CN107669865A - A kind of anti-senile dementia disease oral agents - Google Patents

A kind of anti-senile dementia disease oral agents Download PDF

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Publication number
CN107669865A
CN107669865A CN201711089866.4A CN201711089866A CN107669865A CN 107669865 A CN107669865 A CN 107669865A CN 201711089866 A CN201711089866 A CN 201711089866A CN 107669865 A CN107669865 A CN 107669865A
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parts
water
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medicinal material
decoction
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钟安祺
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Guangxi Nanning Shengqian Technology Development Co Ltd
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Guangxi Nanning Shengqian Technology Development Co 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
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/74—Rubiaceae (Madder family)
    • 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)
    • A61K36/29—Berberidaceae (Barberry family), e.g. barberry, cohosh or mayapple
    • A61K36/296—Epimedium
    • 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)
    • A61K36/40—Cornaceae (Dogwood family)
    • 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)
    • A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • 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)
    • A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/734—Crataegus (hawthorn)
    • 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)
    • A61K36/75—Rutaceae (Rue family)
    • A61K36/752—Citrus, e.g. lime, orange or lemon
    • 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)
    • A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
    • 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)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/894—Dioscoreaceae (Yam family)
    • A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/55—Liquid-liquid separation; Phase separation

Abstract

The present invention provides a kind of anti-senile dementia disease oral agents and preparation method thereof, using Red Psychotria Leaf active material total iridoid glycoside as main material, it is aided with each herbal medicine extract solution of Fructus Corni, barrenwort, dried orange peel, Chinese yam, hawthorn, lavender, Lychee juice to be prepared, utilize mesoporous calcium silicate material assisted extraction Red Psychotria Leaf total iridoid glycoside, mesoporous carbon carries out purification enrichment, can greatly improve the recovery rate and purifying rate of iridoid glycoside.The present invention can effectively improve the recovery rate of iridoid, reduce production cost, have good development prospect.

Description

A kind of anti-senile dementia disease oral agents
Technical field
The invention belongs to extract oral agent preparation and middle medicinal substances extractive technique field, more particularly to a kind of anti-senile dementia Oral agents and preparation method thereof.
Background technology
Alzheimer disease（AD）It is a kind of nervous system degenerative disease of the progress sexual development of onset concealment.Clinically With memory disorders, aphasia, appraxia, agnosia, the infringement of visual space technical ability, perform function obstacle and personality and behavior change etc. comprehensively Property dull-witted performance be characterized, the cause of disease is unknown so far.Hair patient before 65 years old, claims alzheimer's disease；Claimed always with sequela person within 65 years old Year property is dull-witted.Its main pathogenesis can be summarized as " empty, strongly fragrant, phlegm, the stasis of blood ", using the virtual loss of brains and the five internal organs as this, using strongly fragrant, phlegm, the stasis of blood as Mark.Senile dementia is the disease of asthenia in origin and asthenia in superficiality.This void is that declining for negative and positive of qi and blood is few, and mark is mostly the production of the pathology such as gas, fire, phlegm, the stasis of blood actually The accumulation of thing.Though its sick position is in brain, closely related with the function of the internal organs such as conscience spleen kidney.Treatment by Chinese herbs is then dialectical with differentiation of disease phase Heavy curtain is tied, or is controlled from void opinion, or based on eliminating evil, or tonification and purgation in combination.It was verified that traditional Chinese medicine has very to treating this disease and prognosis Important meaning, there is potential advantage and wide DEVELOPMENT PROSPECT.
Patent of invention CN201310064678.1, a kind of kind drug composition for treating senile dementia, it is characterised in that in this Drug composition is made up of the medicine of following parts by weight：Red sage root 25-35 parts, corydalis tuber 15-25 parts, radix paeoniae rubrathe 10-20 parts, tribulus terrestris 15-25 parts, Buddha's hand 10-20 parts, citron 10-20 parts, Ligusticum wallichii 7-17 parts, safflower 5-15 parts, Moschus 0.03-0.07 parts, spina gleditsiae 20-28 parts, Radix Angelicae Sinensis 13-23 parts, raw Radix Astragali 25-35 parts, Flos Albiziae 10-20 parts, licorice 3-9 parts, ginger 6-12 parts, jujube 3- 7 parts.With promoting blood circulation and removing blood stasis, mental-tranquilization, soothing liver-qi stagnation, it is eliminating dampness and eliminating phlegm the effect of, the Chinese medicine composition is old silly for treatment Stay with good effect, target spot is more, the characteristics of Small side effects.
Nine section wood（Red Psychotria Leaf）In contained activity extract total iridoid glycoside etc. there is anti-senile dementia, it is existing Nine section wood in technology（Red Psychotria Leaf）Middle active extraction is mostly alcohol extracting circumfluence method, and total iridoid glycoside recovery rate is relatively low, and only 18% Left and right so that main pharmacodynamics material utilization is low.
