CN104383261A - Health capsule as well as preparation method and identification method thereof - Google Patents

Health capsule as well as preparation method and identification method thereof Download PDF

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CN104383261A
CN104383261A CN201410584001.5A CN201410584001A CN104383261A CN 104383261 A CN104383261 A CN 104383261A CN 201410584001 A CN201410584001 A CN 201410584001A CN 104383261 A CN104383261 A CN 104383261A
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health
capsule
polygoni multiflori
radix polygoni
filtrate
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CN104383261B (en
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张芝庭
张涛涛
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GUIZHOU SHENQI PHARMACEUTICAL CO Ltd
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GUIZHOU SHENQI PHARMACEUTICAL CO Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/70Polygonaceae (Buckwheat family), e.g. spineflower or dock
    • A61K36/704Polygonum, e.g. knotweed
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/63Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
    • A61K36/638Ligustrum, e.g. Chinese privet
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8969Polygonatum (Solomon's seal)
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4841Filling excipients; Inactive ingredients
    • A61K9/4866Organic macromolecular compounds
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography
    • 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • 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
    • A61K2236/331Extraction 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
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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
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    • AHUMAN NECESSITIES
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    • 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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Abstract

The invention relates to the technical field of health capsules, and in particular relates to a health capsule as well as a preparation method and an identification method thereof. According to the invention, through an appropriate ratio of the raw materials such as polygonum multiflorum, rhizoma polygonati, glossy privet fruits and yerbadetajo herbs combined with process steps such as raw material treatment, filtrate mixing and powder addition, nutritional ingredients in raw materials are sufficiently maintained, the nutritional efficacies of the prepared health capsule are improved, the quality of the health capsule is improved, and the soothing of the health capsule on the diseases such as insomnia and dreaminess, tinnitus and amnesia, epilation and premature graying of hair is enhanced, and thus the efficacies of tonifying liver and kidney and benefiting life essence and nourishing blood are achieved. Through the specific identification method provided for the health capsule prepared by the technical scheme provided by the invention, the quality of the health capsule is further ensured.

Description

A kind of health-caring capsule and preparation method thereof and discrimination method
Technical field
The present invention relates to health-caring capsule technical field, especially a kind of health-caring capsule and preparation method thereof and discrimination method.
Background technology
Health preserving is the quality of life that modern people pursue, and in order to health preserving, in the prior art, has occurred a large amount of health care medicines, health care soup, health-care tea, and mostly for be hyperglycemia, hypertension, diabetes, myocardial vascular disease, deficiency of the kidney, suffer from a deficiency of the kidney, nephritis, constipation and other diseases, the technical scheme wherein adopted carries out the Chinese medicine of medicine-food two-purpose or food materials to combine and arrange in pairs or groups nothing but exactly, and is prepared by certain technique, as by Radix Polygoni Multiflori Preparata, Rhizoma Polygonati system, Fructus Ligustri Lucidi system, Herba Ecliptae and other Chinese crude drugs or food materials carry out combination collocation, are obtainedly suitable for diabetes, hypertension, hyperglycemia, the pill that myocardial vascular disease or nephrotic eat, powder, unguentum, decoction, also has Rhizoma amorphophalli simultaneously, Lepidinm meyenii Walp, Semen Tritici aestivi, Semen Maydis, the Chinese crude drug of the food materials that other consumptions such as Oryza glutinosa are stronger and other medicine-food two-purposes combines, and is mixed with cake, the food of paste and so on, for the use of body-care health preserving, but the more healthy nutritional labeling in raw material is retained for how, and the technical literature that the nutritive value of the nutritional labeling in raw material is further enhanced have not been reported, and by Radix Polygoni Multiflori Preparata, Rhizoma Polygonati system, Fructus Ligustri Lucidi system, the report that Herba Ecliptae is prepared into health-caring capsule also yet there are no.
For this reason, this researcher by long-term research and discussion, and is started with from above-mentioned technical problem, Radix Polygoni Multiflori Preparata, Rhizoma Polygonati system, Fructus Ligustri Lucidi system, Herba Ecliptae is made the raw material in field as health-caring capsule, for the making field of health-caring capsule provides a kind of new approaches.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides a kind of health-caring capsule, it has effect of invigorating the liver and kidney, benefiting essence-blood, strenghthening bone, to insomnia and dreamful sleep, tinnitus is forgetful, the disease such as alopecia, early whitening of beard and hair has remarkable therapeutic effect feature.
The present invention also provides a kind of preparation method of health-caring capsule; there is the nutrient in protection raw medicinal material; guarantee that effect of health-caring capsule is better; various nutrient elements can be supplemented for human body; and then relieving insomnia dreaminess, tinnitus are forgetful, the disease such as alopecia, early whitening of beard and hair, and then reach effect of health care.
