CN109481531A - A kind of composition of benefiting qi and nourishing blood and its preparation method and application - Google Patents

A kind of composition of benefiting qi and nourishing blood and its preparation method and application Download PDF

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CN109481531A
CN109481531A CN201811471613.8A CN201811471613A CN109481531A CN 109481531 A CN109481531 A CN 109481531A CN 201811471613 A CN201811471613 A CN 201811471613A CN 109481531 A CN109481531 A CN 109481531A
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extract
red ginseng
radix codonopsis
donkey hide
parts
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CN109481531B (en
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张淹
刘海滨
张雅丽
周祥山
钱景
史兆松
王春艳
孙阳恩
张路
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Dong E E Jiao Co Ltd
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Dong E E Jiao Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/12Materials from mammals; Compositions comprising non-specified tissues or cells; Compositions comprising non-embryonic stem cells; Genetically modified cells
    • A61K35/36Skin; Hair; Nails; Sebaceous glands; Cerumen; Epidermis; Epithelial cells; Keratinocytes; Langerhans cells; Ectodermal cells
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A61K36/185Magnoliopsida (dicotyledons)
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/734Crataegus (hawthorn)
    • AHUMAN NECESSITIES
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    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/80Scrophulariaceae (Figwort family)
    • A61K36/804Rehmannia
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/14Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
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    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH

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Abstract

The invention discloses compositions of a kind of benefiting qi and nourishing blood and its preparation method and application, belong to processing technique of Chinese herbs field.Composition of the present invention includes the raw material of following parts by weight: 35~55 parts of extract of 21~30 parts of the extract of 24~35 parts of donkey hide extract, red ginseng and hawthorn mixture and Rehmannia glutinosa and Radix Codonopsis mixture.For composition of the present invention compared with common process prepares complex prescription glue mucilage, difference is extremely significant, can effectively improve the content of blood red ball, leucocyte, hemoglobin in blood.The composition of benefiting qi and nourishing blood of the present invention has the effect of better benefiting qi and nourishing blood.

Description

A kind of composition of benefiting qi and nourishing blood and its preparation method and application
Technical field
The invention belongs to processing technique of Chinese herbs fields, and in particular to a kind of composition of benefiting qi and nourishing blood and preparation method thereof and Using.
Background technique
Complex prescription glue mucilage is 2015 editions " Chinese Pharmacopoeia " and records kind, is the common medicine of the qi-blood deficiency class asthenic symptoms of clinical treatment Object has benefiting qi and nourishing blood effect.The prescription and preparation method of the product are public in the patent (97111807.8) of application in 1997 It opens, product prescription are as follows: donkey-hide gelatin, red ginseng, Radix Codonopsis, Rehmannia glutinosa, hawthorn.
Red ginseng mainly contains saponins, polysaccharide, polypeptide, fatty acid, amino acid, polyacetylene alcohols etc., domestic and international medicine Worker unanimously thinks that its active constituent is Ginsenosides, and has separated about more than 40 kinds of ginsenoside, and protoplast's ginseng two Pure and mild protopanaxatriol type saponin(e is the main component in ginsenoside.The main component of hawthorn is flavonoids (castine sandlwood Glucosides, Hyperoside, Vitexin, Quercetin etc.), the ingredients such as glycoside and organic acid, hawthorn is treated both at home and abroad in recent years The research of cardiovascular aspect disease and the research of chemical component triterpene, flavonoids are more, and find haw flavonoids substances quercitrin Element etc. can expand coronary artery, kidney and mesenteric, diastole bronchial smooth muscle, and foreign countries have been applied to clinical treatment thrombotic disease Disease, vasospasm disease and chronic bronchial, at the same pretty equality be experimentally confirmed quercitrin be known as apparent free radical resisting, Inhibit growth of cancer cells, the effect to carcinogenesis carcinogenic factor.
Radix Codonopsis, Rehmannia glutinosa main ingredient be respectively the ingredients such as saponins and polysaccharide.
But the complex prescription glue mucilage of prior art preparation uses traditional water extraction, does not fully consider each taste Chinese medicine In effective component physicochemical property difference, obtained composition do not make full use of the various effective components in drug.Therefore, Need to provide a kind of various effective components more effectively utilized in drug, the better pharmaceutical composition of benefiting qi and nourishing blood effect.
Summary of the invention
In view of this, the purpose of the present invention is to provide composition of a kind of benefiting qi and nourishing blood and its preparation method and application, Described pharmaceutical composition preparation process has fully considered the difference of each flavour of a drug effective component physicochemical property, has selected different preparations Technique, obtained composition benefiting qi and nourishing blood effect are more preferable.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of compositions of benefiting qi and nourishing blood, comprise the following components in parts by weight: donkey hide extract 24~ 35 parts, 35~55 parts of extract of 21~30 parts of the extract and Rehmannia glutinosa of red ginseng and hawthorn mixture and Radix Codonopsis mixture.
Preferably, the raw material including following parts by weight: 25~32 parts of donkey hide extract, red ginseng and haw thorn extract 25~28 Part, 40~50 parts of Rehmannia glutinosa and Radix Codonopsis extract.
Preferably, the preparation method of the donkey hide extract includes: by donkey hide skin obtaining skin liquid, by describedization skin liquid It is mixed with rock sugar, yellow rice wine, obtains mixed liquor, mixed liquor concentration plastic is obtained into donkey hide extract.
Preferably, the protein content in the donkey hide extract is not less than 70% by weight percentage.