Patent of invention CN201510363712.4, a kind of pharmaceutical preparation for being used to treat hepatic sclerosis, is prepared by the following raw material Obtain：20 parts of Red Psychotria Leaf, 15 parts of the ears of an ox or cow purple bergenia herb, 12 parts of black nightshade, 15 parts of radix scutellariae, 15 parts of Canton love-pea vine, 12 parts of the membrane of a chicken's gizzard, radix glycyrrhizae 5 Part, 20 parts of oldenlandia diffusa, 10 parts of the tuber of pinellia, 15 parts of the fruit of glossy privet, 30 parts of reticulate millettia, 10 parts of curcuma zedoary, 6 parts of radix bupleuri, 40 parts of stringy stonecrop, 10 parts of the bighead atractylodes rhizome, 12 parts of the fruit of Chinese wolfberry, the invention can treat hepatic sclerosis；The patent utilization decocting method carries out active matter to each medicine and carried Take.Patent of invention CN201210214331.6 Red Psychotria Leaf extracts and preparation method thereof and antitumor application thereof, disclose a kind of mountain Great Yan extracts and preparation method thereof and antitumor application thereof.Red Psychotria Leaf extract is prepared by the following method：Red Psychotria Leaf is passed through Ethanol or methanol are heated to reflux or are percolated extraction, are concentrated under reduced pressure to give medicinal extract, through macroporous resin enrichment, methanol-water elution, obtain To Red Psychotria Leaf extract.The Red Psychotria Leaf extract of the present invention can be used for the medicine and health products for preparing treatment tumour, and it imitates position Definite ingredients, small toxicity, pharmacological action is strong, has good prospect in medicine；Preparation technology is simple, is easy to mass produce.Mountain Great Yan triterpenoid saponins are through ethanol/water heating extraction, and be concentrated under reduced pressure to obtain medicinal extract, and medicinal extract adds water to stir, successively with petroleum ether, ether Low polarity component is proposed, extracting n-butyl alcohol, n-butanol portion macroporous resin enrichment, ethanol/water elution, product is through methanol/water Anti-phase ODS elution isolates and purifies, recrystallize after obtain.
Medicinal plant contains a large amount of active skull cap components, and China is in the world earliest using traditional biological technology from plant The country of active component is prepared, in treatment disease, Chinese herbal medicine possesses many advantages.
The content of the invention
Low for Red Psychotria Leaf anti-senile dementia disease drug rate of exploitation in the prior art, Red Psychotria Leaf active material recovery rate is low Problem, the present invention provide a kind of method of high efficiency extraction Red Psychotria Leaf iridoid and its prepare the side of anti-senile dementia disease oral agents Method.
The present invention is achieved through the following technical solutions：
A kind of anti-senile dementia oral agents, compare component comprising following weight fraction：50 ~ 100 parts of Red Psychotria Leaf, Fructus Corni 50 ~ 100 Part, 10 ~ 20 parts of barrenwort, 10 ~ 20 parts of dried orange peel, 5 ~ 10 parts of Chinese yam, 20 ~ 50 parts of hawthorn, 5 ~ 10 parts of lavender, Lychee juice 50 ~ 100 Part.
It is prepared by following steps：
（1）50 ~ 100 parts of Red Psychotria Leaf is taken, is ground into the coarse powder of 10 ~ 20 mesh, adds water to cook 3 times, it is big that mountain is previously added in decoction liquor The mesoporous silicic acid calcium powder of face meal quality 20% ~ 30%, is filtered, merging filtrate respectively, and concentrated aqueous amount is 20 ~ 30%, is obtained dense Contracting liquid I；
（2）Concentrate I is taken, adds 10 ~ 15 times of purifying water enchroachment (invasion) bubble 30 ~ 60min, 2 ~ 3h of refluxing extraction, filtering, filter residue adds 6 ~ 8 times Purified water, by concentrate add 3 ~ 6mg/ml of cellulase, in constant-temperature heating magnetic stirring apparatus 45 ~ 55 DEG C of water enzyme digestions 2 ~ 3h, filter after enzymolysis, filter residue adds 6 ~ 8 times of amount purified waters, 1 ~ 1.5h of refluxing extraction, extract solution filtered through gauze, filtrate with 3000r/min centrifuges 20 ~ 30min, and by supernatant concentration, sample liquid is made；
（3）Sample liquid is taken, according to sample liquid：Mesoporous carbon=1g：（10~12g）It is static after mesoporous carbon adsorption column loading, loading to inhale Attached 1 ~ 2h, first being cleaned with 2 ~ 2.5BV distillation water elutions, then eluted with the ethanol solution of volume fraction 15 ~ 20%, flow velocity is 1 ~ 1.2BV/h, eluent is collected, concentrated, dried, you can obtain iridoid glycoside powder；
（4）Take 50 ~ 100 parts of Fructus Corni, 10 ~ 20 parts of barrenwort, 10 ~ 20 parts of dried orange peel, 5 ~ 10 parts of Chinese yam, 20 ~ 50 parts of hawthorn, smoke clothing 5 ~ 10 parts of grass, is crushed to 20 ~ 50 mesh, after mixing, adds water to cook 3 times, filter respectively, merging filtrate, be concentrated into water content for 30 ~ 50%；Obtain concentrate II；
（5）Iridoid powder, concentrate II are mixed for 50 ~ 100 parts with Lychee juice, dispensed after sterilizing, you can obtain anti-ageing year Dull-witted oral agents.
Fructus Corni can stomach invigorating, be effectively improved patients of senile dementia because long-term ill and caused by anorexia, be rich in Vitamin can guarantee that iridoid glycoside is not oxidized in Red Psychotria Leaf, improve drug effect.