Be achieved particular by following technical scheme:
A kind of health-caring capsule, its raw material composition is (with parts by weight) Radix Polygoni Multiflori 450-550 part, Rhizoma Polygonati 450-550 part, Fructus Ligustri Lucidi 200-300 part, Herba Ecliptae 200-300 part.
Described raw material composition is (with parts by weight) Radix Polygoni Multiflori 480-520 part, Rhizoma Polygonati 480-520 part, Fructus Ligustri Lucidi 220-280 part, Herba Ecliptae 220-280 part.
Described raw material composition is (with parts by weight) Radix Polygoni Multiflori 500 parts, Rhizoma Polygonati 500 parts, Fructus Ligustri Lucidi 250 parts, Herba Ecliptae 250 parts.
The preparation method of this health-caring capsule, comprises the following steps:
(1) Feedstock treating: the raw material getting above-mentioned raw materials part is stand-by, Radix Polygoni Multiflori is divided into five parts, get two parts of Radix Polygoni Multiflori, be placed in dehydrator, adopt programming rate to be that 3 DEG C/min is warming up to 70 DEG C from 20 DEG C of intensifications, carried out constant temperature process, drying out Radix Polygoni Multiflori moisture is 2-3%, again the Radix Polygoni Multiflori of oven dry is placed in pulverizer and is ground into 120-140 object powder, stand-by, Fructus Ligustri Lucidi is placed in steamer, Fructus Ligustri Lucidi is adopted wine steam carry out temperature be 80-90 DEG C steam 20-40min after, take out Fructus Ligustri Lucidi, again by itself and Rhizoma Polygonati, after Herba Ecliptae and remaining three parts of Radix Polygoni Multiflori mix homogeneously, obtain mixed material, be 1:(3-5 by mixed material and water according to weight ratio again) prepare, and be placed in boiler, after leaving standstill 10-12min, be that 11 DEG C/min is warming up to 110-130 DEG C by boiler according to programming rate again, after constant temperature decocts 3-5min, programming rate is adopted to be that 5 DEG C/min is warming up to 150-170 DEG C again, constant temperature decocts 7-10min, cooling rate is adopted to be that 20 DEG C/min is cooled to 80 DEG C again, constant temperature decocts 20-25min, cooling rate is adopted to be that 15 DEG C/min is cooled to 30 DEG C again, again by its filtration treatment, obtain filtrate a and filtering residue a, again filtering residue is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate b and filtering residue b, again filtering residue a is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate c and filtering residue c, stand-by,
(2) filtrate mixing: by step 1) obtained filtrate a, filtrate b, filtrate c mixes, and to be placed on temperature be in the environment of 70-90 DEG C, be concentrated into the clear paste that relative density is 1.10 ~ 1.15, add ethanol wherein again, the alcohol content (mass percentage) in concentrated solution is made to be 60%, and adopt mixing speed to be 60-70r/min stir process 20-30min, left standstill process >24h again, take out supernatant, again subnatant is concentrated into 1/5th, obtain thick paste, be placed in natural environment again and be cooled to room temperature, stand-by,
(3) powder is added: by step 1) the Radix Polygoni Multiflori powder that obtains adds step 2) in the thick paste that obtains, and adopt mixing speed to be 40-50r/min stir process 20-40min, be placed on again in dehydrator, temperature is adopted to be after 30-40 DEG C of oven dry is 2-5% to moisture, be placed on again in pulverizer and be crushed to 130-140 order, add micropowder silica gel wherein again, magnesium stearate and starch, wherein micropowder silica gel is the powder of 100-300nm, its addition is the 1-2% of raw material gross weight, the addition of magnesium stearate is the 0.5-0.9% of gross weight, starch accounts for the 5-9% of micropowder silica gel and magnesium stearate gross weight, and after being stirred, during it is incapsulated according to 0.45g/ grain, health-caring capsule can be obtained.
The capsule body of described capsule contains the Testa oryzae oil that mass fraction is 7-9%.
The discrimination method of this health-caring capsule, comprises the following steps:
(1) test sample preparation: go bail for strong capsule 's content 0.2g, adds ethanol 25ml, is heated to 80 DEG C of backflows 1 hour, filter, filtrate recycling design is to dry, and the residue 10ml that adds water makes dissolving, by D101 type macroporous adsorptive resins, its column internal diameter 1.2cm, post height 15cm, with water 100ml eluting, discard eluent, then use methanol 50ml eluting, collect eluent, recycling design is to dry, and residue adds methanol 2ml makes dissolving, as need testing solution, stand-by;
(2) reference substance preparation: get Radix Polygoni Multiflori 0.2g, add ethanol 25ml, the method with step 1 makes control medicinal material solution, obtains reference substance solution, stand-by;
(3) differentiate: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform and methanol according to mass ratio for after 7:3 mixing for developing solvent, open up to 3-4cm, take out, dry, then with chloroform and methanol according to mass ratio for after 20:1 mixing for developing solvent, open up to 7-8cm, take out, dry, be placed in daylight respectively and wavelength is inspect under the ultraviolet light of 365nm, the discriminating of health-caring capsule can be completed.
