CN106177345A - QIJU DIHUANG WAN and preparation method thereof - Google Patents

QIJU DIHUANG WAN and preparation method thereof Download PDF

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CN106177345A
CN106177345A CN201610803215.6A CN201610803215A CN106177345A CN 106177345 A CN106177345 A CN 106177345A CN 201610803215 A CN201610803215 A CN 201610803215A CN 106177345 A CN106177345 A CN 106177345A
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parts
dihuang wan
extraction
qiju dihuang
preparation
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刘世超
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Shanghai Chen Song New Mstar Technology Ltd
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Shanghai Chen Song New Mstar Technology Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/06—Fungi, e.g. yeasts
    • A61K36/07—Basidiomycota, e.g. Cryptococcus
    • A61K36/076—Poria
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/287—Chrysanthemum, e.g. daisy
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/40—Cornaceae (Dogwood family)
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A61K36/185—Magnoliopsida (dicotyledons)
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/80—Scrophulariaceae (Figwort family)
    • A61K36/804—Rehmannia
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
    • A61K36/815—Lycium (desert-thorn)
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    • A61K36/884—Alismataceae (Water-plantain family)
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    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/894—Dioscoreaceae (Yam family)
    • A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
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    • A61K9/2004—Excipients; Inactive ingredients
    • A61K9/2013—Organic compounds, e.g. phospholipids, fats
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    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction 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
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    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention discloses a kind of QIJU DIHUANG WAN and preparation method thereof, described QIJU DIHUANG WAN includes that the raw material of following weight parts is prepared from: Fructus Lycii 30 50 parts, Flos Chrysanthemi 30 50 parts, Radix Rehmanniae Preparata 140 180 parts, Fructus Corni (system) 60 100 parts, Cortex Moutan 40 80 parts, Rhizoma Dioscoreae 60 100 parts, 40 80 parts of Poria, Rhizoma Alismatis 40 80 parts.QIJU DIHUANG WAN of the present invention, has effect of nourishing the kidney and liver, can be used for treating hepatic and renal YIN deficiency, vertigo and tinnitus, photophobia photophobia, epiphora induced by wind, the disease such as blurring of vision.Its preparation process uses supercritical CO2Fluid extraction technology, it is possible to fully extract medical material oil-soluble and water miscible effective ingredient, improves the bioavailability of medical material, and the adjuvant of interpolation ensure that the steady quality of medicine.

Description

QIJU DIHUANG WAN and preparation method thereof
Technical field
The present invention relates to technical field of traditional Chinese medicine preparation, be specifically related to a kind of QIJU DIHUANG WAN and preparation method thereof.
Background technology
QIJU DIHUANG WAN comes from " doctor's level ", adds Fructus Lycii, Flos Chrysanthemi forms on the basis of classic prescriptions LIUWEI DIHUANG WAN, tool Having the effect of YIN nourishing, nourishing the liver, improving eyesight, for hepatic and renal YIN deficiency, photophobia photophobia, epiphora induced by wind, the disease such as blurring of vision is evident in efficacy, in Doctor's famous prescription of ophthalmology.LIUWEI DIHUANG WAN comes from key to Therapeutics of Children's Diseases, reuses Radix Rehmanniae Preparata, enriching yin and nourishing kidney, life essence-filling, marrow-benefitting in side； Fructus Corni takes a tonic or nourishing food to build up one's health Liver and kidney energy arresting seminal emission；Rhizoma Dioscoreae spleen reinforcing controlling nocturnal emission with astringent drugs, referred to as three mend.Rush down the muddy kidney that rushes down clearly fiery, and the taste of anti-Radix Rehmanniae Preparata is greasy；Fu Siberian cocklebur spleen invigorating eliminating dampness by diuresis, to help the strong fortune of Rhizoma Dioscoreae；Cortex Moutan lets out clearly liver-fire, and the temperature of FRUCTUS CORNI PREPARATA, and the three of meaning are rushed down.Six medicines share, invigorating middle warmer Having a gulf, residence rushes down in benefit, complements each other, and mends more than rushing down, and gathers the effect of nourishing the liver and kidney altogether.QIJU DIHUANG WAN adds Fructus Lycii on this basis Son, Flos Chrysanthemi.Flos Chrysanthemi acrid in the mouth, hardship, sweet, cold nature, return lung, Liver Channel, the kind clear profit head, a surname dissipates the heat of Liver Channel, suppressing the hyperactive liver improving eyesight.Fructus Lycii Sub-sweet in the mouth is put down, and matter is moistened, and is included into lung, liver, kidney channel, the kidney invigorating and essence nourishing, nourishing the liver to improve visual acuity.Both enters Liver Channel, has the effect of improving eyesight, and because of it Nature and flavor are different, are respectively provided with suppressing the hyperactive liver improving eyesight, mend the merit of suitable kidney essense, nourishing the liver to improve visual acuity, jointly play with six Dihuang Wan compatible combination YIN nourishing, nourishing the liver, the effect of improving eyesight.