Dried orange peel has reason stomach effect, and its fragrance can make patient using not producing vomiting during this oral agents, while dried orange peel has Appetizing is acted on, and patient can be allowed not produce resistance to the taste of oral agents；
Lavender has the effect of useful for sleeping, and patient can improve sleep quality after taking, human body metabolism in sleep is vigorous, Drug effect can preferably be improved；
On the one hand Lychee juice is used as sweetener, improve the sweet taste of oral agents, and another aspect Lychee juice has the effect of regulating qi-flowing for relieving pain, The disease such as insomnia, forgetful, dreaminess can be improved, and skin metabolism, anti-aging can be promoted；
Chinese yam improves patients of senile dementia hematopoietic potential, metabolism is improved, so as to promote human body to medicine rich in trace element The absorption of thing；
As a further improvement on the present invention, the step（1）First time decoction is adjusted to pH as 1.0 with water using 1mol/L hydrochloric acid ~ 2.0, amount of water is 10 ~ 12 times of medicinal material amount, and decocting time is 3.8 ~ 4.5h；Second of decoction water is with saturation sodium hydroxide It is 7.0 ~ 7.5 to be adjusted to pH, and amount of water is 10 ~ 12 times of medicinal material medicinal material amount, and decocting time is 1.8 ~ 2.4h；Third time decoction water PH is adjusted to as 9.5 ~ 10.0 using saturation sodium hydroxide, amount of water is 8 ~ 10 times of medicinal material amount, and decocting time is 1.8 ~ 2.4h.
As a further improvement on the present invention, the step（4）First time decoction is adjusted to pH with water with 1mol/L hydrochloric acid For 2.0 ~ 3.0, amount of water is 12 ~ 16 times of medicinal material amount, and decocting time is 1.8 ~ 2.2h；Second of decoction water is with saturation hydrogen-oxygen It is 7.5 ~ 8.0 to change sodium to be adjusted to pH, and amount of water is 12 ~ 16 times of medicinal material medicinal material amount, and decocting time is 0.8 ~ 1.2h；Third time decocts PH is adjusted to as 9.5 ~ 10.0 with water using saturation sodium hydroxide, amount of water is 10 ~ 14 times of medicinal material amount, decocting time is 0.8 ~ 1.2h。
The high temperature of decocting method is easy to the change for causing traditional Chinese medicine ingredients when soda acid extracts, and influences the safety of traditional Chinese medicine ingredients Property and validity, constrain application of the thermal instability medicine in extraction process；Mesoporous calcium silicates has the suction of Large ratio surface Attached effect, mesoporous effectively to adsorb traditional Chinese medicine ingredients in extraction process, reduce high temperature decoction effect has to active ingredient of Chinese herbs Evil influences, while the bigger serface hole of mesoporous material can more adsorb the iridoid glycoside in Red Psychotria Leaf extract solution, improves The recovery rate of iridoid glycoside and its complete species activity is maintained in Red Psychotria Leaf.
As a further improvement on the present invention, the mesoporous silicic acid calcium powder preparation method is as follows：
（1）Weigh 10 ~ 20 parts of four water-calcium nitrates to be dissolved into 80 ~ 100 parts of distilled water, being sufficiently stirred 1 ~ 2h makes calcium nitrate complete Dissolving, then adds 6 ~ 10 parts of template cetane trimethyl ammonium bromide, 20 ~ 30 parts of geniposide, at 45 ~ 55 DEG C with 120r/min speed stirs 1 ~ 1.5h, and white gels are gradually formed in whipping process；
Maximum as the mesoporous calcium silicates specific surface area that template synthesizes using cetane trimethyl ammonium bromide, surface topography is best, class Seemingly cellular, surface duct is mutually communicated, and excellent place is provided for the absorption of heavy metal ion；
Geniposide has similar structure to iridoid, prepares and divides as analysis marking template instead of the iridoid of costliness The sub- mesoporous calcium silicate material of trace, can effectively adsorb iridoid glycoside in decoction process
（2）According to Ca in four water-calcium nitrate and nine water sodium metasilicate：The amount ratio of Si materials is 1：1 weighs nine water sodium metasilicate, is dissolved in In 40 ~ 60 parts of distilled water, then this sodium silicate solution is slowly dropped in calcium nitrate solution, with the addition of sodium metasilicate, by White gum thing is gradually formed, after reacting 4 ~ 5h, is aged 20 ~ 24h at normal temperatures；Then distilled water washed product is used, then with anhydrous Ethanol is stripped 22 ~ 24h, to remove template agent removing；Products therefrom is placed in vacuum drying chamber at 40 DEG C and dries 12 ~ 14h, Dried product is ground, you can obtain mesoporous silicic acid calcium powder；
As a further improvement on the present invention, the mesoporous carbon absorption column preparation method is as follows：
The mesoporous carbon absorption column preparation method is as follows：
（1）Weigh 16 ~ 22 parts of poly- propoxyl group-polyethoxy-poly- propoxyl group triblock copolymers and 10 ~ 20 parts of 0.2mol/L hydrochloric acid Solution is mixed in 80 ~ 100 parts of ethanol, and 1h is stirred at 40 DEG C, sequentially adds 20 ~ 26 parts of tetraethyl orthosilicates and 40 ~ 50 parts of weights The phenolic resin ethanol solution of percentage 20% is measured, is evenly applied to after continuing 2 ~ 3h of stirring in culture dish, room temprature evaporation 7 ~ Culture 24h at 100 DEG C is placed in baking oven after 9h and obtains pale yellow transparent film；
（2）Transparent membrane is scraped to grinding from culture dish, in N2Under protection, 800 ~ 900 DEG C of calcining 5h are placed in tube furnace just Obtain ordered mesopore carbon-silica composite；
（3）The compound is impregnated in 10% 24 ~ 26h of hf etching, removes silicon components, then respectively with the body of 3 ~ 4 times of amounts The sodium hydrate aqueous solution of fraction 5%, distilled water, the acetic acid aqueous solution of volume fraction 10% of 3 ~ 4 times of amounts of 1 ~ 2 times of amount wash, most Neutrality is washed to distillation afterwards, wet method is fitted into chromatographic column, produces required mesoporous carbon adsorption column.