Identification result is: in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, and the speckle of aobvious same color under daylight, the fluorescence speckle of aobvious same color under ultraviolet light.
To be that binding agent is bonding with sodium carboxymethyl cellulose form described silica gel g thin-layer plate.
The present invention also provides the discrimination method of another health-caring capsule, comprises the following steps:
(1) get health-caring capsule 1g, add the ethanol 4ml that concentration is 70% wherein, then to be placed on temperature be in the water-bath of 80 DEG C, carry out water-bath reflow treatment 1h, filter, obtain filtrate, by filtrate concentrated 1ml at 60 DEG C, obtained need testing solution, stand-by;
(2) get 1g Rhizoma Polygonati, be mixed with reference substance solution according to the operational approach of step 1, stand-by;
(3) need testing solution and reference substance solution 10ul is drawn respectively, and it is put respectively the diverse location on the same level line of same silica gel H lamellae, and with n-butyl alcohol, glacial acetic acid and water are that the mixed liquor of 4:1:1 proportioning is as developing solvent according to mass ratio, and silica gel H lamellae is placed in developing solvent, need testing solution and reference substance solution is made to launch to process 20min on silica gel H lamellae, and then take out, dry under normal temperature environment, sprayed the ethanol solution of ninhydrin that percetage by weight is 2% again, being placed on temperature is again in the environment of 105 DEG C, baking 1-9min, observe the hydrochloric acid situation of change on silica gel H lamellae, the discriminating of health-caring capsule can be completed.
Moreover the present invention also provides the discrimination method of following several health-caring capsule:
1, get this product content 2.7g, add 70% ethanol 30ml, reflux 1 hour, filters while hot, filtrate water bath method, residue acetone 20ml, and water-bath slight fever makes dissolving, and filter, filtrate water-bath is concentrated into about 1ml, as need testing solution.Separately get P. kingianum (system) control medicinal material 3g, the 50ml reflux, extract, that adds water 1 hour, filter, filtrate water-bath is concentrated into about 10ml, lets cool, add ethanol and regulate ethanol content to 60%, centrifugal filtering (3500 revs/min, 5 minutes), supernatant water bath method, residue adds acetone 20ml same treatment, in contrast medical material solution.Test according to thin layer chromatography (annex VI B), draw each 5 ~ 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-formic acid (2:4:0.5) for developing solvent, launch, take out, dry, spray with 2,4 dinitrophenyl hydrazine ethanol test solution, dry, inspect in the sunlight.In test sample chromatograph, with on control medicinal material chromatograph relevant position, show the speckle of same color.
2, get this product content 2.5g, put in conical flask, add Diluted Alcohol 25ml, supersound process (power 250W, frequency 60kHz) 30 minutes, lets cool, shakes up, and filter, subsequent filtrate is as need testing solution.Separately get specnuezhenside reference substance appropriate, accurately weighed, add methanol and make the solution of every 1ml containing 0.1mg, product solution in contrast.According to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VID) test, take octadecylsilane chemically bonded silica as filler; With methanol-water (40: 60) for mobile phase; Determined wavelength is 224nm.Number of theoretical plate calculates should be not less than 3000 by specnuezhenside peak.Accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography.The chromatographic peak identical with retention time in reference substance chromatograph should be presented in need testing solution chromatograph.
3, get this product content 5.4g, add 70% methanol 25ml, supersound process 45 minutes, filter, filtrate is concentrated into about 8ml, and add water 15ml, stir evenly, filter, filtrate extracts 3 times with petroleum ether (60-90 DEG C) jolting, each 20ml, merge petroleum ether liquid, recycling design is to dry, and residue adds methanol 0.5ml makes dissolving, as need testing solution.Separately get Herba Ecliptae control medicinal material 0.5g, add water 50ml, heats micro-boiling 1 hour, let cool, and filter, filtrate is concentrated into about 30ml, from " extracting 3 times with petroleum ether (60-90 DEG C) jolting ", is made in the same way of control medicinal material solution.Test according to thin layer chromatography (annex VI B), draw need testing solution 5 ~ 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with the upper solution of petroleum ether (30-60 DEG C)-Ethyl formate-formic acid (20:5:1) for developing solvent, launch, take out, dry, inspect under ultraviolet light (365nm), in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious same color.
Compared with prior art, technique effect of the present invention is embodied in:
1. by the appropriate proportioning of Radix Polygoni Multiflori, Rhizoma Polygonati, Fructus Ligustri Lucidi, each raw material of Herba Ecliptae, and mix, add the combination of the processing steps such as powder by Feedstock treating, filtrate, and then the nutritional labeling in raw material is retained fully, improve the nutritive effect of the health-caring capsule made, improve the quality of health-caring capsule, strengthen the remission such as health-caring capsule is forgetful to insomnia and dreamful sleep, tinnitus, alopecia, early whitening of beard and hair, and then reach effect of invigorating the liver and kidney, benefiting essence-blood.