Although at present the dosage form of Lycium-rehmannia is many, but really can retain comprehensively prescription active ingredients from traditional Chinese medicinal with Guaranteeing curative effect, can accomplish that again preparation is exquisite, dose is little, fully demonstrates substantially not having of Chinese medicine preparation modernization.This medicine is in system Being typically in Bei that medical material is beaten powder to be used as medicine, cause impurity many, dosage is big, affects its clinical practice.Along with medical science technology Fast development, various new techniques, new equipment, the continuous application of new adjuvant, for excavating motherland's medicine treasure-house, strive for Chinese medicine existing Dai Hua, it is provided that excellent opportunity.
The elite of the QIJU DIHUANG WAN collection Chinese medicine that the present invention provides, it is easy to dissolving and absorb, curative effect is fast.
Summary of the invention
One of the technical problem to be solved is to provide a kind of QIJU DIHUANG WAN.
Solve the technical problem that the two of the present invention are to provide the preparation method of a kind of QIJU DIHUANG WAN.
The present invention seeks to be achieved through the following technical solutions:
A kind of QIJU DIHUANG WAN, the raw material including following weight parts is prepared from: Fructus Lycii 30-50 part, Flos Chrysanthemi 30-50 Part, Radix Rehmanniae Preparata 140-180 part, Fructus Corni (system) 60-100 part, Cortex Moutan 40-80 part, Rhizoma Dioscoreae 60-100 part, Poria 40-80 part, Rhizoma Alismatis 40-80 part.
A kind of QIJU DIHUANG WAN, it is characterised in that be prepared from by the raw material of following weight parts: Fructus Lycii 30-50 part, chrysanthemum Flower 30-50 part, Radix Rehmanniae Preparata 140-180 part, Fructus Corni (system) 60-100 part, Cortex Moutan 40-80 part, Rhizoma Dioscoreae 60-100 part, Poria 40-80 part, Rhizoma Alismatis 40-80 part, adjuvant 0.01-1 part.
Preferably, described adjuvant be oleuropein, belulinic acid Betulinic acid, chlorogenic acid one or more mix.
It is highly preferred that described adjuvant is mixed by oleuropein, belulinic acid Betulinic acid, chlorogenic acid, described oleuropein, birch Acid, the mass ratio of chlorogenic acid are (1-3): (1-3): (1-3).