Preferably, the preparation method of the extract of the red ginseng and hawthorn mixture includes: to crush red ginseng and hawthorn, is obtained To smashed red ginseng powder and hawthorn powders, obtained red ginseng powder and hawthorn powder are mixed, mixture is obtained, by the mixture with 50~70% ethanol water mixing, obtains mixed extracting solution, the mixed extracting solution is dried to obtain red ginseng With haw thorn extract.
Preferably, the weight ratio of the red ginseng and hawthorn is 1:2~4.
Preferably, total saponin content is not less than 1.5% by weight percentage in the red ginseng and haw thorn extract, described General flavone content is not less than 0.14% by weight percentage in red ginseng and haw thorn extract.
Preferably, the preparation method of the extract of the Rehmannia glutinosa and Radix Codonopsis mixture includes: by Rehmannia glutinosa, Radix Codonopsis and water It is extracted after mixing, the mixture after extraction is separated by solid-liquid separation, extracting solution is obtained;The extracting solution is concentrated to get dense Contracting liquid, then will be dry after 40~85% ethanol solution extraction of the concentrate, obtain Rehmannia glutinosa and Radix Codonopsis extract.
Preferably, the weight ratio of the Rehmannia glutinosa and Radix Codonopsis is 1:0.5~1.5.
Preferably, the Rehmannia glutinosa is not less than 0.04% with total saponin content in Radix Codonopsis extract by weight percentage.
The application that the present invention also provides above-mentioned compositions in terms of preparing qi-invigorating, blood-nourishing medicinal.
This application provides a kind of composition, by by the extract of donkey hide extract, red ginseng and hawthorn mixture and ripe Glutinous rehmannia compounds with the extract of Radix Codonopsis mixture, by red ginseng, Radix Codonopsis tonifying middle-Jiao and Qi, donkey hide extract nourishing yin and supplementing blood, hawthorn row Stagnant stagnation resolvation, elimination taste are greasy, have obtained the effect of better benefiting qi and nourishing blood.
Specific embodiment
The present invention provides a kind of compositions of benefiting qi and nourishing blood, comprise the following components in parts by weight: donkey hide extract 24~ 35 parts, 35~55 parts of extract of 21~30 parts of the extract and Rehmannia glutinosa of red ginseng and hawthorn mixture and Radix Codonopsis mixture.
It include donkey hide extract in the composition provided by the invention, donkey hide extract of the present invention is in the combination Parts by weight in object are preferably 25~32 parts, more preferably 27~31 parts, most preferably 29 parts.Donkey hide extract of the present invention In protein content by weight percentage be preferably not less than 70%, more preferably be not less than 80%.Donkey hide of the present invention The effect of extract is nourishing yin and supplementing blood.
In the present invention, the preparation method of the donkey hide extract is preferably included by donkey hide skin obtaining skin liquid, by institute Stating skin liquid is mixed with rock sugar, yellow rice wine, obtains mixed liquor, and mixed liquor concentration plastic is obtained donkey hide extract.
Stripping and slicing after the preparation method of of the present inventionization skin liquid preferably impregnates donkey hide, obtains donkey hide block, by the donkey Skin is washed after skin bit, sodium carbonate and water mixing, the donkey hide after being cleaned, then change after the donkey hide after cleaning is mixed with water Skin, obtaining skin liquid.Immersion of the present invention is preferably water with liquid, and the soaking time is preferably 3~5 days, more preferably 4 It.The present invention preferably changes water 1~3 time daily in the immersion, more preferably changes water 2 times.It is of the present invention to wash Pi Yuhua skin step Suddenly it is preferably carried out in change skin machine.It is of the present invention wash skin during add sodium carbonate.The additive amount of the sodium carbonate is preferred It is the 1.1~1.3% of donkey hide block weight, more preferably 1.15~1.25%, most preferably 1.2%.It is of the present invention to wash skin use Liquid is preferably water, and the additive amount of the water is preferably 1.8~2.0 times of the donkey hide block weight, more preferably 1.9 times.This hair Washing the temperature of skin described in bright is preferably 60~80 DEG C, more preferably 62~68 DEG C, most preferably 65 DEG C.The skin of the present invention washed When temperature reaches 60~80 DEG C, it can exclude to wash the severe edema due to hypofunction of the spleen.The present invention is added sodium carbonate and water preferably since donkey hide block to row It is once to wash skin except this process of the severe edema due to hypofunction of the spleen is washed.The number of the present invention for washing skin is preferably 2~4 times, and more preferably 3 times.
It is once to wash skin that the present invention, which washes this process of the severe edema due to hypofunction of the spleen to exclusion adding sodium carbonate and water preferably since donkey hide block,. The number of the present invention for washing skin is preferably 2~4 times, and more preferably 3 times.
In the present invention, when describedization skin, the weight of the water be preferably the donkey hide weight after the cleaning 1.2~ 1.8 times, more preferably 1.4~1.6 times, most preferably 1.5 times.The temperature of of the present inventionization skin is preferably 110~120 DEG C, More preferably 112~118 DEG C, most preferably 115 DEG C.The number of describedization skin is preferably 2~4 times, and more preferably 3 times.It is described The time for changing skin is preferably 150~170 minutes/time, more preferably 155~165 minutes/time, most preferably 160 minutes/time.