2. the health-caring capsule by preparing technical scheme of the present invention provides one discrimination method targetedly, and then the quality of health-caring capsule is further ensured.
3. by preparation method, accurately appropriate control is carried out to the technological parameter in processing step, especially to the control decocting temperature, ensure that, between the nutritional labeling in raw material, biochemical reaction directed accurately occurs, further enrich the trophic structure in health-caring capsule, reduce the Harmful ingredient content in raw material, and then prepare and have no side effect, and can immunity in reinforcement, reduce blood glucose, the health-caring capsule of improvement function.
Detailed description of the invention
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
A kind of health-caring capsule, its raw material is Radix Polygoni Multiflori 450kg, Rhizoma Polygonati 450kg, Fructus Ligustri Lucidi 200kg, Herba Ecliptae 200kg.
The preparation method of this health-caring capsule, comprises the following steps:
(1) Feedstock treating: the raw material getting above-mentioned raw materials part is stand-by, Radix Polygoni Multiflori is divided into five parts, get two parts of Radix Polygoni Multiflori, be placed in dehydrator, adopt programming rate to be that 3 DEG C/min is warming up to 70 DEG C from 20 DEG C of intensifications, carried out constant temperature process, drying out Radix Polygoni Multiflori moisture is 2%, again the Radix Polygoni Multiflori of oven dry is placed in pulverizer and is ground into 120 object powder, stand-by, Fructus Ligustri Lucidi is placed in steamer, Fructus Ligustri Lucidi is adopted wine steam carry out temperature be 80 DEG C steam 20min after, take out Fructus Ligustri Lucidi, again by itself and Rhizoma Polygonati, after Herba Ecliptae and remaining three parts of Radix Polygoni Multiflori mix homogeneously, obtain mixed material, be that 1:3 prepares by mixed material and water according to weight ratio again, and be placed in boiler, after leaving standstill 10min, be that 11 DEG C/min is warming up to 110 DEG C by boiler according to programming rate again, after constant temperature decocts 3min, programming rate is adopted to be that 5 DEG C/min is warming up to 150 DEG C again, constant temperature decocts 7min, cooling rate is adopted to be that 20 DEG C/min is cooled to 80 DEG C again, constant temperature decocts 20min, cooling rate is adopted to be that 15 DEG C/min is cooled to 30 DEG C again, again by its filtration treatment, obtain filtrate a and filtering residue a, again filtering residue is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate b and filtering residue b, again filtering residue a is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate c and filtering residue c, stand-by,
(2) filtrate mixing: by step 1) obtained filtrate a, filtrate b, filtrate c mix, and to be placed on temperature be in the environment of 70 DEG C, be concentrated into the clear paste that relative density is 1.10, add ethanol wherein again, the alcohol content (mass percentage) in concentrated solution is made to be 60%, and adopt mixing speed to be 60r/min stir process 20min, left standstill process >24h again, take out supernatant, again subnatant is concentrated into 1/5th, obtain thick paste, then be placed in natural environment and be cooled to room temperature, stand-by;
(3) powder is added: by step 1) the Radix Polygoni Multiflori powder that obtains adds step 2) in the thick paste that obtains, and adopt mixing speed to be 40r/min stir process 20min, be placed on again in dehydrator, adopt temperature be 30 DEG C dry to moistures be after 2%, be placed on again in pulverizer and be crushed to 130 orders, add micropowder silica gel wherein again, magnesium stearate and starch, wherein micropowder silica gel is the powder of 100nm, its addition is 1% of raw material gross weight, the addition of magnesium stearate is 0.5% of gross weight, starch accounts for 5% of micropowder silica gel and magnesium stearate gross weight, and after being stirred, during it is incapsulated according to 0.45g/ grain, health-caring capsule can be obtained.
The capsule body of described capsule contains the Testa oryzae oil that mass fraction is 7%.
The discrimination method of this health-caring capsule, comprises the following steps:
(1) test sample preparation: go bail for strong capsule 's content 0.2g, adds ethanol 25ml, is heated to 80 DEG C of backflows 1 hour, filter, filtrate recycling design is to dry, and the residue 10ml that adds water makes dissolving, by D101 type macroporous adsorptive resins, its column internal diameter 1.2cm, post height 15cm, with water 100ml eluting, discard eluent, then use methanol 50ml eluting, collect eluent, recycling design is to dry, and residue adds methanol 2ml makes dissolving, as need testing solution, stand-by;
(2) reference substance preparation: get Radix Polygoni Multiflori 0.2g, add ethanol 25ml, the method with step 1 makes control medicinal material solution, obtains reference substance solution, stand-by;
(3) differentiate: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform and methanol according to mass ratio for after 7:3 mixing for developing solvent, open up to 3.5m, take out, dry, then with chloroform and methanol according to mass ratio for after 20:1 mixing for developing solvent, open up to 7.5cm, take out, dry, be placed in daylight respectively and wavelength is inspect under the ultraviolet light of 365nm, the discriminating of health-caring capsule can be completed.