The preparation method of a kind of QIJU DIHUANG WAN, comprises the following steps:
(1) being pulverized by Cortex Moutan is 40-80 mesh coarse powder, sieves, carries out supercritical CO2Fluid extraction, extraction temperature 35-55 DEG C, extraction time 1.5-3.5 hour, extracting pressure 20-40MPa, the flow of carbon dioxide is 10-20kg/h, obtains extraction medicinal liquid, Extraction medicinal liquid again under the conditions of-3-3 DEG C cold preservation take out after 80-100 minute, filter, obtain paeonol crystallization, pulverize as 100-150 Mesh obtains paeonol crystalline powder (I), standby, and medicinal residues (I) are standby；
(2) by Fructus Lycii, Radix Rehmanniae Preparata, Fructus Corni, Rhizoma Alismatis four taste, pulverize as 40-80 mesh coarse powder, sieve, mix homogeneously, enters Row supercritical CO2Fluid extraction, extraction time 1.5-3.5 hour, extraction temperature 35-55 DEG C, extracting pressure 20-40MPa, extraction During add entrainer, the flow of entrainer is 0.5-1.5kg/h, and the flow of carbon dioxide is 10-20kg/h, obtains extraction medicine Liquid, filters, and filtrate reduced in volume to density is the clear paste (I) of 1.15-1.25g/mL, and medicinal residues (II) are standby；
(3) Rhizoma Dioscoreae, Poria, Flos Chrysanthemi pulverizing are 40-80 mesh coarse powder, and medicinal residues (I), medicinal residues (II) mix homogeneously, add and are used as medicine The water of material amount 8-12 times, decocts 1-2 hour, filtered while hot, collects filtrate；Medicinal residues add the clear water of 6-10 times of medication amount Decoct 0.5-1.5 hour, filter waste；Merge twice filtrate, be evaporated to the clear paste that density is 1.15-1.25g/mL (Ⅱ)；
(4) paeonol crystalline powder (I), clear paste (I), clear paste (II) and adjuvant mix homogeneously, pill, it is dried, to obtain final product.
Preferably, the entrainer of described step (2) is that one or more in ethyl acetate, methanol, toluene mix.
It is highly preferred that the entrainer of described step (2) is mixed by ethyl acetate, methanol, toluene, described acetic acid second Mass ratio in ester, methanol, toluene is (1-3): (1-3): (1-3).
Concrete, in the present invention:
Fructus Lycii, Classification system: LyciumbarbarumL., for plant of Solanaceae lycium barbarum Lycium barbarum L. Dry mature fruit, nature and flavor: sweet, flat.Gui Jing: return liver, kidney channel.Effect: nourishing the liver and kidney, replenishing vital essence to improve eyesight.Cure mainly: for asthenia Damage of essence.Curing knee joint soreness, vertigo and tinnitus, interior-heat is quenched one's thirst, blood deficiency and yellow complexion, and blurred vision is failed to understand.
Flos Chrysanthemi, Classification system: Chrysanthemum, for feverfew chrysanthemum Chrysanthemum morifolium Ramat. dry capitulum, nature and flavor: sweet, bitter, it is slightly cold.Gui Jing: return lung, Liver Channel.Effect: dissipate wind heat clearing away, suppressing the hyperactive liver improving eyesight.Main Controlling: for anemopyretic cold, dizziness of having a headache, conjunctival congestion and swelling pain, eyes is dim-sighted.
Radix Rehmanniae Preparata, Classification system: Prepared rhizome of Adhesive Rehmannia, for the process of preparing Chinese medicine of Radix Rehmanniae Processed goods.Nature and flavor: sweet, tepor.Gui Jing: return liver, kidney channel.Effect: nourishing YIN and supplementing blood, benefit essence fills out marrow.Cure mainly: for the hepatic and renal YIN deficiency, Soreness of the waist and knees, osteopyrexia and fever, night sweat passes out semen, and interior-heat quenches one's thirst, blood deficiency and yellow complexion, severe palpitation, menoxenia, metrostaxis, dizziness, Tinnitus, early whitening of beard and hair.
Fructus Corni, Classification system: Cornusofficinalis, for Fructus Corni English section plant Fructus Corni Cornus The drying and ripening sarcocarp of officinalis Sieb.et Zucc., nature and flavor: sour, puckery, tepor.Gui Jing: return liver, kidney channel.Effect: Liver and kidney tonifying, essence astringing and desertion stemming.Curing mainly: for vertigo and tinnitus. soreness of waist and knee joint, sun is passed out semen repeatly.Enuresis frequent micturition, bleeding not during menses, profuse sweating Collapse, interior-heat is quenched one's thirst.Concocting method: take clean Fructus Corni, according to " Chinese Pharmacopoeia " 2005 editions appendix II D stewed with wine methods or wine steam method stew or Steam to wine exhaustion.