After obtaining skin liquid, the present invention mixes describedization skin liquid with rock sugar, yellow rice wine, obtains mixed liquor, by the mixing Liquid concentration plastic obtains donkey hide extract.In the present invention, it is also preferable to include change what skin liquid was centrifuged and was concentrated before the mixing Step, the revolving speed of the centrifugation are preferably 6500~7500r/ minutes, more preferably 7000r/ minutes.When centrifugation of the present invention The flow velocity for changing skin liquid is preferably 30~50kg/ minutes, more preferably 35~45kg/ minutes, most preferably 40kg/ minutes.This hair Temperature when the bright concentration is preferably 60~80 DEG C, more preferably 65~75 DEG C, most preferably 70 DEG C.Mixing of the present invention Liquid concentration plastic obtains donkey hide extract, and the moisture content of donkey hide extract of the present invention is preferably 65~75%, more preferably It is 68~72%, most preferably 70%.Rock sugar of the present invention is preferably rock sugar solution, and the mass concentration of the rock sugar solution is excellent It is selected as 38~42%, more preferably 39~41%, most preferably 40%.The additive amount of rock sugar solution of the present invention is preferably donkey The 7.2~7.8% of tare weight amount, more preferably 7.6%.In the present invention, the rock sugar can improve the mouthfeel of glue.Institute of the present invention The additive amount for stating yellow rice wine is preferably the 1.3~1.5% of donkey hide weight, more preferably 1.4%.The effect of yellow rice wine of the present invention is Improve the mouthfeel of glue.The present invention does not have special restriction to the source of the donkey hide, is using this field conventional commercial product It can.The present invention does not have special restriction to the source of the sodium carbonate, selects this field conventional commercial product.The present invention couple The source of the rock sugar and yellow rice wine does not have special restriction, selects this field conventional commercial product.
Composition provided by the invention includes the extract of red ginseng and hawthorn mixture.The red ginseng and hawthorn mixture The parts by weight of extract are preferably 25~28 parts, more preferably 25.5~27 parts, most preferably 26 parts.Red ginseng of the present invention with The effect of the extract of hawthorn mixture in this application is tonifying Qi and invigorating the spleen.
In the present invention, the preparation method of the red ginseng and the extract of hawthorn mixture preferably includes: by red ginseng and mountain Short, bristly hair or beard crushes, and obtains smashed red ginseng powder and hawthorn powder, and obtained red ginseng powder and hawthorn powder are mixed, mixture is obtained, by institute The ethanol water that mixture is stated with 50~70% mixes, and obtains mixed extracting solution, and the mixed extracting solution is done It is dry to obtain red ginseng and haw thorn extract.The preferred red ginseng medicine materical crude slice of red ginseng of the present invention, red ginseng medicine materical crude slice of the present invention preferably conform to Medicine materical crude slice requirement under 2015 editions " Chinese Pharmacopoeia " red ginseng items of page 153.The preferred uctus Crataegi of hawthorn of the present invention, the uctus Crataegi Preferably conform to the lower medicine materical crude slice requirement of 2015 editions " Chinese Pharmacopoeia " hawthorn of page 31.The weight ratio of red ginseng of the present invention and hawthorn is preferred For 1:2~4, more preferably 1:3.Red ginseng of the present invention is not preferably low by weight with total saponin content in haw thorn extract In 1.5%, more preferably it is not less than 2% by weight.Red ginseng of the present invention and general flavone content in haw thorn extract are preferred It is not less than 0.14% by weight percentage, is more preferably not less than 0.15%.Red ginseng of the present invention and hawthorn are smashed Partial size preferably can all by 24 meshes, but be mixed with can pass through 65 meshes no more than 40% powder.Ethyl alcohol of the present invention Weight be preferably 16~22 times of 10~28 times of red ginseng and hawthorn total weight, more preferably red ginseng and hawthorn total weight, most Preferably 18 times.It is 50%~70% ethanol water that the present invention, which preferably uses volume fraction, is more preferably 55 with volume fraction ~65% ethanol water, the ethanol water that optimal selection volume fraction is 60%.Red ginseng of the present invention and hawthorn with The incorporation time of ethanol water is preferably 8~18 hours, more preferably 14~17 hours, most preferably 16 hours.The present invention Percolate is preferably collected with the flow velocity of 12~36ml/min*kg after the mixing, more preferably 22~26ml/min*kg is optimal It is selected as 24ml/min*kg.Ethyl alcohol is recycled after collection percolate of the present invention, is concentrated, is dried to obtain the extraction of red ginseng and hawthorn Object.
Composition provided by the invention includes the extract of Rehmannia glutinosa Yu Radix Codonopsis mixture.The Rehmannia glutinosa is mixed with Radix Codonopsis The parts by weight of the extract of object are preferably 40~50 parts, more preferably 42~48 parts, most preferably 45 parts.Radix rehmanniae preparata of the present invention The yellow effect with the extract of Radix Codonopsis mixture is to fill blood.