To be that binding agent is bonding with sodium carboxymethyl cellulose form described silica gel g thin-layer plate.
Embodiment 2
On the basis of embodiment 1, other steps are with embodiment 1, and a kind of health-caring capsule, its raw material composition is Radix Polygoni Multiflori 480kg, Rhizoma Polygonati 480kg, Fructus Ligustri Lucidi 220kg, Herba Ecliptae 220kg.
The preparation method of this health-caring capsule, comprises the following steps:
(1) Feedstock treating: the raw material getting above-mentioned raw materials part is stand-by, Radix Polygoni Multiflori is divided into five parts, get two parts of Radix Polygoni Multiflori, be placed in dehydrator, adopt programming rate to be that 3 DEG C/min is warming up to 70 DEG C from 20 DEG C of intensifications, carried out constant temperature process, drying out Radix Polygoni Multiflori moisture is 3%, again the Radix Polygoni Multiflori of oven dry is placed in pulverizer and is ground into 140 object powder, stand-by, Fructus Ligustri Lucidi is placed in steamer, Fructus Ligustri Lucidi is adopted wine steam carry out temperature be 90 DEG C steam 40min after, take out Fructus Ligustri Lucidi, again by itself and Rhizoma Polygonati, after Herba Ecliptae and remaining three parts of Radix Polygoni Multiflori mix homogeneously, obtain mixed material, be that 1:5 prepares by mixed material and water according to weight ratio again, and be placed in boiler, after leaving standstill 12min, be that 11 DEG C/min is warming up to 130 DEG C by boiler according to programming rate again, after constant temperature decocts 5min, programming rate is adopted to be that 5 DEG C/min is warming up to 170 DEG C again, constant temperature decocts 10min, cooling rate is adopted to be that 20 DEG C/min is cooled to 80 DEG C again, constant temperature decocts 25min, cooling rate is adopted to be that 15 DEG C/min is cooled to 30 DEG C again, again by its filtration treatment, obtain filtrate a and filtering residue a, again filtering residue is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate b and filtering residue b, again filtering residue a is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate c and filtering residue c, stand-by,
(2) filtrate mixing: by step 1) obtained filtrate a, filtrate b, filtrate c mix, and to be placed on temperature be in the environment of 90 DEG C, be concentrated into the clear paste that relative density is 1.15, add ethanol wherein again, the alcohol content (mass percentage) in concentrated solution is made to be 60%, and adopt mixing speed to be 70r/min stir process 30min, left standstill process >24h again, take out supernatant, again subnatant is concentrated into 1/5th, obtain thick paste, then be placed in natural environment and be cooled to room temperature, stand-by;
(3) powder is added: by step 1) the Radix Polygoni Multiflori powder that obtains adds step 2) in the thick paste that obtains, and adopt mixing speed to be 50r/min stir process 40min, be placed on again in dehydrator, adopt temperature be 40 DEG C dry to moistures be after 5%, be placed on again in pulverizer and be crushed to 140 orders, add micropowder silica gel wherein again, magnesium stearate and starch, wherein micropowder silica gel is the powder of 300nm, its addition is 2% of raw material gross weight, the addition of magnesium stearate is 0.9% of gross weight, starch accounts for 9% of micropowder silica gel and magnesium stearate gross weight, and after being stirred, during it is incapsulated according to 0.45g/ grain, health-caring capsule can be obtained.
The capsule body of described capsule contains the Testa oryzae oil that mass fraction is 9%.
Embodiment 3
On the basis of embodiment 1, other are set forth with embodiment 1, and a kind of health-caring capsule, its raw material composition is Radix Polygoni Multiflori 500kg, Rhizoma Polygonati 500kg, Fructus Ligustri Lucidi 250kg, Herba Ecliptae 250kg.