Cortex Moutan, the dry root bark of ranunculaceae peony Paeonia suffruticosa Andr..Nature and flavor: bitter, pungent, It is slightly cold.Gui Jing: GUIXIN, liver, kidney channel.Effect: clearing away heat and cooling blood, blood circulation promoting and blood stasis dispelling.Cure mainly: for maculae caused by violent heat pathogen. hematemesis and epistaxis, fever at night The coolest, lossless hectic fever due to YIN-deficiency, amenorrhea dysmenorrhea, carbuncle sore tumefacting virus, falls and flutters the pain of injury.
Rhizoma Dioscoreae, Classification system: Dioscorea opposita, Dioscoreaceae plant Rhizoma Dioscoreae Dioscorea opposita Thunb. dry rhizome.Nature and flavor: sweet are flat.Gui Jing: return spleen, lung, kidney channel.Effect: spleen reinforcing nourishing the stomach, promote the production of body fluid lung benefiting, and the kidney invigorating is puckery Essence.Curing mainly: for insufficiency of the spleen lack of appetite, incessant chronic diarrhea, the deficiency of the lung is breathed with cough, and emission due to deficiency of the kidney, leukorrhagia, frequent micturition, deficiency-heat is quenched one's thirst.Rhizoma Dioscoreae (parched with bran) is mended Spleen stomach invigorating.For insufficiency of the spleen lack of appetite, loose stool of having loose bowels, leukorrhagia.
Poria, Classification system: the dry sclerotia of On Polyporaceae Poria Poria cocos (Schw.) Wolf.Nature and flavor: Sweet, light, flat.Gui Jing: GUIXIN, lung, spleen, kidney channel.Effect: promoting diuresis to eliminate damp pathogen, spleen invigorating mind calming.Curing mainly: for edema oliguria. phlegm retention is dizzy Throbbing with fear, insufficiency of the spleen lack of appetite, loose stool has loose bowels, irritability, palpitation with fear insomnia.
Rhizoma Alismatis, the dry tuber of Notes On Alism At Aceae Rhizoma Alismatis Alisma orientalis (Sam.) Juzep..Nature and flavor: sweet, Cold.Gui Jing: return kidney, bladder warp.Effect: diuresis, clearing away damp-heat.Cure mainly: for dysuria.Edema distension, oliguria of having loose bowels, expectorant Drink dizziness, the puckery pain of pyretic stranguria；Hyperlipidemia.
Oleuropein, No. CAS: 32619-42-4.
Belulinic acid Betulinic acid, No. CAS: 472-15-1.
Chlorogenic acid, No. CAS: 327-97-9.
Ethyl acetate, No. CAS: 141-78-6.
Methanol, No. CAS: 67-56-1.
Toluene, No. CAS: 108-88-3.
QIJU DIHUANG WAN of the present invention, has effect of nourishing the kidney and liver, can be used for treating hepatic and renal YIN deficiency, vertigo and tinnitus, photophobia Photophobia, epiphora induced by wind, the disease such as blurring of vision.Its preparation process uses supercritical CO2Fluid extraction technology, it is possible to fully extract Medical material oil-soluble and water miscible effective ingredient, improve the bioavailability of medical material, and the adjuvant of interpolation ensure that the matter of medicine Amount is stable.
Detailed description of the invention
Embodiment 1
QIJU DIHUANG WAN raw material (weight portion): Fructus Lycii 40 parts, Flos Chrysanthemi 40 parts, Radix Rehmanniae Preparata 160 parts, Fructus Corni (system) 80 Part, Cortex Moutan 60 parts, Rhizoma Dioscoreae 80 parts, 60 parts of Poria, Rhizoma Alismatis 60 parts, adjuvant 0.03 part.