In the present invention, the preparation method of the extract of the Rehmannia glutinosa and Radix Codonopsis mixture, preferably includes following steps: It is extracted after Rehmannia glutinosa, Radix Codonopsis and water are mixed, the mixture after extraction is separated by solid-liquid separation, extracting solution is obtained;By institute It states extracting solution and is concentrated to get concentrate, then will be dry after 40~85% ethanol solution extraction of the concentrate, obtain radix rehmanniae preparata Yellow and Radix Codonopsis extract.The preferred Rehmannia glutinosa medicine materical crude slice of Rehmannia glutinosa of the present invention, Rehmannia glutinosa medicine materical crude slice of the present invention preferably conform to Medicine materical crude slice requirement under 2015 editions " Chinese Pharmacopoeia " Rehmannia glutinosa items of page 125.The preferred Radix Codonopsis medicine materical crude slice of Radix Codonopsis of the present invention, the Radix Codonopsis drink Piece preferably conforms to medicine materical crude slice requirement under 2015 editions " Chinese Pharmacopoeia " Radix Codonopsis items of page 125.The weight of Rehmannia glutinosa and Radix Codonopsis of the present invention Than being preferably 1:0.5~1.5, more preferably 1:0.7~1.2, most preferably 1:1.Rehmannia glutinosa of the present invention and Radix Codonopsis extract Total saponin content is preferably not less than 0.04% by weight in object, is more preferably not less than 0.05% by weight.The present invention The number of the extraction is preferably 3 times.The method of separation of solid and liquid of the present invention preferably filters.The present invention preferably mentions 3 times The extracting solution obtained after taking merges, and obtains mixed extracting solution.Extraction of the present invention preferably includes: first extracts, The weight ratio of water and Rehmannia glutinosa and Radix Codonopsis mixture is preferably 4~6:1 when second extraction is extracted with third extraction, described first, More preferably 4.5~5.5:1, most preferably 5:1.First extraction of the present invention preferably carries out under normal pressure.The present invention into Row described first is preferably stirred when extracting, and the speed of agitator is preferably 1~3r/min, more preferably 2r/min.This hair Bright described first temperature extracted is preferably 100 DEG C.Of the present invention first time extracted was preferably 80~100 minutes, more Preferably 85~95 minutes, most preferably 90 minutes.The present invention collects the first extracting solution and the first filter residue after the first extraction, will First filter residue carry out second extract, described second extract when, the mass ratio of the first filter residue and water is preferably 1:2~4, more preferably 1:3.Of the present invention second temperature extracted and pressure are preferably identical as the first extraction.Of the present invention second time extracted Preferably 50~70 minutes, more preferably 60 minutes.The present invention collects the second filtrate and the second filter residue after the second extraction, will The second filter residue arrived carries out third extraction, and the temperature and pressure when the third is extracted are preferably identical as the first extraction.The present invention When the third is extracted, the mass ratio of second filter residue and water is preferably 1:1.3~1.7, more preferably 1:1.5.Described Three times extracted were preferably 30~50 minutes, and more preferably 40 minutes.The third filtrate and first that the present invention will preferably obtain Filtrate and the mixing of the second filtrate, obtain extracting solution.Extracting solution of the present invention is preferably concentrated, and concentrate is obtained.The present invention Crude drug amount after the concentration is preferably 0.2~0.5g/ml, more preferably 0.25~0.45g/ml, most preferably 0.3g/ml. Crude drug amount of the present invention is The Quality of Sliced Herbal Medicine.
After obtaining concentrate, the present invention will be dry after 40~85% ethanol solution extraction by concentrate, obtains Rehmannia glutinosa and Radix Codonopsis extract.The step of extracting concentrate with ethanol solution of the present invention includes being added under stirring Ethanol solution after standing, is concentrated after taking supernatant to recycle ethanol solution, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract.The present invention Described the step of extracting concentrate with ethanol solution, preferably carries out 2 times, and respectively first time ethanol solution extracts and second Ethanol solution extracts.First time ethanol solution of the present invention extracts the ethanol solution that preferred volume score is 40~60%, more Preferably volume fraction be 45~55% ethanol solution, most preferably volume fraction be 50% ethanol solution.Institute of the present invention State time of repose preferably 6~20 hours, more preferably 12~19 hours, most preferably 18 hours.The temperature of standing of the present invention Preferably 5~30 DEG C of degree, more preferably 10~29 DEG C, most preferably 28 DEG C.Second of ethanol solution of the present invention extracts excellent Select volume fraction be 60~85% ethanol solution, more preferably volume fraction be 70~82% ethanol solution, most preferably The ethanol solution that volume fraction is 80%.Time of repose of the present invention preferably 6~20 hours, more preferably 12~19 hours, Most preferably 18 hours.The temperature of standing of the present invention is preferably 5~30 DEG C, more preferably 10~29 DEG C, most preferably 28 ℃。
The application that the present invention also provides above-mentioned compositions in terms of preparing qi-invigorating, blood-nourishing medicinal.
In this application, red ginseng, Radix Codonopsis tonifying middle-Jiao and Qi, donkey hide extract nourishing yin and supplementing blood, the stagnant stagnation resolvation of hawthorn row, elimination are grown It is greasy.
Composition provided by the invention is described in detail below with reference to embodiment, but they cannot be interpreted as Limiting the scope of the present invention.
Embodiment 1
1, donkey hide extract is prepared
By donkey hide 40kg water impregnate 4 days, change daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.5 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
2.1 total saposins measuring methods
2.1.1 the preparation of standard curve
It is 0.94mg/ml ginsenoside Re reference substance (lot number 0754- that precision, which draws 75,100,125,150,175 μ l concentration, 9913) in 10ml tool plug test tube, methanol is flung in water-bath, it is cooling, residue add 0.2ml5% vanillic aldehyde glacial acetic acid solution and 0.8ml perchloric acid mixes, and in 60 DEG C of water bath with thermostatic control 15min, taking-up cools down immediately, then plus 5ml glacial acetic acid, shake up, in 560nm Colorimetric estimation.