Mesoporous carbon adsorption column can more effectively adsorb the glycoside such as iridoid glycoside and terpene substances in Red Psychotria Leaf, but not adsorb Or other materials are seldom adsorbed, have and preferably isolate and purify effect, while meso-hole structure can more adsorb iridoid glycoside Material, improve purifying rate.
Beneficial effects of the present invention：
1st, the extraction of iridoid glycoside material in Red Psychotria Leaf is carried out by mesoporous material secondary analog human body intestinal canal acid or alkali environment, no The recovery rate of medicinal substances in Red Psychotria Leaf is only effectively increased, while reduces the destructiveness that active material is subject to by high temperature；Profit Purifying rate is not only increased with meso-porous carbon material, more active principle is more retained.
2nd, the oral agents prepared by the present invention, iridoid recovery rate is high, and its activity is high, reduces cost, has very Good economic benefit.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
A kind of anti-senile dementia disease oral agents, are prepared by following steps：
（1）50 parts of Red Psychotria Leaf is taken, is ground into the coarse powder of 10 mesh, is added water to cook 3 times, Red Psychotria Leaf coarse powder matter is previously added in decoction liquor The mesoporous silicic acid calcium powder of amount 20%, is filtered, merging filtrate respectively, and concentrated aqueous amount is 20%, obtains concentrate I；
The decocting method is：First time decoction is adjusted to pH as 1.0 with water using 1mol/L hydrochloric acid, and amount of water is the 10 of medicinal material amount Times, decocting time 3.8h；Second of decoction is adjusted to pH as 7.0 with water using saturation sodium hydroxide, and amount of water is medicinal material medicinal material amount 10 times, decocting time 1.8h；Third time decoction is adjusted to pH as 9.5 with water using saturation sodium hydroxide, and amount of water is medicinal material amount 8 times, decocting time 1.8h.
The mesoporous silicic acid calcium powder preparation method is as follows：
A. weigh 10 parts of four water-calcium nitrates to be dissolved into 80 parts of distilled water, being sufficiently stirred 1h is completely dissolved calcium nitrate, then 6 parts of template cetane trimethyl ammonium bromide is added, 20 parts of geniposide, 1h, stirring are stirred with 120rmin speed at 45 DEG C During gradually form white gels；
B. according to Ca in four water-calcium nitrate and nine water sodium metasilicate：The amount ratio of Si materials is 1：1 weighs nine water sodium metasilicate, is dissolved in 40 In part distilled water, then this sodium silicate solution is slowly dropped in calcium nitrate solution, with the addition of sodium metasilicate, gradually formed White gum thing, after reacting 5h, 24h is aged at normal temperatures；Then distilled water washed product is used, then is stripped with absolute ethyl alcohol 24h, to remove template agent removing；Products therefrom is placed in vacuum drying chamber at 40 DEG C and dries 12h, dried product is ground Mill, you can obtain mesoporous silicic acid calcium powder；
（2）Concentrate I is taken, adds 10 times of purifying water enchroachment (invasion) bubble 30min, refluxing extraction 2h, filtering, filter residue adds 6 times of purified waters, by dense Contracting liquid adds cellulase 3mg/ml, 45 DEG C of water enzyme digestion 2h in constant-temperature heating magnetic stirring apparatus, filters after enzymolysis, filter residue adds Enter 6 times of amount purified waters, refluxing extraction 1h, extract solution filtered through gauze, filtrate centrifuges 20min with 3000r/min, and supernatant is dense Contracting, sample liquid is made；
（3）Sample liquid is taken, according to sample liquid：Mesoporous carbon=1g：10g Static Adsorption 1h after mesoporous carbon adsorption column loading, loading, First cleaned, then eluted with the ethanol solution of volume fraction 15%, flow velocity 1BV/h with 2BV distillation water elutions, collect eluent, it is dense Contracting, dry, you can obtain iridoid glycoside powder；
（4）50 parts of Fructus Corni, 10 parts of barrenwort, 10 parts of dried orange peel, 5 parts of Chinese yam, 20 parts of hawthorn, 5 parts of lavender are taken, is crushed to 20 Mesh, after mixing, add water to cook 3 times, filter respectively, merging filtrate, be concentrated into water content as 30%；Obtain concentrate II；
First time decoction is adjusted to pH as 2.0 with water using 1mol/L hydrochloric acid, and amount of water is 12 times of medicinal material amount, and decocting time is 1.8h；Second of decoction is adjusted to pH as 7.5 with water using saturation sodium hydroxide, and amount of water is 12 times of medicinal material medicinal material amount, during decoction Between be 0.8h；Third time decoction is adjusted to pH as 9.5 with water using saturation sodium hydroxide, and amount of water is 10 times of medicinal material amount, during decoction Between be 0.8h.