The preparation method of QIJU DIHUANG WAN, comprises the following steps:
(1) being pulverized by Cortex Moutan is 60 mesh coarse powder, sieves, carries out supercritical CO2Fluid extraction, extraction temperature 45 DEG C, extraction Taking time 2 h, extracting pressure 25MPa, the flow of carbon dioxide is 15kg/h, must extract medicinal liquid and medicinal residues (I), extracts medicinal liquid Cold preservation was taken out after 90 minutes under the conditions of-1 DEG C again, used 300 mesh filter-cloth filterings, obtained paeonol crystallization, and it is red that pulverizing is that 120 mesh obtain Skin phenol crystalline powder (I), standby, medicinal residues (I) are standby；
(2) by Fructus Lycii, Radix Rehmanniae Preparata, Fructus Corni, Rhizoma Alismatis four taste, pulverizing is 60 mesh coarse powder, sieves, and mix homogeneously is carried out Supercritical CO2Fluid extraction, extraction time 2 hours, extraction temperature 45 DEG C, extracting pressure 25MPa, extraction process adds and carries secretly Agent, the flow of entrainer is 0.9kg/h, and the flow of carbon dioxide is 15kg/h, must extract medicinal liquid and medicinal residues (II), uses 300 Mesh filter-cloth filtering, filtrate reduced in volume to density is the clear paste (I) of 1.20g/mL (50 DEG C), and medicinal residues (II) are standby；
(3) Rhizoma Dioscoreae, Poria, Flos Chrysanthemi pulverizing are 60 mesh coarse powder, and medicinal residues (I), medicinal residues (II) mix homogeneously, obtain medical material, Add the water of medical material weight 10 times, decoct 2 hours, use 300 mesh filter-cloth filterings while hot, collect filtrate；Medicinal residues add The soak by water that medical material weight is 8 times 1 hour, uses 300 mesh filter-cloth filtering wastes；Merge twice filtrate, be evaporated to density Clear paste (II) for 1.20g/mL (50 DEG C)；
(4) paeonol crystalline powder (I), clear paste (I), clear paste (II) and adjuvant mix homogeneously, pill, it is dried, to obtain final product.
Described adjuvant is mixed by oleuropein, belulinic acid Betulinic acid, chlorogenic acid, described oleuropein, belulinic acid Betulinic acid, chlorogenic acid Mass ratio be 1:1:1.
The entrainer of described step (2) is mixed by ethyl acetate, methanol, toluene, described ethyl acetate, methanol, first Mass ratio in benzene is 1:1:1.
Embodiment 2
Substantially the same manner as Example 1, differ only in: described adjuvant is 1:1 in mass ratio by oleuropein, belulinic acid Betulinic acid Mix homogeneously obtains.Obtain the QIJU DIHUANG WAN of embodiment 2.
Embodiment 3
Substantially the same manner as Example 1, differ only in: described adjuvant is 1:1 in mass ratio by oleuropein, chlorogenic acid Mix homogeneously obtains.Obtain the QIJU DIHUANG WAN of embodiment 3.
Embodiment 4
Substantially the same manner as Example 1, differ only in: described adjuvant is mixed for 1:1 in mass ratio by belulinic acid Betulinic acid, chlorogenic acid Close and uniformly obtain.Obtain the QIJU DIHUANG WAN of embodiment 4.
Embodiment 5
Substantially the same manner as Example 1, differ only in: the entrainer of described step (2) by ethyl acetate, methanol by matter Amount ratio obtains for 1:1 mix homogeneously.Obtain the QIJU DIHUANG WAN of embodiment 5.
Embodiment 6
Substantially the same manner as Example 1, differ only in: the entrainer of described step (2) by ethyl acetate, toluene by matter Amount ratio obtains for 1:1 mix homogeneously.Obtain the QIJU DIHUANG WAN of embodiment 6.
