CN101732608B - Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder - Google Patents
Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder Download PDFInfo
- Publication number
- CN101732608B CN101732608B CN2010101017942A CN201010101794A CN101732608B CN 101732608 B CN101732608 B CN 101732608B CN 2010101017942 A CN2010101017942 A CN 2010101017942A CN 201010101794 A CN201010101794 A CN 201010101794A CN 101732608 B CN101732608 B CN 101732608B
- Authority
- CN
- China
- Prior art keywords
- chrysanthemum
- lonicera
- forsythia
- mulberry
- thin
- 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.)
- Active
Links
- 235000007516 Chrysanthemum Nutrition 0.000 title claims abstract description 45
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 240000000249 Morus alba Species 0.000 title claims abstract description 36
- 235000008708 Morus alba Nutrition 0.000 title claims abstract description 35
- 241000245240 Lonicera Species 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 32
- 244000189548 Chrysanthemum x morifolium Species 0.000 title description 33
- 241000555682 Forsythia x intermedia Species 0.000 title 1
- 240000005528 Arctium lappa Species 0.000 claims abstract description 35
- 235000003130 Arctium lappa Nutrition 0.000 claims abstract description 34
- 241000555712 Forsythia Species 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000003814 drug Substances 0.000 claims abstract description 12
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 241000723353 Chrysanthemum Species 0.000 claims abstract 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 238000012360 testing method Methods 0.000 claims description 44
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 241000576429 Forsythia suspensa Species 0.000 claims description 15
- 239000002775 capsule Substances 0.000 claims description 15
- 235000008078 Arctium minus Nutrition 0.000 claims description 14
- 241000628997 Flos Species 0.000 claims description 14
- 229930182470 glycoside Natural products 0.000 claims description 14
- 150000002338 glycosides Chemical class 0.000 claims description 14
- 239000013558 reference substance Substances 0.000 claims description 12
- 235000014676 Phragmites communis Nutrition 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000004587 chromatography analysis Methods 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000741 silica gel Substances 0.000 claims description 8
- 229910002027 silica gel Inorganic materials 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 239000000454 talc Substances 0.000 claims description 8
- 229910052623 talc Inorganic materials 0.000 claims description 8
- 235000012222 talc Nutrition 0.000 claims description 8
- 241000255789 Bombyx mori Species 0.000 claims description 7
- 241000931705 Cicada Species 0.000 claims description 7
- 244000068988 Glycine max Species 0.000 claims description 7
- 240000003915 Lophatherum gracile Species 0.000 claims description 7
- 235000006753 Platycodon grandiflorum Nutrition 0.000 claims description 7
- 240000004922 Vigna radiata Species 0.000 claims description 7
- 238000012850 discrimination method Methods 0.000 claims description 7
- 235000010469 Glycine max Nutrition 0.000 claims description 6
- 244000246386 Mentha pulegium Species 0.000 claims description 6
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 6
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 6
- 240000003582 Platycodon grandiflorus Species 0.000 claims description 6
- 241000951473 Schizonepeta Species 0.000 claims description 6
- 235000010721 Vigna radiata var radiata Nutrition 0.000 claims description 6
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 claims description 6
- 235000001050 hortel pimenta Nutrition 0.000 claims description 6
- 210000000582 semen Anatomy 0.000 claims description 6
- 244000303040 Glycyrrhiza glabra Species 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 4
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims description 4
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000000796 flavoring agent Substances 0.000 claims description 4
- 235000019634 flavors Nutrition 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
- 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
- 238000002156 mixing Methods 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000011003 system suitability test Methods 0.000 claims description 4
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 238000003908 quality control method Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- NQWVSMVXKMHKTF-JKSUJKDBSA-N (-)-Arctigenin Chemical compound C1=C(OC)C(OC)=CC=C1C[C@@H]1[C@@H](CC=2C=C(OC)C(O)=CC=2)C(=O)OC1 NQWVSMVXKMHKTF-JKSUJKDBSA-N 0.000 abstract 1
- YYGRXNOXOVZIKE-UHFFFAOYSA-N Arctigenin Natural products COC1CCC(CC2COC(=O)C2CC3CCC(O)C(C3)OC)CC1OC YYGRXNOXOVZIKE-UHFFFAOYSA-N 0.000 abstract 1
- OIFFJDGSLVHPCW-UHFFFAOYSA-N Guayarol Natural products COc1ccc(CC2C(Cc3ccc(O)c(O)c3)COC2=O)cc1OC OIFFJDGSLVHPCW-UHFFFAOYSA-N 0.000 abstract 1
- NQWVSMVXKMHKTF-UHFFFAOYSA-N L-Arctigenin Natural products C1=C(OC)C(OC)=CC=C1CC1C(CC=2C=C(OC)C(O)=CC=2)C(=O)OC1 NQWVSMVXKMHKTF-UHFFFAOYSA-N 0.000 abstract 1
- NWFYESYCEQICQP-UHFFFAOYSA-N methylmatairesinol Natural products C1=C(OC)C(OC)=CC=C1CC1C(=O)OCC1CC1=CC=C(O)C(OC)=C1 NWFYESYCEQICQP-UHFFFAOYSA-N 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 19