2.1.2 the measurement of test solution
Precision draws test sample 10ml, flings to ethyl alcohol in water-bath in evaporating dish, residue adds water 20ml to make to dissolve, sets liquid separation It in funnel, is extracted twice with ether defatting, each 20ml, water layer flings to ether, the n-butanol extraction being saturated with water four times, every time 20ml merges n-butanol extracting liquid, sets water bath method in evaporating dish, residue adds water 10ml to make to dissolve, the upper D101 pre-processed Macroporous resin column is first washed with 80ml, is then washed with 60ml20% ethyl alcohol, then with 60ml70% ethanol elution, collects 70% second For alcohol eluen in being evaporated in water-bath, residue adds methanol to dissolve, and is transferred in 10ml measuring bottle, adds proper amount of methanol to scale, mixes, i.e., For test solution.
Precision draws 0.2ml test solution in 10ml tool plug test tube, and methanol is flung in water-bath, cooling, and residue adds 0.2ml5% vanillic aldehyde glacial acetic acid solution and 0.8ml perchloric acid mix, and in 60 DEG C of water bath with thermostatic control 15min, taking-up cools down immediately, Again plus 5ml glacial acetic acid, it shakes up, obtains the amount of total saposins in 560nm colorimetric estimation.
2.2 Determination of Total Flavonoids methods
2.2.1 the preparation of standard curve
Draw concentration be 52 μ g/ml rutin (lot number 080-9002) standard solution 0,1.0,2.0,3.0,4.0,5.0ml in In 10ml colorimetric cylinder, adds methanol to scale, shake up, Yu Bochang 360nm measurement absorbs.
2.2.2 the measurement of test solution
Precision draws this product 20ml, flings to ethyl alcohol in water-bath in evaporating dish, residue adds water 20ml to make to dissolve, and adds 3g polyamides Amine powder (30~60 mesh) adsorb 30min, absorbent cotton filtering, be first washed to 80ml it is colourless, transfer set in conical flask, add 30ml Methanol ultrasound 15min filtering, filtrate are concentrated into 25ml measuring bottle, add proper amount of methanol to scale, mix, as test solution.
Precision draws 2ml test solution in 10ml tool plug test tube, adds 8ml methanol, shakes up, in 360nm colorimetric estimation.
2.3 prepare red ginseng and haw thorn extract
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 60% ethanol solution that medicinal material total amount is 18 times of amounts is added, after impregnating 16 hours, with The flow velocity of 12ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 4.400mg/g, general flavone content 0.296mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.2g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 60%, when temperature reaches 28 degrees Celsius After standing 18 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then in stirring Lower addition ethyl alcohol makes ethanol content reach 80%, and temperature reached 28 degrees Celsius of standings after 18 hours, and supernatant is taken to recycle ethyl alcohol, Concentration, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 20.34mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 2
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 3 days, is changed daily water 1 time, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.1%Na2CO3With 1.8 times of water, heating makes coolant-temperature gage up to 60 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.2 times of donkey hide weight of water, heating to keep temperature 150 minutes at 112 DEG C, collectionization skin liquid, repetitionization skin 2 After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 30kg/ minutes states, centrifugate is concentrated at 60 DEG C, until from Heart glue be evaporated to moisture content be 65% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.3% of donkey hide weight 7.2% is added Plastic is concentrated in yellow rice wine, spare;
3, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 50% ethanol solution that medicinal material total amount is 14 times of amounts is added, after impregnating 16 hours, with The flow velocity of 36ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 3.896mg/g, general flavone content 0.321mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 1/3g/ml, 90% ethyl alcohol is added under stirring, so that ethyl alcohol volume parts is reached 60%, temperature reaches quiet at 5 degrees Celsius After setting 12 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then under stirring Ethyl alcohol is added, so that ethanol content is reached 80%, temperature reached 5 degrees Celsius of standings after 12 hours, and supernatant is taken to recycle ethyl alcohol, dense Contracting, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 18.65mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 3
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 5 days, is changed daily water 3 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.3%Na2CO3With 2.0 times of water, heating makes coolant-temperature gage up to 80 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.8 times of donkey hide weight of water, heating to keep temperature 160 minutes at 120 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 50kg/ minutes states, centrifugate is concentrated at 75 DEG C, until from Heart glue be evaporated to moisture content be 75% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.5% of donkey hide weight 7.8% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 50% ethanol solution that medicinal material total amount is 18 times of amounts is added, after impregnating 12 hours, with The flow velocity of 24ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 4.400mg/g, general flavone content 0.296mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.2g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 50%, when temperature reaches 15 degrees Celsius After standing 12 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then in stirring Lower addition ethyl alcohol makes ethanol content reach 70%, and temperature reached 15 degrees Celsius of standings after 12 hours, and supernatant is taken to recycle ethyl alcohol, Concentration, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 16.70mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 4
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 3 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.8 times of water, heating makes coolant-temperature gage up to 67 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.6 times of donkey hide weight of water, heating to keep temperature 158 minutes at 117 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 70% ethanol solution that medicinal material total amount is 10 times of amounts is added, after impregnating 16 hours, with The flow velocity of 24ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 3.863mg/g, general flavone content 0.252mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.2g/ml, 90% ethyl alcohol is added under stirring, so that ethyl alcohol volume parts is reached 40%, temperature reaches quiet at 5 degrees Celsius After setting 6 hours, take supernatant recycle ethyl alcohol after, and be concentrated into medical fluid containing crude drug amount be 0.2g/ml when, then under stirring plus Enter ethyl alcohol, ethanol content is made to reach 60%, temperature reached 5 degrees Celsius of standings after 6 hours, takes supernatant to recycle ethyl alcohol, is concentrated, does It is dry to obtain Rehmannia glutinosa and Radix Codonopsis extract, it is spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 15.98mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 5