Embodiment 7
Substantially the same manner as Example 1, differ only in: the entrainer of described step (2) is by methanol, toluene in mass ratio Obtain for 1:1 mix homogeneously.Obtain the QIJU DIHUANG WAN of embodiment 7.
Test case 1
Containing morroniside, loganin, paeonol in QIJU DIHUANG WAN of the present invention.The Qi chrysanthemum ground of testing example 1-7 respectively Morroniside, loganin, the content of paeonol in yellow ball, with reference to Li Runze etc., " HPLC method measures in QIJU DIHUANG WAN method of testing The content of morroniside, loganin and paeonol ", concrete outcome is shown in Table 1.
Table 1: each component content test list position: mg/g in QIJU DIHUANG WAN
Morroniside Loganin Paeonol
Embodiment 1 8.95 6.03 13.12
Embodiment 2 6.87 4.38 9.65
Embodiment 3 6.48 4.16 10.01
Embodiment 4 6.93 4.14 10.05
Embodiment 5 7.42 4.86 10.24
Embodiment 6 7.53 5.02 10.63
Embodiment 7 7.68 5.12 10.88
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (oleuropein, belulinic acid Betulinic acid, chlorogenic acid are compounding) ferulaic acid content Apparently higher than embodiment 2-4 (arbitrarily the two compounds for oleuropein, belulinic acid Betulinic acid, chlorogenic acid).Comparing embodiment 1 and embodiment 5-7, Embodiment 1 (ethyl acetate, methanol, toluene are compounding) ferulaic acid content is apparently higher than embodiment 5-7 (ethyl acetate, methanol, toluene Arbitrarily the two compounds).
Test case 2
QIJU DIHUANG WAN embodiment 1-7 prepared, is placed in 25 DEG C, preservation half a year under relative humidity 85% environment, then Carry out the test of escherichia coli (ATYCC 25922) total plate count, with reference to " GBT 4789.2-2008 food hygiene microbiology is examined Test total plate count to measure ".Concrete test result is shown in Table 2.
Table 2: total plate count test table cfu/ part
E. coli clones sum
Embodiment 1 212
Embodiment 2 428
Embodiment 3 417
Embodiment 4 406
Embodiment 5 449
Embodiment 6 452
Embodiment 7 462
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (oleuropein, belulinic acid Betulinic acid, chlorogenic acid are compounding) antiseptic property is bright Show and be better than embodiment 2-4 (arbitrarily the two compounds for oleuropein, belulinic acid Betulinic acid, chlorogenic acid).Comparing embodiment 1 and embodiment 5-7, real Execute example 1 (ethyl acetate, methanol, toluene are compounding) antiseptic property to be substantially better than embodiment 5-7 (ethyl acetate, methanol, toluene are any The two is compounding).

Claims (7)

1. a QIJU DIHUANG WAN, it is characterised in that include that the raw material of following weight parts is prepared from: Fructus Lycii 30-50 part, chrysanthemum Flower 30-50 part, Radix Rehmanniae Preparata 140-180 part, Fructus Corni (system) 60-100 part, Cortex Moutan 40-80 part, Rhizoma Dioscoreae 60-100 part, Poria 40-80 part, Rhizoma Alismatis 40-80 part.
2. a QIJU DIHUANG WAN, it is characterised in that be prepared from by the raw material of following weight parts: Fructus Lycii 30-50 part, Flos Chrysanthemi 30-50 part, Radix Rehmanniae Preparata 140-180 part, Fructus Corni (system) 60-100 part, Cortex Moutan 40-80 part, Rhizoma Dioscoreae 60-100 part, Poria 40- 80 parts, Rhizoma Alismatis 40-80 part, adjuvant 0.01-1 part.
3. the preparation method of QIJU DIHUANG WAN as claimed in claim 2, it is characterised in that: described adjuvant be oleuropein, Belulinic acid Betulinic acid, chlorogenic acid one or more mix.