- 206010011224 Cough Diseases 0.000 description 7
- 229940079593 drug Drugs 0.000 description 7
- 210000004072 lung Anatomy 0.000 description 5
- 230000001737 promoting effect Effects 0.000 description 5
- 230000005180 public health Effects 0.000 description 4
- 206010062717 Increased upper airway secretion Diseases 0.000 description 3
- 206010068319 Oropharyngeal pain Diseases 0.000 description 3
- 201000007100 Pharyngitis Diseases 0.000 description 3
- 244000018633 Prunus armeniaca Species 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 235000021374 legumes Nutrition 0.000 description 3
- 208000026435 phlegm Diseases 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 2
- 244000192528 Chrysanthemum parthenium Species 0.000 description 2
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 241000935235 Fritillaria meleagris Species 0.000 description 2
- 241000202807 Glycyrrhiza Species 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 2
- 241001170080 Lonicera hypoglauca Species 0.000 description 2
- 208000004880 Polyuria Diseases 0.000 description 2
- 235000009827 Prunus armeniaca Nutrition 0.000 description 2
- 208000001431 Psychomotor Agitation Diseases 0.000 description 2
- 206010038743 Restlessness Diseases 0.000 description 2
- 206010000269 abscess Diseases 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000035619 diuresis Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 235000008384 feverfew Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 231100000869 headache Toxicity 0.000 description 2
- 208000021760 high fever Diseases 0.000 description 2
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 210000004243 sweat Anatomy 0.000 description 2
- 241000254032 Acrididae Species 0.000 description 1
- 235000003840 Amygdalus nana Nutrition 0.000 description 1
- 235000010864 Armeniaca mandshurica Nutrition 0.000 description 1
- 244000147617 Armeniaca mandshurica Species 0.000 description 1
- 235000015577 Armeniaca sibirica Nutrition 0.000 description 1
- 244000141006 Armeniaca sibirica Species 0.000 description 1
- 241000751139 Beauveria bassiana Species 0.000 description 1
- 241000208671 Campanulaceae Species 0.000 description 1
- 241000131317 Capitulum Species 0.000 description 1
- 241000208828 Caprifoliaceae Species 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- 241001000583 Cryptotympana atrata Species 0.000 description 1
- 241000201295 Euphrasia Species 0.000 description 1
- 241001547127 Fritillaria cirrhosa Species 0.000 description 1
- 241001644297 Fritillaria delavayi Species 0.000 description 1
- 241001644295 Fritillaria przewalskii Species 0.000 description 1
- 241001644290 Fritillaria unibracteata Species 0.000 description 1
- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
- 241000100289 Lonicera confusa Species 0.000 description 1
- 241001170076 Lonicera macranthoides Species 0.000 description 1
- 241001570521 Lonicera periclymenum Species 0.000 description 1
- 244000280293 Mentha haplocalyx Species 0.000 description 1
- 235000001878 Mentha haplocalyx Nutrition 0.000 description 1
- 241000819999 Nymphes Species 0.000 description 1
- 241000207834 Oleaceae Species 0.000 description 1
- 244000273256 Phragmites communis Species 0.000 description 1
- 244000274050 Platycodon grandiflorum Species 0.000 description 1
- 235000011432 Prunus Nutrition 0.000 description 1
- 241000220299 Prunus Species 0.000 description 1
- 235000002413 Prunus ansu Nutrition 0.000 description 1
- 241000951376 Schizonepeta tenuifolia Species 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 230000002498 deadly effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004377 improving vision Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 235000014774 prunus Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000009792 yinqiao Substances 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to a method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder according to standards described in volume XI of Medicament Standard of Ministry of Health of the People's Republic of China (Chinese medicinal set prescription preparation), which comprises a microscopic identification method of chrysanthemum, lonicera confuse and great burdock achene, a thin-layer chromatography identification method of forsythia, a thin-layer chromatography identification method of liquoric root and a content measuring method of arctigenin in medicaments. The quality detection method of the mulberry and chrysanthemum lonicera and forsythia powder improves the quality control standard of the mulberry and chrysanthemum lonicera and forsythia powder, establishes content measuring indexes in the preparation and a detection method thereof, improves the thin-layer chromatography identification method of the forsythia and the liquoric root by making the thin-layer chromatography identification method of the forsythia and the liquoric root more specific and accurate, increases microscopic characteristics of the chrysanthemum and the great burdock achene, revises the microscopic characteristic of the lonicera confuse to make the description of the lonicera confuse more standard and accurate, and ensures the high quality standard level of the compound preparation.