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 4 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.4 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 60% ethanol solution that medicinal material total amount is 14 times of amounts is added, after impregnating 8 hours, with The flow velocity of 24ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 2.730mg/g, general flavone content 0.339mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.25g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 60%, when temperature reaches 15 degrees Celsius After standing 6 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then under stirring Ethyl alcohol is added, so that ethanol content is reached 80%, temperature reached 15 degrees Celsius of standings after 6 hours, and supernatant is taken to recycle ethyl alcohol, dense Contracting, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 15.98mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 6
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 4 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.7 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 60% ethanol solution that medicinal material total amount is 10 times of amounts is added, after impregnating 12 hours, with The flow velocity of 36ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 3.398mg/g, general flavone content 0.273mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 1/3g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 40%, when temperature reaches 15 degrees Celsius After standing 18 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then in stirring Lower addition ethyl alcohol makes ethanol content reach 60%, and temperature reached 15 degrees Celsius of standings after 18 hours, and supernatant is taken to recycle ethyl alcohol, Concentration, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 14.84mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 7
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 4 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.5 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 50% ethanol solution that medicinal material total amount is 10 times of amounts is added, after impregnating 8 hours, with The flow velocity of 12ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 2.349mg/g, general flavone content 0.320mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.25g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 40%, when temperature reaches 28 degrees Celsius After standing 12 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then in stirring Lower addition ethyl alcohol makes ethanol content reach 60%, and temperature reached 28 degrees Celsius of standings after 12 hours, and supernatant is taken to recycle ethyl alcohol, Concentration, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 13.46mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 8
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 4 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.6 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 70% ethanol solution that medicinal material total amount is 14 times of amounts is added, after impregnating 12 hours, with The flow velocity of 12ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 2.892mg/g, general flavone content 0.266mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 0.25g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 50%, when temperature reaches 5 degrees Celsius After standing 18 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then in stirring Lower addition ethyl alcohol makes ethanol content reach 70%, and temperature reached 5 degrees Celsius of standings after 18 hours, and supernatant is taken to recycle ethyl alcohol, dense Contracting, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 10.31mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
Embodiment 9
1, donkey hide extract is prepared
Donkey hide 40kg is soaked in water 4 days, is changed daily water 2 times, soak cut after cleaning up it is blocking;Skin bit is in change skin machine It is interior, add donkey hide weight 1.2%Na2CO3With 1.9 times of water, heating makes coolant-temperature gage up to 65 DEG C, and draining-off sewage, repeated washing is three times Afterwards;After adding 1.8 times of donkey hide weight of water, heating to keep temperature 160 minutes at 115 DEG C, collectionization skin liquid, repetitionization skin three After secondary, collectionization skin liquid, after filtering, flow control are centrifuged under 40kg/ minutes states, centrifugate is concentrated at 70 DEG C, until from Heart glue be evaporated to moisture content be 70% or so mention it is miscellaneous after, the rock sugar solution and donkey hide weight 1.4% of donkey hide weight 7.6% is added Plastic is concentrated in yellow rice wine, spare;
2, red ginseng and haw thorn extract are prepared
Red ginseng medicine materical crude slice 5kg, uctus Crataegi 15kg, being respectively crushed into can be all by the coarse powder of 24 meshes, according to the ratio of 1:3 Example weighs red ginseng coarse powder and hawthorn coarse powder, and 70% ethanol solution that medicinal material total amount is 18 times of amounts is added, after impregnating 8 hours, with The flow velocity of 36ml/min*kg collects percolate, is concentrated after recycling ethyl alcohol, is dried to obtain the extract of red ginseng and hawthorn.According to 2.1 Total saponin content with 2.2 method measurement extract is 4.400mg/g, general flavone content 0.296mg/g.
3, Radix Codonopsis and prepared rehmannia root extract are prepared
Take the Rehmannia glutinosa medicine materical crude slice and Radix Codonopsis medicine materical crude slice 50kg of weight ratio 1:1,5 times of amount water of dosing material weight, after impregnating 30 minutes, Under normal pressure state, speed of agitator 2r/min, boiling is extracted 90 minutes, and filtrate is collected in filtering;Second of 3 times of dosing material weight Water is measured, under normal pressure state, boiling is extracted 60 minutes, and filtrate is collected in filtering;1.5 times of amount water of third time dosing material weight, normal Under pressure condition, boiling is extracted 40 minutes, and filtrate is collected in filtering;Above-mentioned filtrate three times is mixed, filtrate is concentrated into is containing crude drug amount When 1/3g/ml, 90% ethyl alcohol is added under stirring, ethyl alcohol volume parts is made to reach 50%, when temperature reaches 28 degrees Celsius After standing 6 hours, after taking supernatant to recycle ethyl alcohol, and when to be concentrated into medical fluid containing crude drug amount be 0.2g/ml, then under stirring Ethyl alcohol is added, so that ethanol content is reached 70%, temperature reached 28 degrees Celsius of standings after 6 hours, and supernatant is taken to recycle ethyl alcohol, dense Contracting, is dried to obtain Rehmannia glutinosa and Radix Codonopsis extract, spare;
The total saponin content of the Rehmannia glutinosa and Radix Codonopsis extract that measure according to the method for 2.1 parts in embodiment 1 is 10.30mg/80g crude drug.
4, donkey hide extract, red ginseng and haw thorn extract obtained above and Radix Codonopsis and prepared rehmannia root extract are crushed respectively It sieves with 100 mesh sieve and to can all lead to containing being mixed after capable of being no less than 95% powder by 120 meshes, obtains mixture.
