra-violet lamp and is inspected with 1% aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show same color fluorescence speckle;
Get JIAWEI HUOXIANG ZHENGQI RUANJIAONANG content 2g, add petroleum ether 30ml, supersound process 30 minutes discards petroleum ether, volatilize, residue adds chloroform 25ml and hydrochloric acid 2ml, puts in the water-bath reflux 1 hour, filters, filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add methanol and make the solution that every 1ml contains 0.5mg, product solution according to the thin layer chromatography test, is drawn above-mentioned two kinds of each 5ul of solution in contrast, put respectively in same be on the silica GF254 lamellae of binding agent with 0.5% sodium carboxymethyl cellulose, with 30: 15: 1 toluene-ethyl acetate-formic acid was developing solvent, launched, and took out, dry, put under the 254nm uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:, be filler with the octadecylsilane chemically bonded silica according to high effective liquid chromatography for measuring chromatographic condition and system suitability test; 75: 25 methanol-waters are mobile phase; Flow velocity 1ml/min; Detect wavelength 294nm; Column temperature is a room temperature; Theoretical cam curve is calculated by the magnolol peak should be not less than 3800; The preparation of reference substance solution, precision take by weighing magnolol and the honokiol reference substance is an amount of, and add methanol and make into the mixed solution that every 1ml contains magnolol 30ug, honokiol 25ug, mixing, promptly; The system of need testing solution each, precision takes by weighing JIAWEI HUOXIANG ZHENGQI RUANJIAONANG 2g, precision adds 60% ethanol 20ml, weigh, supersound process 45 minutes is weighed again, supply solvent and subtract the weight of mistake, shake well filters, discard filtrate just, precision is measured subsequent filtrate 5ml, to the 50ml measuring bottle, with 60% ethanol dilution to scale, shake up, promptly;
Algoscopy, accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures, promptly.
3, the method for quality control of JIAWEI HUOXIANG ZHENGQI RUANJIAONANG as claimed in claim 1 or 2 is characterized in that described JIAWEI HUOXIANG ZHENGQI RUANJIAONANG is to be made by following bulk drugs:
Herba Pogostemonis 326.8 weight portion Folium Perillaes 108.9 weight portions
The Radix Angelicae Dahuricae 108.9 weight portion Rhizoma Atractylodis Macrocephalae (parched)s 217.9 weight portions
Pericarpium Citri Reticulatae 217.9 weight portion Rhizoma Pinelliae Preparata 217.9 weight portions
Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 217.9 weight portion Poria 108.9 weight portions
Radix Platycodonis 217.9 weight portion Radix Glycyrrhizaes 217.9 weight portions
Pericarpium Arecae 108.9 weight portions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100010437A CN100367996C (en) | 2003-12-23 | 2003-12-23 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100010437A CN100367996C (en) | 2003-12-23 | 2003-12-23 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310122427 Division CN1251733C (en) | 2002-12-23 | 2003-12-23 | Preparation of enhanced agastache capsules and quality control thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1840050A true CN1840050A (en) | 2006-10-04 |
| CN100367996C CN100367996C (en) | 2008-02-13 |
Family
ID=37029353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100010437A Expired - Lifetime CN100367996C (en) | 2003-12-23 | 2003-12-23 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100367996C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102178829A (en) * | 2011-05-06 | 2011-09-14 | 江西九华药业有限公司 | Method for detecting ingredients of Chinese medicinal compound suppository for haemorrhoids |
| CN101334385B (en) * | 2008-07-21 | 2011-11-30 | 深圳职业技术学院 | Aromatic plant volatility organic matter analytical method |
| CN101732608B (en) * | 2010-01-27 | 2012-05-23 | 昆明中药厂有限公司 | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder |
| CN102100818B (en) * | 2009-12-16 | 2012-12-12 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for lophanthus antifebrile tablets |
| CN103330861A (en) * | 2013-07-24 | 2013-10-02 | 肖振锋 | Medicine for curing cholera and preparation method thereof |
| CN104363773A (en) * | 2012-05-19 | 2015-02-18 | 江苏康缘药业股份有限公司 | Herbal composition for treatment of gastrointestinal inflammatory diseases and method to prepare and use thereof |
| CN104606611A (en) * | 2014-12-29 | 2015-05-13 | 王琪 | Traditional Chinese medicine mixture for treating summer heat and damp disease |