Description
Technical field
The present invention relates to the quality determining method of the ten mulberry and chrysanthemum lonicera and forsythia powder of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Technical background
Medicine mulberry and chrysanthemum lonicera and forsythia powder in the 11 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation) has suffering cool completely table, the cough-relieving of a surname's lung, clearing heat and detoxicating effect, is used for affection of exogenous wind-heat, loathing of cold high fever, headache cough, abscess of throat.This compound preparation is made up of Chinese crude drug mulberry leaf 60g, chrysanthemum 60g, Flos Lonicerae 60g, capsule of weeping forsythia 60g, Bulbus Fritillariae Cirrhosae 60g, balloonflower root 30g, peppermint 40g, lophatherum gracile 40g, schizonepeta 40g, great burdock achene 40g, semen armeniacae amarae 40g, reed rhizome 60g, cicada slough 60g, stiff silkworm 30g, talcum 60g, mung bean 60g, Fermented Soybean 20g, Radix Glycyrrhizae 40g, and above-mentioned raw materials is processed 860g altogether.Mulberry leaf are the dried leaves of moraceae plants mulberry Morus alba L., have dispelling wind and heat from the body, clearing away the lungheat and moisturizing, the effect of clearing liver and improving vision; Chrysanthemum is the dry capitulum of feverfew chrysanthemum Chrysanthemum morifolium Ramat., has diffusing wind heat-clearing, the effect that flat liver makes eye bright; Flos Lonicerae is the dry flower of caprifoliaceae plant largeflower-like honeysuckle flower Lonicera macranthoides Hand.-Mazz., lonicera hypoglauca miq Lonicera hypoglauca Miq. or Lonicera confusa Lonicera confusa DC. or the flower that band is just opened; Tool is clearing heat and detoxicating, the effect of wind-heat dissipating; The capsule of weeping forsythia is the dry fruit of Oleaceae plant capsule of weeping forsythia Forsythia suspensa (Thunb.) Vahl, have clearing heat and detoxicating, the effect of dispersing swelling and dissipating binds; Bulbus Fritillariae Cirrhosae is the dry bulb of liliaceous plant Bulbus Fritillariae Cirrhosae Fritillaria cirrhosa D.Don, dark violet bulb of fritillary Fritillaria unibracteata Hsiao et K.C.Hsia, Gansu bulb of fritillary Fritillaria przewalskii Maxim. or Bulbus Fritillariae cirrhosae Fritillaria delavayi Franch.; Have clearing heat and moistening lung, the effect of preventing phlegm from forming and stopping coughing; Balloonflower root is the dry root of Campanulaceae plant Platycodon grandiflorum (Jacq.) A.DC., has a surname's lung, relieve sore throat, the effect of apocenosis; Peppermint is the dry aerial parts of labiate Menthahaplocalyx Briq., has dispelling wind-heat, refresh oneself, the effect of promoting eruption; Lophatherum gracile is the dry cauline leaf of grass lophatherum gracile Lophatherum gracile Brongn., has clearing heat and relieving fidgetness, the effect of diuresis; Schizonepeta is the dry aerial parts of labiate schizonepeta Schizonepeta tenuifolia Briq., has the diffusing wind that induces sweat, the effect of promoting eruption; Great burdock achene is the dry mature fruit of feverfew burdock Arctium lappa L, has dispelling wind and heat from the body, a surname's lung promoting eruption, the effect of detoxifcation relieve sore throat; Semen armeniacae amarae is the dry mature seed of rosaceous plant ansu apricot Prunus armeniaca L.var.ansuMaxim., Siberia apricot Prunus sibirica L., prunus mandshuricaKoehne Prunus mandshurica (Maxim.) Koehne or apricot Prunus armeniaca L.; It is relieving cough and asthma to have sending down abnormally ascending, the effect that relaxes bowel; Reed rhizome is the fresh or dry rhizome of grass reed Phragmites communis Trin., has clearing heat and promoting fluid, the effect of relieving restlessness; Cicada slough is the nymph of the black grasshopper Cryptotympana pustulata Fabricius of cicada exuviae shell when sprouting wings, and has diffusing wind heat extraction, relieve sore throat, the effect of promoting eruption; Stiff silkworm is that the larva in Bombycidae insect silkworm Bombyx mori Linnaeus4～5 ages infects (or artificial infection) muscardine Beauveria bassiana (Bals) Vuillant and deadly dry body has dispelling wind and relieving convulsion, the effect of reducing phlegm and resolving masses; Talcum is a silicates mineral talc family talcum, the main hydrous magnesium silicate (Mg that contains
3(Si
4O