The Testing index present invention measures the composition of the Examples 1 to 9 of preparation and the active constituent content of complex prescription glue mucilage It see the table below 1.
The composition each 1g and complex prescription glue mucilage 2ml for weighing embodiment 1-9, are detected using identical method.
Detection method:
Instrument: LC-MS/MS LC-MS instrument: 1290 high performance liquid chromatograph of Agilent (Agilent, USA), TSQ QuantumAccess Max type mass spectrograph (Thermo Fisher, USA).
1. liquid phase and mass spectral analysis condition
1.1 Mass Spectrometry Conditions
Collision gas is ultrapure helium, and sheath gas and auxiliary gas are High Purity Nitrogen;Electrospray ionisation (ESI), detection pattern are anion Mode;Sheath gas (Shoath Gas Pressure): 40psi;Auxiliary gas (Aux Gas Pressure): 20psi;Heter temperature (Temp): 350 DEG C;Voltage (IonSpray): -3000V;It uses choice ion pattern (MRM).
Main component selects each ion and design parameter as shown in table 1 in complex prescription glue mucilage:
1 HPLC-MS/MS of table measures the mass spectrometry parameters optimum results of 6 components Components simultaneously
1.2 chromatographic condition
Chromatographic condition: AgilentZorbax SB-C18 (250mm × 4.6mm, 5 μm);Mobile phase: A phase (0.02% first Acid/water)-B phase (0.02% formic acid/acetonitrile);Flow velocity: 0.5ml/min;Column temperature: 30 DEG C;Sample injection volume: 20 μ L.Linear gradient Elution, gradient are as shown in table 2.
2 gradient of table
2. the preparation of standard solution
The preparation of 2.1 inner mark solutions takes aurantiin, appropriate digoxin, adds 80% methanol that every 1ml is made containing 200 μ g, 150 μ g Inner mark solution to get.
The preparation of 2.2 reference substance solutions takes chlorogenic acid, acteoside, Isoacteoside, lobetyolin, 20 (S)-ginseng soaps Glycosides Rg2,20 (R)-ginsenoside Rg2s, 20 (S) appropriate reference substances, it is accurately weighed, add 70% methanol be made every 1ml contain respectively it is green 110 μ g of ortho acid, 100 μ g of acteoside, 200 μ g of Isoacteoside, 280 μ g of lobetyolin, 20 (S)-ginsenoside Rg2,200 μ g, The mixed standard solution of 20 (R)-ginsenoside Rg2,150 μ g, it is spare.
Precision measures the blank solution 2mL of removal medicinal material, sets in 15mL centrifuge tube, takes 5 parts altogether, accurate respectively that mixed mark is added 5,10,20,40,80 μ L of solution respectively complements to 80 μ L with 70% methanol, then accurate respectively above-mentioned aurantiin is added, in digoxin Mark each 40 μ L of solution, oscillation mixing 10min;Acetonitrile 6mL is added in precision, and oscillation mixes 10min, stands 12h in 4 DEG C of refrigerators;From The heart (2500rpm, 4 DEG C) 20min.Precision measures supernatant 2.5mL, is concentrated to dryness in 45 DEG C, is turned with the dissolution of 30% methanol It moves in 5ml measuring bottle, is settled to scale, shake up, filter to get control series product solution.
The preparation of 2.3 standard curves is accurate respectively to draw above-mentioned 10 μ l of control series product solution (concentration see the table below 3), injection Liquid chromatograph carries out LC-MS/MS analysis measurement.Using the amount of each reference substance as abscissa, with each peak area with it is corresponding Interior target peak area (chlorogenic acid, acteoside, Isoacteoside, lobetyolin using aurantiin as internal standard, 20 (S)-ginsenosides Rg2,20 (R)-ginsenoside Rg2s are using digoxin as internal standard) ratio is ordinate, standard curve drawn, see the table below 3.
3 standard curve concentration of table (μ g/mL)
3. the preparation of test solution
The preparation precision of test solution measures this product 2mL or 1g and dissolves into 2ml, sets in 15mL centrifuge tube, and precision adds Above-mentioned aurantiin, each 40 μ L of digoxin inner mark solution, oscillation mixing 10min is added in 70% methanol, 80 μ L, precision;Accurate plus second again Nitrile 6mL, oscillation mix 10min, stand 12h in 4 DEG C of refrigerators;It is centrifuged (2500rpm, 4 DEG C) 20min.Precision measures supernatant 2.5mL is concentrated to dryness in 45 DEG C, with 30% methanol solution transfer into 5ml measuring bottle, is settled to scale, is shaken up, filtration, To obtain the final product.
4. measuring method precision draws each 10 μ l of test solution, liquid chromatograph is injected, carries out LC-MS/MS analysis measurement, From the amount of each ingredient read on standard curve in test solution, calculate to get as a result, being shown in Table 4.
The composition effective component of 4 the application of table preparation and the effective component contrast table of primary blood medicament for enriching blood
Comparative example 1
1, this research of purpose is small to BALB/c by the composition of effective extract of the observation based on complex prescription glue mucilage prescription The therapeutic effect of mouse blood loss anemia model, and be compared with the raw material of complex prescription glue mucilage prescription.
2 methods take BALB/c mouse 80, and ♀ ♂ is fifty-fifty.8 groups are randomly divided into according to weight, normal blank control group (Con Group), model control group (Mod group), raw material low dose group (YL group), raw material middle dose group (YM group), raw material high dose group (YH Group), new process low dose group (L group), new process middle dose group (M group) and new process high dose group (H group).