The preparation method of this health-caring capsule, comprises the following steps:
(1) Feedstock treating: the raw material getting above-mentioned raw materials part is stand-by, Radix Polygoni Multiflori is divided into five parts, get two parts of Radix Polygoni Multiflori, be placed in dehydrator, adopt programming rate to be that 3 DEG C/min is warming up to 70 DEG C from 20 DEG C of intensifications, carried out constant temperature process, drying out Radix Polygoni Multiflori moisture is 2.5%, again the Radix Polygoni Multiflori of oven dry is placed in pulverizer and is ground into 130 object powder, stand-by, Fructus Ligustri Lucidi is placed in steamer, Fructus Ligustri Lucidi is adopted wine steam carry out temperature be 85 DEG C steam 30min after, take out Fructus Ligustri Lucidi, again by itself and Rhizoma Polygonati, after Herba Ecliptae and remaining three parts of Radix Polygoni Multiflori mix homogeneously, obtain mixed material, be that 1:4 prepares by mixed material and water according to weight ratio again, and be placed in boiler, after leaving standstill 11min, be that 11 DEG C/min is warming up to 120 DEG C by boiler according to programming rate again, after constant temperature decocts 4min, programming rate is adopted to be that 5 DEG C/min is warming up to 160 DEG C again, constant temperature decocts 9min, cooling rate is adopted to be that 20 DEG C/min is cooled to 80 DEG C again, constant temperature decocts 23min, cooling rate is adopted to be that 15 DEG C/min is cooled to 30 DEG C again, again by its filtration treatment, obtain filtrate a and filtering residue a, again filtering residue is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate b and filtering residue b, again filtering residue a is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate c and filtering residue c, stand-by,
(2) filtrate mixing: by step 1) obtained filtrate a, filtrate b, filtrate c mix, and to be placed on temperature be in the environment of 80 DEG C, be concentrated into the clear paste that relative density is 1.13, add ethanol wherein again, the alcohol content (mass percentage) in concentrated solution is made to be 60%, and adopt mixing speed to be 65r/min stir process 25min, left standstill process >24h again, take out supernatant, again subnatant is concentrated into 1/5th, obtain thick paste, then be placed in natural environment and be cooled to room temperature, stand-by;
(3) powder is added: by step 1) the Radix Polygoni Multiflori powder that obtains adds step 2) in the thick paste that obtains, and adopt mixing speed to be 45r/min stir process 30min, be placed on again in dehydrator, adopt temperature be 35 DEG C dry to moistures be after 3%, be placed on again in pulverizer and be crushed to 135 orders, add micropowder silica gel wherein again, magnesium stearate and starch, wherein micropowder silica gel is the powder of 200nm, its addition is 1.5% of raw material gross weight, the addition of magnesium stearate is 0.8% of gross weight, starch accounts for 7% of micropowder silica gel and magnesium stearate gross weight, and after being stirred, during it is incapsulated according to 0.45g/ grain, health-caring capsule can be obtained.
The capsule body of described capsule contains the Testa oryzae oil that mass fraction is 8%.
The discrimination method of this health-caring capsule, comprises the following steps:
(1) get health-caring capsule 1g, add the ethanol 4ml that concentration is 70% wherein, then to be placed on temperature be in the water-bath of 80 DEG C, carry out water-bath reflow treatment 1h, filter, obtain filtrate, by filtrate concentrated 1ml at 60 DEG C, obtained need testing solution, stand-by;
(2) get 1g Rhizoma Polygonati, be mixed with reference substance solution according to the operational approach of step 1, stand-by;
(3) need testing solution and reference substance solution 10ul is drawn respectively, and it is put respectively the diverse location on the same level line of same silica gel H lamellae, and with n-butyl alcohol, glacial acetic acid and water are that the mixed liquor of 4:1:1 proportioning is as developing solvent according to mass ratio, and silica gel H lamellae is placed in developing solvent, need testing solution and reference substance solution is made to launch to process 20min on silica gel H lamellae, and then take out, dry under normal temperature environment, sprayed the ethanol solution of ninhydrin that percetage by weight is 2% again, being placed on temperature is again in the environment of 105 DEG C, baking 1-9min, observe the hydrochloric acid situation of change on silica gel H lamellae, the discriminating of health-caring capsule can be completed.
Embodiment 4
On the basis of embodiment 1, other are all with embodiment 1, a kind of health-caring capsule, and its raw material is Radix Polygoni Multiflori 550g, Rhizoma Polygonati 550g, Fructus Ligustri Lucidi 300g, Herba Ecliptae 300g.Make 1200.
Its discrimination method is, gets this product content 2.5g, puts in conical flask, add Diluted Alcohol 25ml, and supersound process (power 250W, frequency 60kHz) 30 minutes, lets cool, shake up, and filter, subsequent filtrate is as need testing solution.Separately get specnuezhenside reference substance appropriate, accurately weighed, add methanol and make the solution of every 1ml containing 0.1mg, product solution in contrast.According to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VID) test, take octadecylsilane chemically bonded silica as filler; With methanol-water (40: 60) for mobile phase; Determined wavelength is 224nm.Number of theoretical plate calculates should be not less than 3000 by specnuezhenside peak.Accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography.The chromatographic peak identical with retention time in reference substance chromatograph should be presented in need testing solution chromatograph.
This product every contains Radix Polygoni Multiflori Preparata with 2,3,5,4 '-tetrahydroxystilbene-2-O-β-D-Glucose glycosides (C 20h 22o 9) meter, must not>=2.5mg.
Embodiment 5
On the basis of embodiment 1, other are all with embodiment 1, a kind of health-caring capsule, and its raw material composition is Radix Polygoni Multiflori 520g, Rhizoma Polygonati 520g, Fructus Ligustri Lucidi 280g, Herba Ecliptae 280g.Make 1000.