10) (OH)
2), have inducing diuresis for treating strangurtia, clearing away summerheat, the effect of sore is held back in clearing damp; Mung bean is the dry seed of legume mung bean Phaseolus radiatus L., has clearing heat and detoxicatingly, relieves summer heat the effect of sharp water; Tasteless preserved soybean is the fermentation processed goods of the mature seed of legume soybean Glycine max (L.) Merr., has and induces sweat, relieving restlessness, the effect that a surname sends out hot and suffocating; Radix Glycyrrhizae is the dry root and rhizome of glycyrrhizic legume Glycyrrhiza inflata Bat., glycyrrhiza inflate bat Glycyrrhiza in flataBat or glycyrrhiza glabra Glycyrrhiza glabra L.; Have invigorate the spleen and benefit qi, clearing heat and detoxicating, expelling phlegm and arresting coughing, the effect of coordinating the drug actions of a prescription." Drug Standard of Ministry of Public Health of the Peoples Republic of China " the 11 issued the quality control standard (WS3-B-2219-96) of mulberry and chrysanthemum lonicera and forsythia powder; But in the existing mulberry and chrysanthemum lonicera and forsythia powder method of quality control that the Ministry of Public Health issues; Have only microscopical identification and thin-layer chromatography to differentiate; Limitation is very big, is difficult to accurately control the quality of mulberry and chrysanthemum lonicera and forsythia powder;
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of quality determining method of mulberry and chrysanthemum lonicera and forsythia powder is provided, to improve the quality control standard of mulberry and chrysanthemum lonicera and forsythia powder.
The pharmaceutical formulation of mulberry and chrysanthemum lonicera and forsythia powder is: mulberry leaf 60g, chrysanthemum 60g, Flos Lonicerae 60g, capsule of weeping forsythia 60g, Bulbus Fritillariae Cirrhosae 60g; Balloonflower root 30g, peppermint 40g, lophatherum gracile 60g, schizonepeta 40g, great burdock achene 40g; Semen armeniacae amarae 40g, reed rhizome 60g, cicada slough 60g, stiff silkworm 30g; Talcum 60g, mung bean 60g, Fermented Soybean 20g, Radix Glycyrrhizae 40g.More than 18 the flavor, be ground into fine powder, sieve, mixing promptly gets.These article are lark to filemot powder; Bitter, sweet, little puckery.
The quality determining method of mulberry and chrysanthemum lonicera and forsythia powder of the present invention is:
1, the microscopical identification method of chrysanthemum, Flos Lonicerae and great burdock achene: get mulberry and chrysanthemum lonicera and forsythia powder and put the microscopically observation: pollen granule is yellow, type sphere, and outer wall is thicker, tool bastard, 3 germinal aperatures of tool (chrysanthemum); Pollen granule is yellow, sphere, and outer wall is thin, 3 germinal aperatures of tool (Flos Lonicerae); The endocarp lithocyte is slightly flat, and the surface is seen and is sharp fusiformis, oblong, and sharp oval is inlayed closely (great burdock achene);
2, the thin-layer chromatography discrimination method of the capsule of weeping forsythia: get mulberry and chrysanthemum lonicera and forsythia powder 10g, add ethanol 40-60ml, sonicated 20-40 minute, filter; The filtrating evaporate to dryness, residue adds water 15-25ml makes dissolving, and absorbent cotton filters; Filtrating is extracted 2-3 time with the ethyl acetate jolting, each 15-25ml, combined ethyl acetate liquid; Evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets capsule of weeping forsythia control medicinal material 0.5g, adds ethyl acetate 15-25ml, and sonicated 20-40 minute, filter, the filtrating evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate (volume proportion 17-23: 0.9-1.1) be developping agent, launch, take out; Dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
3, the thin-layer chromatography discrimination method of Radix Glycyrrhizae: get need testing solution under above-mentioned 2 as need testing solution, extracting liquorice control medicinal material 1g adds ethanol 20ml in addition; Reflux 1 hour filters, the filtrating evaporate to dryness; Residue adds absolute ethyl alcohol 1ml makes dissolving, filters, and filtrating is as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-methanol-water (volume proportion 36-44: 9-11: 0.8-1.2) be developping agent, launch, take out; Dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical yellow spotting.