The mesoporous carbon absorption column preparation method is as follows：
A. 16 parts of poly- propoxyl group-polyethoxy-poly- propoxyl group triblock copolymers are weighed and 10 parts of 0.2mol/L hydrochloric acid solutions mix Together in 80 parts of ethanol, 1h is stirred at 40 DEG C, sequentially adds the phenolic aldehyde of 20 parts of tetraethyl orthosilicates and 40 parts of percentage by weights 20% Resin ethanol solution, continue to be evenly applied in culture dish after stirring 2h, be placed in after room temprature evaporation 7h in baking oven at 100 DEG C Culture 24h obtains pale yellow transparent film；
B., transparent membrane is scraped to grinding from culture dish, in N2Under protection, being placed in 800 DEG C of calcining 5h in tube furnace is just had Sequence mesoporous carbon-silica composite；
C., the compound is impregnated in 10% hf etching 24h, removes silicon components, then respectively with the volume fraction of 3 times of amounts 5% sodium hydrate aqueous solution, distilled water, the acetic acid aqueous solution of volume fraction 10% of 3 times of amounts of 1 times of amount wash, and finally use distilled water Neutrality is washed till, wet method is fitted into chromatographic column, produces required mesoporous carbon adsorption column.
（5）Iridoid powder, concentrate II are mixed with Lychee juice, dispensed after sterilizing, you can obtain anti-senile dementia Oral agents.
The present embodiment iridoid glycoside recovery rate is 21.1%, and purifying rate is 99.8%.
Embodiment 2
A kind of anti-senile dementia disease oral agents, are prepared by following steps：
（1）100 parts of Red Psychotria Leaf is taken, is ground into the coarse powder of 20 mesh, adds water to cook 3 times, Red Psychotria Leaf coarse powder is previously added in decoction liquor The mesoporous silicic acid calcium powder of quality 30%, is filtered, merging filtrate respectively, and concentrated aqueous amount is 30%, obtains concentrate I；
First time decoction is adjusted to pH as 2.0 with water using 1mol/L hydrochloric acid, and amount of water is 12 times of medicinal material amount, and decocting time is 4.5h；Second of decoction is adjusted to pH as 7.5 with water using saturation sodium hydroxide, and amount of water is 12 times of medicinal material medicinal material amount, during decoction Between be 2.4h；Third time decoction is adjusted to pH as 10.0 with water using saturation sodium hydroxide, and amount of water is 10 times of medicinal material amount, during decoction Between be 2.4h.
The mesoporous silicic acid calcium powder preparation method is as follows：
A. weigh 20 parts of four water-calcium nitrates to be dissolved into 100 parts of distilled water, being sufficiently stirred 2h is completely dissolved calcium nitrate, then 10 parts of template cetane trimethyl ammonium bromide is added, 30 parts of geniposide, 2h is stirred with 120r/min speed at 45 DEG C, stirred White gels are gradually formed during mixing；
B. according to Ca in four water-calcium nitrate and nine water sodium metasilicate：The amount ratio of Si materials is 1：1 weighs nine water sodium metasilicate, is dissolved in 60 In part distilled water, then this sodium silicate solution is slowly dropped in calcium nitrate solution, with the addition of sodium metasilicate, gradually formed White gum thing, after reacting 5h, 24h is aged at normal temperatures；Then distilled water washed product is used, then is stripped with absolute ethyl alcohol 24h, to remove template agent removing；Products therefrom is placed in vacuum drying chamber at 40 DEG C and dries 14h, dried product is ground Mill, you can obtain mesoporous silicic acid calcium powder；
（2）Concentrate I is taken, adds 15 times of purifying water enchroachment (invasion) bubble 60min, refluxing extraction 3h, filtering, filter residue adds 8 times of purified waters, by dense Contracting liquid adds 3 ~ 6mg/ml of cellulase, 55 DEG C of water enzyme digestion 3h in constant-temperature heating magnetic stirring apparatus, filters after enzymolysis, filter residue 8 times of amount purified waters are added, refluxing extraction 1.5h, extract solution filtered through gauze, filtrate centrifuges 30min with 3000r/min, by supernatant Liquid concentrates, and sample liquid is made；
（3）Sample liquid is taken, according to sample liquid：Mesoporous carbon=1g：12g Static Adsorption 2h after mesoporous carbon adsorption column loading, loading, First cleaned with 2.5BV distillation water elutions, then eluted with the ethanol solution of volume fraction 20%, flow velocity 1.2BV/h, collect elution Liquid, concentrate, dry, you can obtain iridoid glycoside powder；
（4）100 parts of Fructus Corni, 20 parts of barrenwort, 20 parts of dried orange peel, 10 parts of Chinese yam, 50 parts of hawthorn, 10 parts of lavender are taken, is crushed to 50 mesh, after mixing, add water to cook 3 times, filter respectively, merging filtrate, be concentrated into water content as 50%；Obtain concentrate II；
First time decoction is adjusted to pH as 3.0 with water using 1mol/L hydrochloric acid, and amount of water is 16 times of medicinal material amount, and decocting time is 2.2h；Second of decoction is adjusted to pH as 8.0 with water using saturation sodium hydroxide, and amount of water is 16 times of medicinal material medicinal material amount, during decoction Between be 1.2h；Third time decoction is adjusted to pH as 10.0 with water using saturation sodium hydroxide, and amount of water is 14 times of medicinal material amount, during decoction Between be 1.2h.