The present invention has: invigorating the liver and kidney, benefiting essence-blood, strengthening bone and muscle.Cure mainly: insomnia and dreamful sleep, tinnitus is forgetful, the disease such as alopecia and early whitening of beard and hair.
Usage and dosage is: two courses for the treatment of Monday, three times on the one, one time six.
Test example:
The secondary experiment of test example 1 poison
Get mice 40, be divided into two groups, label is A, B, often organizes 20; A group adopts the embodiment of the present invention 2 to obtain health-caring capsule 100 pulverizing+conventional feed 2kg and feeds; Normal saline+conventional feed 2kg mixing of the weight such as the employing of B group and health-caring capsule is fed; After feeding 3 days, observe the physiological change situation of mice, mice is without difference, and average activity time every day of A group mice is more normal than the feces of the excretion of B long 3-4h, A group mice, and B group stool in mice is dry; Continue to feed to 100 days, and continue to observe the physiological change situation of mice and the body weight change situation of mice, A group mice was weighed at the 100th day, the average 1.12kg that often only increases weight; B group mice was weighed at the 100th day, the average 0.73kg that often only increases weight.
Have in above-mentioned experimentation and can find out, health-caring capsule of the present invention has no side effect, and obviously can improve intestinal, strengthens digestion, promotes mice develop and weightening finish.
Test example 2 immunity is tested
Get the test example 1A group feeding mice of 100 days, and from ear's blood-letting of mice after the 100th day feeding 30min, measure the sugar content in blood, and observe the cytophagous content in blood; Get the test example B group feeding mice of 100 days simultaneously, and from ear's blood-letting of mice after the 100th day feeding 30min, measure the sugar content in blood, and observe the cytophagous content in blood; And the sugar content in the mouse blood of A group and B group and cytophagous accounting are analyzed, the sugar content in A group mouse blood has 17 to maintain lower level, have 3 higher a little; Sugar content in B group mouse blood has 6 to maintain lower level, have 14 higher a little; And the phagocyte accounting in A group mouse blood is than the cytophagous accounting height 4-8 percentage point in B group mouse blood.
This shows, health-caring capsule of the present invention significantly can reduce the sugar content of blood, and then reduces blood glucose, also can enhancing immunity.
It is important to point out at this; above embodiment and test example are only limitted to further set forth the present invention and understand; be not restriction, the essential characteristics of the non-protruding that those skilled in the art make on this basis and the improvement of non-significant progress, all belong to protection category of the present invention.

Claims (7)

1. a health-caring capsule, is characterized in that, its raw material composition is (with parts by weight) Radix Polygoni Multiflori 450-550 part, Rhizoma Polygonati 450-550 part, Fructus Ligustri Lucidi 200-300 part, Herba Ecliptae 200-300 part.
2. health-caring capsule as claimed in claim 1, it is characterized in that, described raw material composition is (with parts by weight) Radix Polygoni Multiflori 480-520 part, Rhizoma Polygonati 480-520 part, Fructus Ligustri Lucidi 220-280 part, Herba Ecliptae 220-280 part.
3. health-caring capsule as claimed in claim 1, it is characterized in that, described raw material composition is (with parts by weight) Radix Polygoni Multiflori 500 parts, Rhizoma Polygonati 500 parts, Fructus Ligustri Lucidi 250 parts, Herba Ecliptae 250 parts.
4. the preparation method of the health-caring capsule as described in any one of claim 1-3, is characterized in that, comprises the following steps:
(1) Feedstock treating: the raw material getting above-mentioned raw materials part is stand-by, Radix Polygoni Multiflori is divided into five parts, get two parts of Radix Polygoni Multiflori, be placed in dehydrator, adopt programming rate to be that 3 DEG C/min is warming up to 70 DEG C from 20 DEG C of intensifications, carried out constant temperature process, drying out Radix Polygoni Multiflori moisture is 2-3%, again the Radix Polygoni Multiflori of oven dry is placed in pulverizer and is ground into 120-140 object powder, stand-by, Fructus Ligustri Lucidi is placed in steamer, Fructus Ligustri Lucidi is adopted wine steam carry out temperature be 80-90 DEG C steam 20-40min after, take out Fructus Ligustri Lucidi, again by itself and Rhizoma Polygonati, after Herba Ecliptae and remaining three parts of Radix Polygoni Multiflori mix homogeneously, obtain mixed material, be 1:(3-5 by mixed material and water according to weight ratio again) prepare, and be placed in boiler, after leaving standstill 10-12min, be that 11 DEG C/min is warming up to 110-130 DEG C by boiler according to programming rate again, after constant temperature decocts 3-5min, programming rate is adopted to be that 5 DEG C/min is warming up to 150-170 DEG C again, constant temperature decocts 7-10min, cooling rate is adopted to be that 20 DEG C/min is cooled to 80 DEG C again, constant temperature decocts 20-25min, cooling rate is adopted to be that 15 DEG C/min is cooled to 30 DEG C again, again by its filtration treatment, obtain filtrate a and filtering residue a, again filtering residue is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate b and filtering residue b, again filtering residue a is placed in boiler, adds the clear water of 3 times of weight, repeat above-mentioned decoction step, refilter, obtain filtrate c and filtering residue c, stand-by,