Con group: without any processing;Mod group: sterile purified water is given;YL group: 600mgkg-1;YM group: 1200mg kg-1;YH group: 2400mgkg-1;L group: 600mgkg-1;M group: 1200mgkg-1;H group: 2400mgkg-1
Every group 10, ♀ ♂ is fifty-fifty.After grouping, in addition to Con group animal, it is small that other groups of animals eye sockets take blood 0.5ml to cause Mouse blood loss anemia model.WBC is detected before blood loss and after blood loss for 24 hours;Subsequent successive administration 7d, for 24 hours every after the last administration Mouse orbit takes blood examination to survey WBC, the results are shown in Table 5.
5 testing result of table
Note: * is compared with Con, P < 0.01 * P < 0.05, * *;△ is compared with Mod, P < 0.01 △ P < 0.05, △ △
Before 3 result mouse blood loss modelings, compared with Mod group, WBC index is showed no obvious abnormalities each group.After blood loss for 24 hours, Mod group and each administration group each index compared with Con group reduce, and have statistical difference (P < 0.05 or P < 0.01);Each administration group Statistical difference is had no compared with Mod group, shows that Anemia model is established substantially.After administration, compared with Con group, Mod group is each Index is relatively low, and raw material YH group WBC index increases (P < 0.05), and each administration group index of new process is normal;With Mod group ratio Compared with each index value of administration group increases, and wherein raw material YH group WBC is significantly raised, has significant difference (P < 0.05).
Under 4 conclusion this experimental condition, the application composition has certain therapeutic effect to chmice acute blood loss anemia, WBC value increases, and the application composition is compared with compound ass-hide gelatin raw material with certain advantage.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of composition of benefiting qi and nourishing blood, comprises the following components in parts by weight: 24~35 parts of donkey hide extract, red ginseng and hawthorn 35~55 parts of extract of 21~30 parts of the extract of mixture and Rehmannia glutinosa and Radix Codonopsis mixture.
2. composition according to claim 1, which is characterized in that the raw material including following parts by weight: donkey hide extract 25 ~32 parts, red ginseng with 25~28 parts of haw thorn extract, 40~50 parts of Rehmannia glutinosa and Radix Codonopsis extract.
3. composition according to claim 1 or 2, which is characterized in that the preparation method of the donkey hide extract include: by Donkey hide skin obtaining skin liquid, describedization skin liquid is mixed with rock sugar, yellow rice wine, mixed liquor is obtained, the mixed liquor is condensed into Glue obtains donkey hide extract.
4. composition according to claim 3, which is characterized in that the protein content in the donkey hide extract is by weight Percentages are not less than 70%.
5. composition according to claim 1 or 2, which is characterized in that the extract of the red ginseng and hawthorn mixture Preparation method includes: to crush red ginseng and hawthorn, smashed red ginseng powder and hawthorn powder is obtained, by obtained red ginseng powder and hawthorn Powder mixing, obtains mixture, the mixture is mixed with 50~70% ethanol water, obtains mixed extracting solution, The mixed extracting solution is dried to obtain red ginseng and haw thorn extract.
6. composition according to claim 4, it is characterised in that: the weight ratio of the red ginseng and hawthorn is 1:2~4, institute It states total saponin content in red ginseng and haw thorn extract and is not less than 1.5% by weight percentage, the red ginseng and haw thorn extract Middle general flavone content is not less than 0.14% by weight percentage.
7. composition according to claim 1 or 2, which is characterized in that the extract of the Rehmannia glutinosa and Radix Codonopsis mixture Preparation method include: by Rehmannia glutinosa, Radix Codonopsis and water mix after extract, the mixture after extraction is separated by solid-liquid separation, Obtain extracting solution;The extracting solution is concentrated to get concentrate, then 40~85% ethanol solution of the concentrate is extracted After dry, obtain Rehmannia glutinosa and Radix Codonopsis extract.
8. composition according to claim 7, which is characterized in that the weight ratio of the Rehmannia glutinosa and Radix Codonopsis be 1:0.5~ 1.5。
9. composition according to claim 7, which is characterized in that total saponin content in the Rehmannia glutinosa and Radix Codonopsis extract It is not less than 0.04% by weight percentage.
10. application of the composition according to any one of claims 1 to 9 in terms of preparing qi-invigorating, blood-nourishing medicinal.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114306372A (en) * 2021-12-07 2022-04-12 兰州大学 Polysaccharide extract of traditional Chinese medicine composition and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN102526106A (en) * 2010-12-31 2012-07-04 山东东阿阿胶股份有限公司 Donkey-hide gelatine raw powder and preparation method thereof
CN104069242A (en) * 2013-07-09 2014-10-01 山东东阿阿胶股份有限公司 Nano composition of compound e-jiao slurry and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102526106A (en) * 2010-12-31 2012-07-04 山东东阿阿胶股份有限公司 Donkey-hide gelatine raw powder and preparation method thereof
CN104069242A (en) * 2013-07-09 2014-10-01 山东东阿阿胶股份有限公司 Nano composition of compound e-jiao slurry and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114306372A (en) * 2021-12-07 2022-04-12 兰州大学 Polysaccharide extract of traditional Chinese medicine composition and preparation method and application thereof
CN114306372B (en) * 2021-12-07 2023-10-31 兰州大学 Polysaccharide extract of traditional Chinese medicine composition and preparation method and application thereof

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