The mesoporous carbon absorption column preparation method is as follows：
A. 22 parts of poly- propoxyl group-polyethoxy-poly- propoxyl group triblock copolymers are weighed and 20 parts of 0.2mol/L hydrochloric acid solutions mix Together in 100 parts of ethanol, 1h is stirred at 40 DEG C, sequentially adds the phenol of 26 parts of tetraethyl orthosilicates and 50 parts of percentage by weights 20% Urea formaldehyde ethanol solution, continue to be evenly applied in culture dish after stirring 2h, 100 DEG C are placed in baking oven after room temprature evaporation 7h Lower culture 24h obtains pale yellow transparent film；
B., transparent membrane is scraped to grinding from culture dish, in N2Under protection, being placed in 900 DEG C of calcining 5h in tube furnace is just had Sequence mesoporous carbon-silica composite；
C., the compound is impregnated in 10% hf etching 26h, removes silicon components, then respectively with the volume fraction of 4 times of amounts 5% sodium hydrate aqueous solution, distilled water, the acetic acid aqueous solution of volume fraction 10% of 4 times of amounts of 2 times of amounts wash, and finally use distilled water Neutrality is washed till, wet method is fitted into chromatographic column, produces required mesoporous carbon adsorption column.
（5）Iridoid powder, concentrate II are mixed with Lychee juice, dispensed after sterilizing, you can obtain anti-senile dementia Oral agents.
The present embodiment iridoid glycoside recovery rate is 20.6%, and purifying rate is 99.7%.
Embodiment 3
A kind of anti-senile dementia disease oral agents, are prepared by following steps：
（1）80 parts of Red Psychotria Leaf is taken, is ground into the coarse powder of 15 mesh, is added water to cook 3 times, Red Psychotria Leaf coarse powder matter is previously added in decoction liquor The mesoporous silicic acid calcium powder of amount 25%, is filtered, merging filtrate respectively, and concentrated aqueous amount is 25%, obtains concentrate I；
First time decoction is adjusted to pH as 1.8 with water using 1mol/L hydrochloric acid, and amount of water is 11 times of medicinal material amount, and decocting time is 4h；Second of decoction is adjusted to pH as 7.2 with water using saturation sodium hydroxide, and amount of water is 11 times of medicinal material medicinal material amount, decocting time For 2h；Third time decoction is adjusted to pH as 9.6 with water using saturation sodium hydroxide, and amount of water is 9 times of medicinal material amount, and decocting time is 2h。
The mesoporous silicic acid calcium powder preparation method is as follows：
A. weigh 15 parts of four water-calcium nitrates to be dissolved into 90 parts of distilled water, being sufficiently stirred 1h is completely dissolved calcium nitrate, then 8 parts of template cetane trimethyl ammonium bromide is added, 25 parts of geniposide, 1h is stirred with 120r/min speed at 45 DEG C, stirred White gels are gradually formed during mixing；
B. according to Ca in four water-calcium nitrate and nine water sodium metasilicate：The amount ratio of Si materials is 1：1 weighs nine water sodium metasilicate, is dissolved in 50 In part distilled water, then this sodium silicate solution is slowly dropped in calcium nitrate solution, with the addition of sodium metasilicate, gradually formed White gum thing, after reacting 5h, 24h is aged at normal temperatures；Then distilled water washed product is used, then is stripped with absolute ethyl alcohol 24h, to remove template agent removing；Products therefrom is placed in vacuum drying chamber at 40 DEG C and dries 12h, dried product is ground Mill, you can obtain mesoporous silicic acid calcium powder；
（2）Concentrate I is taken, adds 12 times of purifying water enchroachment (invasion) bubble 50min, refluxing extraction 2.5h, filtering, filter residue adds 7 times of purified waters, pressed Concentrate adds cellulase 5mg/ml, 50 DEG C of water enzyme digestion 3h in constant-temperature heating magnetic stirring apparatus, filters after enzymolysis, filter residue 7 times of amount purified waters are added, refluxing extraction 1.2h, extract solution filtered through gauze, filtrate centrifuges 25min with 3000r/min, by supernatant Liquid concentrates, and sample liquid is made；
（3）Sample liquid is taken, according to sample liquid：Mesoporous carbon=1g：11g Static Adsorptions after mesoporous carbon adsorption column loading, loading 1.5h, first cleaned with 2.2BV distillation water elutions, then eluted with the ethanol solution of volume fraction 16%, flow velocity 1.1BV/h, collected Eluent, concentrate, dry, you can obtain iridoid glycoside powder；
（4）60 parts of Fructus Corni, 12 parts of barrenwort, 12 parts of dried orange peel, 8 parts of Chinese yam, 30 parts of hawthorn, 6 parts of lavender are taken, is crushed to 30 Mesh, after mixing, add water to cook 3 times, filter respectively, merging filtrate, be concentrated into water content as 40%；Obtain concentrate II；
First time decoction is adjusted to pH as 2.2 with water using 1mol/L hydrochloric acid, and amount of water is 13 times of medicinal material amount, and decocting time is 2h；Second of decoction is adjusted to pH as 7.6 with water using saturation sodium hydroxide, and amount of water is 13 times of medicinal material medicinal material amount, decocting time For 1h；Third time decoction is adjusted to pH as 9.5 ~ 10.0 with water using saturation sodium hydroxide, and amount of water is 12 times of medicinal material amount, during decoction Between be 1h.