4, the content assaying method of burdock glycosides in the medicine: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With methanol-water by volume proportioning be at 35: 65 moving phase, the detection wavelength is 280 ± 2nm.Number of theoretical plate calculates by the burdock glycosides should be not less than 2000.
2) preparation of reference substance solution: it is an amount of to get burdock glycosides reference substance, and accurate the title decides, and adds 50% (g/ml) methyl alcohol and processes the solution that every 1ml contains 0.1mg, promptly gets.
3) preparation of need testing solution: get the about 1g of these article, the accurate title, decide, and puts in the tool plug conical flask, accurate 50% (g/ml) methyl alcohol 25ml that adds; Claim to decide weight, sonicated (power 160w, frequency 50KHz) 20-40 minute is taken out; Put coldly, weigh, supply weight, shake up with 50% (g/ml) methyl alcohol; Filter, get subsequent filtrate, promptly get.
4) determination method: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.The every 1g of these article contains great burdock achene with burdock glycosides (C
27H
34O
11) meter, must not be less than 1.9mg.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution.
The quality determining method of mulberry and chrysanthemum lonicera and forsythia powder of the present invention has improved the quality control standard of mulberry and chrysanthemum lonicera and forsythia powder, has set up assay index and detection method thereof in the preparation; Improved the thin-layer chromatography discrimination method of the capsule of weeping forsythia and Radix Glycyrrhizae; Make its method have more specificity, more accurate, increased the microscopic features of chrysanthemum and great burdock achene, revised the microscopic features of Flos Lonicerae; Make it describe more standard, more accurate, guaranteed this compound preparation higher quality standard level.
Embodiment
Embodiment:
The pharmaceutical formulation of mulberry and chrysanthemum lonicera and forsythia powder is: mulberry leaf 60g, chrysanthemum 60g, Flos Lonicerae 60g, capsule of weeping forsythia 60g, Bulbus Fritillariae Cirrhosae 60g; Balloonflower root 30g, peppermint 40g, lophatherum gracile 60g, schizonepeta 40g, great burdock achene 40g; Semen armeniacae amarae 40g, reed rhizome 60g, cicada slough 60g, stiff silkworm 30g; Talcum 60g, mung bean 60g, Fermented Soybean 20g, Radix Glycyrrhizae 40g.More than 18 the flavor, be ground into fine powder, sieve, mixing promptly gets.These article are lark to filemot powder; Bitter, sweet, little puckery.
The quality determining method of mulberry and chrysanthemum lonicera and forsythia powder of the present invention is:
1, the microscopical identification method of chrysanthemum, Flos Lonicerae and great burdock achene: get mulberry and chrysanthemum lonicera and forsythia powder and put the microscopically observation: pollen granule is yellow, type sphere, and outer wall is thicker, tool bastard, 3 germinal aperatures of tool (chrysanthemum); Pollen granule is yellow, sphere, and outer wall is thin, 3 germinal aperatures of tool (Flos Lonicerae); The endocarp lithocyte is slightly flat, and the surface is seen and is sharp fusiformis, oblong, and sharp oval is inlayed closely (great burdock achene);
2, the thin-layer chromatography discrimination method of the capsule of weeping forsythia: get mulberry and chrysanthemum lonicera and forsythia powder 10g, add ethanol 50ml, sonicated 30 minutes filters; The filtrating evaporate to dryness, residue adds water 20ml makes dissolving, and absorbent cotton filters; Filtrating is extracted 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid; Evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets capsule of weeping forsythia control medicinal material 0.5g, adds ethyl acetate 20ml, and sonicated 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate (volume proportion 20: 1) is developping agent, launches, and takes out; Dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
3, the thin-layer chromatography discrimination method of Radix Glycyrrhizae: get need testing solution under above-mentioned 2 as need testing solution, extracting liquorice control medicinal material 1g adds ethanol 20ml in addition; Reflux 1 hour filters, the filtrating evaporate to dryness; Residue adds absolute ethyl alcohol 1ml makes dissolving, filters, and filtrating is as control medicinal material solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-methanol-water (volume proportion 40: 10: 1) is developping agent, launches, and takes out; Dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical yellow spotting.
4, the content assaying method of burdock glycosides in the medicine: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With methanol-water (volume proportion 35: 65) is moving phase, and the detection wavelength is 280nm.Number of theoretical plate calculates by the burdock glycosides should be not less than 2000.