(2) filtrate mixing: by step 1) obtained filtrate a, filtrate b, filtrate c mixes, and to be placed on temperature be in the environment of 70-90 DEG C, be concentrated into the clear paste that relative density is 1.10 ~ 1.15, add ethanol wherein again, the alcohol content (mass percentage) in concentrated solution is made to be 60%, and adopt mixing speed to be 60-70r/min stir process 20-30min, left standstill process >24h again, take out supernatant, again subnatant is concentrated into 1/5th, obtain thick paste, be placed in natural environment again and be cooled to room temperature, stand-by,
(3) powder is added: by step 1) the Radix Polygoni Multiflori powder that obtains adds step 2) in the thick paste that obtains, and adopt mixing speed to be 40-50r/min stir process 20-40min, be placed on again in dehydrator, temperature is adopted to be after 30-40 DEG C of oven dry is 2-5% to moisture, be placed on again in pulverizer and be crushed to 130-140 order, add micropowder silica gel wherein again, magnesium stearate and starch, wherein micropowder silica gel is the powder of 100-300nm, its addition is the 1-2% of raw material gross weight, the addition of magnesium stearate is the 0.5-0.9% of gross weight, starch accounts for the 5-9% of micropowder silica gel and magnesium stearate gross weight, and after being stirred, during it is incapsulated according to 0.45g/ grain, health-caring capsule can be obtained.
5. the preparation method of health-caring capsule as claimed in claim 4, it is characterized in that, the capsule body of described capsule contains the Testa oryzae oil that mass fraction is 7-9%.
6. the discrimination method of the health-caring capsule that the preparation method of the health-caring capsule as described in any one of claim 1-3 and the health-caring capsule as described in any one of claim 4-5 obtains, is characterized in that, comprise the following steps:
(1) test sample preparation: go bail for strong capsule 's content 0.2g, adds ethanol 25ml, is heated to 80 DEG C of backflows 1 hour, filter, filtrate recycling design is to dry, and the residue 10ml that adds water makes dissolving, by D101 type macroporous adsorptive resins, its column internal diameter 1.2cm, post height 15cm, with water 100ml eluting, discard eluent, then use methanol 50ml eluting, collect eluent, recycling design is to dry, and residue adds methanol 2ml makes dissolving, as need testing solution, stand-by;
(2) reference substance preparation: get Radix Polygoni Multiflori 0.2g, add ethanol 25ml, the method with step 1 makes control medicinal material solution, obtains reference substance solution, stand-by;
(3) differentiate: draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform and methanol according to mass ratio for after 7:3 mixing for developing solvent, open up to 3-4cm, take out, dry, then with chloroform and methanol according to mass ratio for after 20:1 mixing for developing solvent, open up to 7-8cm, take out, dry, be placed in daylight respectively and wavelength is inspect under the ultraviolet light of 365nm, the discriminating of health-caring capsule can be completed.
7. the discrimination method of health-caring capsule as claimed in claim 6, is characterized in that, to be that binding agent is bonding with sodium carboxymethyl cellulose form described silica gel g thin-layer plate.
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CN105748829A (en) * 2016-04-18 2016-07-13 宝应县中医医院 Healthcare capsule and production process thereof
CN105853652A (en) * 2016-03-29 2016-08-17 李庆河 Yitang bong reinforcing health capsule and preparation method thereof
CN107693715A (en) * 2017-11-09 2018-02-16 璧电健 A kind of composition of hair growth
CN107744572A (en) * 2017-11-09 2018-03-02 璧电健 A kind of preparation method of the composition of hair growth

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CN103235082A (en) * 2013-04-27 2013-08-07 贵州盛世龙方制药股份有限公司 Method for detecting Jingwu capsule
CN103977352A (en) * 2014-05-26 2014-08-13 徐殿红 Traditional Chinese medicine composition for treating cancers and preparation method thereof

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CN1840087A (en) * 2006-02-06 2006-10-04 贵州神奇集团控股有限公司 King solomonseal- and fleece-flower root-containing Chinese medicinal formulation for treating chronic fatigue syndrome and its preparation method
CN103235082A (en) * 2013-04-27 2013-08-07 贵州盛世龙方制药股份有限公司 Method for detecting Jingwu capsule
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CN105853652A (en) * 2016-03-29 2016-08-17 李庆河 Yitang bong reinforcing health capsule and preparation method thereof
CN105748829A (en) * 2016-04-18 2016-07-13 宝应县中医医院 Healthcare capsule and production process thereof
CN107693715A (en) * 2017-11-09 2018-02-16 璧电健 A kind of composition of hair growth
CN107744572A (en) * 2017-11-09 2018-03-02 璧电健 A kind of preparation method of the composition of hair growth

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