The mesoporous carbon absorption column preparation method is as follows：
A. 20 parts of poly- propoxyl group-polyethoxy-poly- propoxyl group triblock copolymers are weighed and 15 parts of 0.2mol/L hydrochloric acid solutions mix Together in 90 parts of ethanol, 1h is stirred at 40 DEG C, sequentially adds the phenolic aldehyde of 22 parts of tetraethyl orthosilicates and 45 parts of percentage by weights 20% Resin ethanol solution, continue to be evenly applied in culture dish after stirring 2h, be placed in after room temprature evaporation 7h in baking oven at 100 DEG C Culture 24h obtains pale yellow transparent film；
B., transparent membrane is scraped to grinding from culture dish, in N2Under protection, being placed in 850 DEG C of calcining 5h in tube furnace is just had Sequence mesoporous carbon-silica composite；
C., the compound is impregnated in 10% hf etching 24h, removes silicon components, then respectively with the volume fraction of 3 times of amounts 5% sodium hydrate aqueous solution, distilled water, the acetic acid aqueous solution of volume fraction 10% of 3 times of amounts of 1 times of amount wash, and finally use distilled water Neutrality is washed till, wet method is fitted into chromatographic column, produces required mesoporous carbon adsorption column.
（5）Iridoid powder, concentrate II are mixed with Lychee juice, dispensed after sterilizing, you can obtain anti-senile dementia Oral agents.
In the present embodiment, the recovery rate of iridoid glycoside is 22.1%, and purifying rate is 99.8%.

Claims (3)

1. a kind of anti-senile dementia oral agents, it is characterised in that compare component comprising following weight fraction：50 ~ 100 parts of Red Psychotria Leaf, 50 ~ 100 parts of Fructus Corni, 10 ~ 20 parts of barrenwort, 10 ~ 20 parts of dried orange peel, 5 ~ 10 parts of Chinese yam, 20 ~ 50 parts of hawthorn, 5 ~ 10 parts of lavender, 50 ~ 100 parts of Lychee juice；
It is prepared by following steps：
（1）50 ~ 100 parts of Red Psychotria Leaf is taken, is ground into the coarse powder of 10 ~ 20 mesh, adds water to cook 3 times, it is big that mountain is previously added in decoction liquor The mesoporous silicic acid calcium powder of face meal quality 20% ~ 30%, is filtered, merging filtrate respectively, and concentrated aqueous amount is 20% ~ 30%, is obtained Concentrate I；
（2）Concentrate I is taken, adds 10 ~ 15 times of purifying water enchroachment (invasion) bubble 30 ~ 60min, 2 ~ 3h of refluxing extraction, filtering, filter residue adds 6 ~ 8 times Purified water, by concentrate add 3 ~ 6mg/ml of cellulase, in constant-temperature heating magnetic stirring apparatus 45 ~ 55 DEG C of water enzyme digestions 2 ~ 3h, filter after enzymolysis, filter residue adds 6 ~ 8 times of amount purified waters, 1 ~ 1.5h of refluxing extraction, extract solution filtered through gauze, filtrate with 3000r/min centrifuges 20 ~ 30min, and by supernatant concentration, sample liquid is made；
（3）Sample liquid is taken, according to sample liquid：Mesoporous carbon=1g：（10~12g）It is static after mesoporous carbon adsorption column loading, loading to inhale Attached 1 ~ 2h, first being cleaned with 2 ~ 2.5BV distillation water elutions, then eluted with the ethanol solution of volume fraction 15% ~ 20%, flow velocity is 1 ~ 1.2BV/h, eluent is collected, concentrated, dried, you can obtain iridoid glycoside powder；
（4）Take 50 ~ 100 parts of Fructus Corni, 10 ~ 20 parts of barrenwort, 10 ~ 20 parts of dried orange peel, 5 ~ 10 parts of Chinese yam, 20 ~ 50 parts of hawthorn, smoke clothing 5 ~ 10 parts of grass, is crushed to 20 ~ 50 mesh, after mixing, adds water to cook 3 times, filter respectively, merging filtrate, is concentrated into water content as 30% ~50%；Obtain concentrate II；
（5）Iridoid powder, concentrate II are mixed for 50 ~ 100 parts with Lychee juice, dispensed after sterilizing, you can obtain anti-ageing year Dull-witted oral agents；
The mesoporous silicic acid calcium powder preparation method is as follows：
A. weigh 10 ~ 20 parts of four water-calcium nitrates to be dissolved into 80 ~ 100 parts of distilled water, being sufficiently stirred 1 ~ 2h makes calcium nitrate complete Dissolving, then adds 6 ~ 10 parts of template cetane trimethyl ammonium bromide, 20 ~ 30 parts of geniposide, at 45 ~ 55 DEG C with 120r/min speed stirs 1 ~ 1.5h, and white gels are gradually formed in whipping process；