2) preparation of reference substance solution: it is an amount of to get burdock glycosides reference substance, and accurate the title decides, and adds 50% (g/ml) methyl alcohol and processes the solution that every 1ml contains 0.1mg, promptly gets.
3) preparation of need testing solution: get the about 1g of these article, the accurate title, decide, and puts in the tool plug conical flask, accurate 50% (g/ml) methyl alcohol 25ml that adds; Claim to decide weight, sonicated (power 160w, frequency 50KHz) 30 minutes is taken out; Put coldly, weigh, supply weight, shake up with 50% (g/ml) methyl alcohol; Filter, get subsequent filtrate, promptly get.
4) determination method: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.The every 1g of these article contains great burdock achene with burdock glycosides (C
27H
34O
11) meter, must not be less than 1.9mg.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution.
Mulberry and chrysanthemum lonicera and forsythia powder drug standard after the improvement is:
Mulberry and chrysanthemum lonicera and forsythia powder
Sangju?Yinqiao?San
[prescription] mulberry leaf 60g chrysanthemum 60g Flos Lonicerae 60
Capsule of weeping forsythia 60g Bulbus Fritillariae Cirrhosae 60g balloonflower root 30
Peppermint 40g lophatherum gracile 60g schizonepeta 40g
Great burdock achene 40g semen armeniacae amarae 40g reed rhizome 60g
The stiff silkworm 30g of cicada slough 60g talcum 60g
Mung bean 60g Fermented Soybean 20g Radix Glycyrrhizae 40g
[method for making] above 18 flavors are ground into fine powder, sieve, and mixing promptly gets.
[proterties] these article are lark to filemot powder; Bitter, sweet, little puckery.
These article are got in [discriminating] (1), and put microscopically and observe: pollen granule is yellow, type sphere, and outer wall is thicker, tool bastard, 3 germinal aperatures of tool (chrysanthemum).Pollen granule is yellow, sphere, and outer wall is thin, 3 germinal aperatures of tool (Flos Lonicerae).The endocarp lithocyte is slightly flat, and the surface is seen and is sharp fusiformis, oblong, and sharp oval is inlayed closely (great burdock achene).
(2) get these article 10g, add ethanol 50ml, sonicated 30 minutes filters, the filtrating evaporate to dryness; Residue adds water 20ml makes dissolving, and absorbent cotton filters, and filtrating is extracted 2 times with the ethyl acetate jolting, each 20ml; Combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets capsule of weeping forsythia control medicinal material 0.5g, adds ethyl acetate 20ml, and sonicated 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethyl acetate 1ml makes dissolving, as control medicinal material solution.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 5 μ l; Putting respectively on same silica gel g thin-layer plate, is developping agent with normal hexane-ethyl acetate (20: 1), launches; Take out; Dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) get need testing solution under [discriminating] (2) as need testing solution.Extracting liquorice control medicinal material 1g adds ethanol 20ml in addition, and reflux 1 hour filters, the filtrating evaporate to dryness, and residue adds absolute ethyl alcohol 1ml makes dissolving, filters, and filtrating is as control medicinal material solution.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride-methanol-water (40: 10: 1) is developping agent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical yellow spotting.
[inspection] should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 B) relevant under the powder item.
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With methanol-water (35: 65) is moving phase, and the detection wavelength is 280nm.Number of theoretical plate calculates by the burdock glycosides should be not less than 2000.
It is an amount of that burdock glycosides reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds 50% methyl alcohol and processes the solution that every 1ml contains 0.1mg, promptly gets.
The about 1g of these article is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, and the accurate 50% methyl alcohol 25ml that adds claims to decide weight; Sonicated (power 160w, frequency 50KHz) 30 minutes is taken out, and puts coldly, weighs; Supply weight with 50% methyl alcohol, shake up, filter, get subsequent filtrate, promptly get.
Accurate respectively above-mentioned reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.
The every 1g of these article contains great burdock achene with burdock glycosides (C
27H
34O
11) meter, must not be less than 1.9mg.
[function with cure mainly] suffering table that cools completely is declared the lung cough-relieving, and is clearing heat and detoxicating.Be used for affection of exogenous wind-heat, loathing of cold high fever, headache cough, abscess of throat.
[usage and consumption] is oral, a 10g, 2～3 times on the one.
[specification] every packed 10g.
[storage] is airtight, protection against the tide.