4. the preparation method of QIJU DIHUANG WAN as claimed in claim 3, it is characterised in that: described adjuvant by oleuropein, Belulinic acid Betulinic acid, chlorogenic acid mix, and described oleuropein, belulinic acid Betulinic acid, the mass ratio of chlorogenic acid are (1-3): (1-3): (1-3).
5. the preparation method of the QIJU DIHUANG WAN as according to any one of claim 1-4, it is characterised in that include following step Rapid:
(1) being pulverized by Cortex Moutan is 40-80 mesh coarse powder, sieves, carries out supercritical CO2Fluid extraction, extraction temperature 35-55 DEG C, extraction Taking the time 1.5-3.5 hour, extracting pressure 20-40MPa, the flow of carbon dioxide is 10-20kg/h, obtains extraction medicinal liquid, extraction Medicinal liquid again under the conditions of-3-3 DEG C cold preservation take out after 80-100 minute, filter, obtain paeonol crystallization, pulverize and obtain for 100-150 mesh Paeonol crystalline powder (I), standby, medicinal residues (I) are standby；
(2) by Fructus Lycii, Radix Rehmanniae Preparata, Fructus Corni, Rhizoma Alismatis four taste, pulverize as 40-80 mesh coarse powder, sieve, mix homogeneously, surpass Critical CO2Fluid extraction, extraction time 1.5-3.5 hour, extraction temperature 35-55 DEG C, extracting pressure 20-40MPa, extraction process Middle interpolation entrainer, the flow of entrainer is 0.5-1.5kg/h, and the flow of carbon dioxide is 10-20kg/h, obtains extraction medicinal liquid, Filtering, filtrate reduced in volume to density is the clear paste (I) of 1.15-1.25g/mL, and medicinal residues (II) are standby；
(3) Rhizoma Dioscoreae, Poria, Flos Chrysanthemi pulverizing are 40-80 mesh coarse powder, and medicinal residues (I), medicinal residues (II) mix homogeneously, add medical material amount The water of 8-12 times, decocts 1-2 hour, filtered while hot, collects filtrate；The clear water adding 6-10 times of medication amount in medicinal residues decocts 0.5-1.5 hour, filter waste；Merge twice filtrate, be evaporated to the clear paste (II) that density is 1.15-1.25g/mL；
(4) paeonol crystalline powder (I), clear paste (I), clear paste (II) and adjuvant mix homogeneously, pill, it is dried, to obtain final product.
6. the preparation method of QIJU DIHUANG WAN as claimed in claim 5, it is characterised in that: the entrainer of described step (2) is One or more in ethyl acetate, methanol, toluene mix.
7. the preparation method of QIJU DIHUANG WAN as claimed in claim 6, it is characterised in that: the entrainer of described step (2) by Ethyl acetate, methanol, toluene mix, and the mass ratio in described ethyl acetate, methanol, toluene is (1-3): (1-3): (1- 3)。
CN201610803215.6A 2016-09-06 2016-09-06 QIJU DIHUANG WAN and preparation method thereof Withdrawn CN106177345A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108562681A (en) * 2018-06-28 2018-09-21 江苏海昇药业有限公司 The quantitative detection method of QIJU DIHUANG KOUFUYE multicomponent
CN116459306A (en) * 2023-05-06 2023-07-21 江西广恩和药业股份有限公司 Traditional Chinese medicine extracting solution, preparation method and application thereof in oral liquid

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108562681A (en) * 2018-06-28 2018-09-21 江苏海昇药业有限公司 The quantitative detection method of QIJU DIHUANG KOUFUYE multicomponent
CN108562681B (en) * 2018-06-28 2019-04-05 江苏海昇药业有限公司 The quantitative detection method of QIJU DIHUANG KOUFUYE multicomponent
CN116459306A (en) * 2023-05-06 2023-07-21 江西广恩和药业股份有限公司 Traditional Chinese medicine extracting solution, preparation method and application thereof in oral liquid
CN116459306B (en) * 2023-05-06 2024-05-03 江西广恩和药业股份有限公司 Traditional Chinese medicine extracting solution, preparation method and application thereof in oral liquid

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