B. according to Ca in four water-calcium nitrate and nine water sodium metasilicate：The amount ratio of Si materials is 1：1 weighs nine water sodium metasilicate, is dissolved in 40 In ~ 60 parts of distilled water, then this sodium silicate solution is slowly dropped in calcium nitrate solution, it is old at normal temperatures after reacting 4 ~ 5h Change 20 ~ 24h；Then distilled water washed product is used, then 22 ~ 24h is stripped with absolute ethyl alcohol, to remove template agent removing；By gained Product, which is placed in vacuum drying chamber at 40 DEG C, dries 12 ~ 14h, dried product is ground, you can obtain mesoporous calcium silicates Powder；
The mesoporous carbon absorption column preparation method is as follows：
A. 16 ~ 22 parts of poly- propoxyl group-polyethoxy-poly- propoxyl group triblock copolymers and 10 ~ 20 parts of 0.2mol/L hydrochloric acid are weighed Solution is mixed in 80 ~ 100 parts of ethanol, and 1h is stirred at 40 DEG C, sequentially adds 20 ~ 26 parts of tetraethyl orthosilicates and 40 ~ 50 parts of weights The phenolic resin ethanol solution of percentage 20% is measured, is evenly applied to after continuing 2 ~ 3h of stirring in culture dish, room temprature evaporation 7 ~ Culture 24h at 100 DEG C is placed in baking oven after 9h and obtains pale yellow transparent film；
B., transparent membrane is scraped to grinding from culture dish, in N2Under protection, it is placed in 800 ~ 900 DEG C of calcining 5h in tube furnace and just obtains To ordered mesopore carbon-silica composite；
C., the compound is impregnated in 10% 24 ~ 26h of hf etching, removes silicon components, then respectively with the body of 3 ~ 4 times of amounts The sodium hydrate aqueous solution of fraction 5%, distilled water, the acetic acid aqueous solution of volume fraction 10% of 3 ~ 4 times of amounts of 1 ~ 2 times of amount wash, most Neutrality is washed to distillation afterwards, wet method is fitted into chromatographic column, produces required mesoporous carbon adsorption column.
2. anti-senile dementia disease oral agents according to claim 1, it is characterised in that：Step（1）Decoction water for the first time PH is adjusted to as 1.0 ~ 2.0 using 1mol/L hydrochloric acid, amount of water is 10 ~ 12 times of medicinal material amount, and decocting time is 3.8 ~ 4.5h；Second Secondary decoction is adjusted to pH as 7.0 ~ 7.5 with water using saturation sodium hydroxide, and amount of water is 10 ~ 12 times of medicinal material medicinal material amount, decocting time For 1.8 ~ 2.4h；Third time decoction is adjusted to pH as 9.5 ~ 10.0 with water using saturation sodium hydroxide, and amount of water is the 8 ~ 10 of medicinal material amount Times, decocting time is 1.8 ~ 2.4h.
3. anti-senile dementia disease oral agents according to claim 1, it is characterised in that：Step（4）Decoction water for the first time PH is adjusted to as 2.0 ~ 3.0 using 1mol/L hydrochloric acid, amount of water is 12 ~ 16 times of medicinal material amount, and decocting time is 1.8 ~ 2.2h；Second Secondary decoction is adjusted to pH as 7.5 ~ 8.0 with water using saturation sodium hydroxide, and amount of water is 12 ~ 16 times of medicinal material medicinal material amount, decocting time For 0.8 ~ 1.2h；Third time decoction is adjusted to pH as 9.5 ~ 10.0 with water using saturation sodium hydroxide, and amount of water is the 10 ~ 14 of medicinal material amount Times, decocting time is 0.8 ~ 1.2h.
CN201711089866.4A 2017-11-08 2017-11-08 A kind of anti-senile dementia disease oral agents Withdrawn CN107669865A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3106754A1 (en) * 2020-02-04 2021-08-06 Isp Investments Llc PROCESS FOR OBTAINING AN AQUEOUS LAVENDER EXTRACT, COMPOSITIONS INCLUDING SUCH EXTRACT AND THEIR COSMETIC USES

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3106754A1 (en) * 2020-02-04 2021-08-06 Isp Investments Llc PROCESS FOR OBTAINING AN AQUEOUS LAVENDER EXTRACT, COMPOSITIONS INCLUDING SUCH EXTRACT AND THEIR COSMETIC USES
WO2021156104A1 (en) * 2020-02-04 2021-08-12 ISP Investments LLC. Method for obtaining an aqueous extract of lavender, compositions comprising such an extract and their cosmetic uses
CN115135301A (en) * 2020-02-04 2022-09-30 Isp投资有限责任公司 Method for obtaining an aqueous extract of lavender, composition comprising such an extract and cosmetic use thereof

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