Claims (1)
1. the quality determining method of a mulberry and chrysanthemum lonicera and forsythia powder, the pharmaceutical formulation of mulberry and chrysanthemum lonicera and forsythia powder is: mulberry leaf 60g, chrysanthemum 60g, Flos Lonicerae 60g, capsule of weeping forsythia 60g; Bulbus Fritillariae Cirrhosae 60g, balloonflower root 30g, peppermint 40g, lophatherum gracile 60g, schizonepeta 40g; Great burdock achene 40g, semen armeniacae amarae 40g, reed rhizome 60g, cicada slough 60g, stiff silkworm 30g; Talcum 60g, mung bean 60g, Fermented Soybean 20g, Radix Glycyrrhizae 40g; More than 18 the flavor, be ground into fine powder, sieve, mixing promptly gets; The quality determining method that it is characterized in that mulberry and chrysanthemum lonicera and forsythia powder is:
1) the microscopical identification method of chrysanthemum, Flos Lonicerae and great burdock achene: get mulberry and chrysanthemum lonicera and forsythia powder and put the microscopically observation: pollen granule is yellow, type sphere, and outer wall is thicker, tool bastard, 3 germinal aperatures of chrysanthemum tool; Pollen granule is yellow, sphere, and outer wall is thin, 3 germinal aperatures of Flos Lonicerae tool; The endocarp lithocyte is slightly flat, and the surface is seen and is sharp fusiformis, oblong, and sharp oval, great burdock achene are inlayed closely;
2) the thin-layer chromatography discrimination method of the capsule of weeping forsythia: get mulberry and chrysanthemum lonicera and forsythia powder 10g, add ethanol 40-60ml, sonicated 20-40 minute, filter; The filtrating evaporate to dryness, residue adds water 15-25ml makes dissolving, and absorbent cotton filters; Filtrating is extracted 2-3 time with the ethyl acetate jolting, each 15-25ml, combined ethyl acetate liquid; Evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets capsule of weeping forsythia control medicinal material 0.5g, adds ethyl acetate 15-25ml, and sonicated 20-40 minute, filter, the filtrating evaporate to dryness, residue adds ethyl acetate 1ml makes dissolving, as control medicinal material solution; According to the thin-layered chromatography test, draw above-mentioned need testing solution 5～10 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate; By volume proportioning 17-23: 0.9-1.1 is as developping agent with normal hexane-ethyl acetate, and expansion is taken out, and dries; Spray is with 10%, the g/ml ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
3) the thin-layer chromatography discrimination method of Radix Glycyrrhizae: get need testing solution under above-mentioned 2 as need testing solution, extracting liquorice control medicinal material 1g adds ethanol 15-25ml in addition; Reflux 0.5-1.5 hour; Filter, the filtrating evaporate to dryness, residue adds absolute ethyl alcohol 1ml makes dissolving; Filter, filtrating is as control medicinal material solution; According to thin-layered chromatography test, draw each 10 μ l of need testing solution and above-mentioned control medicinal material solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methanol-water proportioning 36-44: 9-11 by volume: 0.8-1.2 is as developping agent; Launch, take out, dry; Spray is with 10%, the g/ml ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical yellow spotting;
4) content assaying method of burdock glycosides in the medicine: according to high effective liquid chromatography for measuring
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With methanol-water by volume proportioning the detection wavelength was 280 ± 2nm as moving phase in 35: 65;
(2) preparation of reference substance solution: it is an amount of to get burdock glycosides reference substance, and accurate the title decides, and adds 50%, and g/ml methyl alcohol is processed the solution that every 1ml contains 0.1mg, promptly gets;
(3) preparation of need testing solution: get these article 1g, the accurate title, decide, and puts in the tool plug conical flask, accurate 50% methyl alcohol, g/ml, the 25ml of adding; Claim decide weight, sonicated 20-40 minute, taking-up was put coldly, weighs, with 50%; G/ml methyl alcohol is supplied weight, shakes up, and filters, and gets subsequent filtrate, promptly gets;
(4) determination method: accurate respectively above-mentioned reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get, the every 1g of these article contains great burdock achene in the burdock glycosides, must not be less than 1.9mg
Wherein, and " %, g/ml, " represent to contain the some grams of solute among the every 100ml of solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101017942A CN101732608B (en) | 2010-01-27 | 2010-01-27 | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101017942A CN101732608B (en) | 2010-01-27 | 2010-01-27 | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101732608A CN101732608A (en) | 2010-06-16 |
| CN101732608B true CN101732608B (en) | 2012-05-23 |
Family
ID=42456976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101017942A Active CN101732608B (en) | 2010-01-27 | 2010-01-27 | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101732608B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225170B (en) * | 2011-06-08 | 2014-05-07 | 马增旺 | Honeysuckle and broom cypress fruit carminative liquid |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102972599A (en) * | 2012-12-03 | 2013-03-20 | 陶杨杨 | Throat-wetting herbal tea and preparation method thereof |