| WO2015149389A1 (en) * | 2014-03-31 | 2015-10-08 | 袁志贤 | Traditional chinese medicine for treating chronic enteritis and preparation method therefor |
-
2003
- 2003-12-23 CN CNB2006100010437A patent/CN100367996C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334385B (en) * | 2008-07-21 | 2011-11-30 | 深圳职业技术学院 | Aromatic plant volatility organic matter analytical method |
| CN102100818B (en) * | 2009-12-16 | 2012-12-12 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for lophanthus antifebrile tablets |
| CN101732608B (en) * | 2010-01-27 | 2012-05-23 | 昆明中药厂有限公司 | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder |
| CN102178829A (en) * | 2011-05-06 | 2011-09-14 | 江西九华药业有限公司 | Method for detecting ingredients of Chinese medicinal compound suppository for haemorrhoids |
| CN102178829B (en) * | 2011-05-06 | 2013-01-30 | 江西九华药业有限公司 | Method for detecting ingredients of Chinese medicinal compound suppository for haemorrhoids |
| CN104363773A (en) * | 2012-05-19 | 2015-02-18 | 江苏康缘药业股份有限公司 | Herbal composition for treatment of gastrointestinal inflammatory diseases and method to prepare and use thereof |
| CN104363773B (en) * | 2012-05-19 | 2017-03-01 | 江苏康缘药业股份有限公司 | For treating herbal-composition of gastroenteritis disease and its production and use |
| CN103330861A (en) * | 2013-07-24 | 2013-10-02 | 肖振锋 | Medicine for curing cholera and preparation method thereof |
| WO2015149389A1 (en) * | 2014-03-31 | 2015-10-08 | 袁志贤 | Traditional chinese medicine for treating chronic enteritis and preparation method therefor |
| CN104606611A (en) * | 2014-12-29 | 2015-05-13 | 王琪 | Traditional Chinese medicine mixture for treating summer heat and damp disease |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100367996C (en) | 2008-02-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110455965B (en) | Preparation method of pharmaceutical composition and HPLC fingerprint spectrum establishment method thereof | |
| CN101708223B (en) | Preparation method, quality control method and application for Chinese medicinal compound indigowoad leaf preparation | |
| CN102269751B (en) | Detection method of Liuweinengxiao preparation | |
| CN102091168B (en) | Detection method for Chinese medicine preparation Xuefuzhuyu capsule | |
| CN1251733C (en) | Preparation of enhanced agastache capsules and quality control thereof | |
| CN102114155B (en) | Serial Chinese medicinal preparation for treating phaseolus cold and preparation process and quality control method thereof | |
| CN102028859A (en) | Quality control method for Chinese medicinal preparation for treating asthma | |
| CN1840050A (en) | Quality control method of 'Jia Wei Huo Xiang' soft capsule | |
| CN101987121A (en) | Detection method of medicine composition for treating hepatitis | |
| CN102114060B (en) | Amur valeriana extract and preparation method and applications thereof | |
| CN106370756B (en) | A kind of detection method of Chinese materia medica preparation that preventing and treating infectious bronchitis of chicken | |
| CN1895438B (en) | Chinese-medicinal composition for treating cephalagia and its preparation | |
| CN1907481B (en) | Medicinal composition for treating summer heat-dampness rheum and preparation method thereof | |
| CN100342847C (en) | Stomach nourishing dispersible tablet with aucklandia root and amomum fruit and its preparation method | |
| CN102419357B (en) | Method for detecting eighteen-component codonopsis pilosula preparation | |
| CN102068649B (en) | Quality control method for gastric condition-regulating pill as traditional Chinese preparation | |
| CN1226033C (en) | Method for preparing traditional Chinese medicine concentrated pill | |
| CN102068656A (en) | Quality control method for traditional Chinese medicinal preparation epilepsy pills | |
| CN1879850A (en) | Capsule with hairy vein agrimony and arenobufagin, its preparation process and quality control method | |
| CN101647997B (en) | Influenza wind-dispelling capsule and preparation method and quality control method thereof | |
| CN106728651B (en) | Preparation method and quality detection method of rhizoma cyperi four-ingredient granules | |
| CN103655821B (en) | Chinese medicine preparation of a kind of beneficial gas establishing-Yang and Tianjing Busuiye medicinal and preparation method thereof | |
| CN102608249A (en) | Detection method of Tenghuang Jiangu pill | |
| CN101336967A (en) | Tongbianling preparation and quality control method | |
| CN1840032A (en) | Granule for treating infant's rhinitis, its preparation method and quality control 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 | ||
| CX01 | Expiry of patent term |
Granted publication date: 20080213 |
|
| CX01 | Expiry of patent term |