| CN104435839A (en) * | 2014-12-10 | 2015-03-25 | 葛文农 | Pure traditional Chinese medicine preparation for quickly treating infantile convulsion |
| CN104931642B (en) * | 2015-06-18 | 2016-10-05 | 河北中医学院 | A kind of Fructus Forsythiae medical material and the quick multi information thin-layer identification method of water extract thereof |
| CN105806975B (en) * | 2016-03-14 | 2018-12-04 | 贵阳德昌祥药业有限公司 | A kind of method for building up of Yinqiao San UPLC finger-print |
| CN105866264B (en) * | 2016-03-25 | 2018-07-13 | 贵阳德昌祥药业有限公司 | A kind of detection method of Yinqiao San |
| CN105770648A (en) * | 2016-04-07 | 2016-07-20 | 刘爱红 | Oral traditional Chinese medicine preparation for treating cold |
| CN107247111A (en) * | 2017-06-15 | 2017-10-13 | 江西傲新生物科技有限公司 | The thin-layered chromatography detection method of lophatherum gracile in a kind of Yinqiao San |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840050A (en) * | 2003-12-23 | 2006-10-04 | 江苏康缘药业股份有限公司 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
-
2010
- 2010-01-27 CN CN2010101017942A patent/CN101732608B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840050A (en) * | 2003-12-23 | 2006-10-04 | 江苏康缘药业股份有限公司 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225170B (en) * | 2011-06-08 | 2014-05-07 | 马增旺 | Honeysuckle and broom cypress fruit carminative liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101732608A (en) | 2010-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101732608B (en) | Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder | |
| CN101732463B (en) | Quality detection method for Jinhuaxiaocuo pills | |
| WO2022057360A1 (en) | Pharmaceutical composition for use preventing and curing respiratory diseases in winter | |
| Ghorpade et al. | Pharmacognostic and phytochemical evaluation of Celosia argentea | |
| CN102068600A (en) | Quality control method of venation relaxing and heart-nourishing pill as Chinese herbal preparation | |
| CN102091168A (en) | Quality control method for Chinese medicine preparation Xuefuzhuyu capsule | |
| CN107102093B (en) | The detection method of compound pellet mattress cream | |
| CN101773560A (en) | Method for testing quality of Nguyen supernatant pills | |
| CN101890087A (en) | Composition containing coptis root, rhubarb and baikal skullcap root | |
| CN102068573B (en) | Quality control method for stomach reinforcing and digestion promoting tangerine peel, pinellia, immature bitter orange and atractylodes macrocephala pill | |
| CN109200082A (en) | A method of extracting from emblic, there is antioxidant activity to have Substance simultaneously | |
| CN101732552B (en) | Method for detecting quality of lung clearing and phlegm eliminating pill | |
| CN101732527B (en) | Quality detection method for liver-soothing granules | |
| CN101732553B (en) | Quality inspection method of cough pills | |
| CN102038785B (en) | Detection method for traditional Chinese medicinal preparation of children eyesight pills | |
| CN101057895B (en) | 'Fuyanshu' preparation for treating gynopathy and its quality controlling method | |
| CN102526305A (en) | Chinese medicinal capsules for treating prostatitis and prostatic hyperplasia and preparation method for Chinese medicinal capsules | |
| CN101716270A (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN106706766A (en) | Method for detecting newly increased detection components in traditional Chinese medicinal Tang Herb for treating AIDS | |
| CN102038869B (en) | Quality control method of traditional Chinese medical preparation | |
| CN107014945B (en) | A kind of detection method of Chinese medicine preparation that treating acute infectious hepatitis | |
| CN101269175B (en) | Detection method for comfortable wash liquid for hemorrhoids | |
| CN107202856A (en) | A kind of detection method for the Chinese medicine preparation for treating flu | |
| CN103478342A (en) | Honeysuckle stem type oolong tea processing technology | |
| CN102590430B (en) | Method for detecting liuwei caragana preparation |
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 | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder Effective date of registration: 20140609 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming Dianchi road subbranch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2014990000447 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20160426 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming Dianchi road subbranch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2014990000447 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder Effective date of registration: 20160426 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2016990000339 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20170519 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2016990000339 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for detecting quality of mulberry and chrysanthemum lonicera and forsythia powder Effective date of registration: 20170519 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2017990000427 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20190716 Granted publication date: 20120523 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2017990000427 |