CN109172769A - A kind of Sessileflower Acanthopanax Bark compound and preparation method thereof - Google Patents
A kind of Sessileflower Acanthopanax Bark compound and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of using classification ultrafiltration, pulverizes the Sessileflower Acanthopanax Bark compound of method for combined use preparation, it belongs to traditional Chinese medicine and field of food industry.A kind of Sessileflower Acanthopanax Bark compound, it is mainly prepared by following raw materials by the parts by weight: 10-20 parts of Sessileflower Acanthopanax Bark, 7-8 parts of dried orange peel, 4-8 parts of mulberry fruit, 1-2 parts of fructus alpiniae oxyphyllae.Sessileflower Acanthopanax Bark compound of the present invention, it is raw material that it, which selects the Chinese medicine of positive, nourishing kidney-yin the integration of drinking and medicinal herbs of kidney tonifying gas, warm kidney, has the function of nourishing liver and kidney, regulating qi-flowing for strengthening spleen, warm kidney controlling nocturnal emission with astringent drugs, relieves fatigue, can be prepared into series beverage, safely and effectively, without any toxicity and side effects.Preparation method of the invention, it prepares Sessileflower Acanthopanax Bark complex composition using classification ultrafiltration, ultramicro grinding joint technology, it destroys raw material cell wall using classification ultrafiltration, ultramicro grinding and effective component in cell is precipitated, effective component structure will not be damaged simultaneously, Sessileflower Acanthopanax Bark compound combination ultra-micro powder obtained is set to play curative effect, the antifatigue significant effect of kidney tonifying quickly.
Description
Technical field
The present invention relates to a kind of using classification ultrafiltration, pulverizes the Sessileflower Acanthopanax Bark compound of method for combined use preparation,
It belongs to traditional Chinese medicine and field of food industry.
Background technique
Modern medicine thinks that kidney is the vitals of human body, its basic function is to generate urine, internal so as to removing
Metabolite and certain wastes, poisonous substance, while retaining moisture content and other utilities through reabsorption function, such as glucose, albumen
Matter, amino acid, sodium ion, potassium ion, sodium bicarbonate etc., to adjust water, electrolyte balance and maintenance acid-base balance.Kidney is simultaneously
There are also endocrine functions, generate feritin, hematopoietin, activity of vitamin d3, prostaglandin, kassinin kinin etc., and are body
The target organ in the degradation place and kidney pheromone of part endocrine hormone.These functions of kidney, ensure that organismic internal environment
Stablize, metabolism is enable to be normally carried out.
Seen in Chinese medicine angle, the main Physiological Function of kidney be store essential substances, main water, it is main receive gas, main reproduction, this and doctor trained in Western medicine viewpoint
It is consistent with.Since kidney keeps congenital essence, it is the internal organs yin-yang source of this and growth in humans, development, reproduction, is raw
Life activity is basic, referred to as " the congenital foundation ".
Whether kidney qi waxing and waning response kidney and its relevant tissue health, it is weak that also to represent vitality, which be prosperous,.Kidney yin and kidney
Positive common adjusting controls the viscera function activity of human body and the metabolic process of essence and blood body fluid.Kidney deficiency is mostly long-term accumulation into disease,
The qi-blood circulating or function and kidney for covering kidney and kidney channel generate associated organ-tissue --- and uropoiesis, reproductive system etc. are asked
Topic.Kidney qi is weak, hypofunction, and the dereliction of duty of Feng Zanggu camera shooting function can further cause the pathological change of imbalance of yin and yang.Kidney deficiency can't
It is nourished, or the tonifying kidney and strengthening yang drug unknown with composition, and should be slowly improved with the medicine of big benefit due to anxious for success, reached with it
New balance restores health.
Traditional Chinese medicine belongs to the food or drug of different colours the five internal organs of human body, red enters the heart, cyan enters liver,
Yellow enters spleen, white enters lung, black enters kidney.Black food is referred to as kidney-tonifying health-care agent, typically contain microelement abundant and
Vitamin has certain nourishing and care, the Chinese medicine of especially some integration of drinking and medicinal herbs to kidney.
Chemical composition of Chinese materia medica is complicated, and traditional is used as medicine mode based on decocting, decoction process along with a large amount of ingredients from lossing,
And medicinal ingredient cannot be precipitated completely, and the process time is long, and energy consumption is high.With modern medicine and pharmacology development in science and technology, with tradition
Experience extractive technique have been unable to meet the needs of prophylactic treatment, and effective component of chinese medicine is typically distributed on cell wall and is wrapped in
Cell interior, to improve the recovery rate of target product and make full use of resource, need to take effective ways destroy its cell wall and
Effective component in cell is precipitated, while too big destruction will not be caused to effective component structure, it is seen that effective component of chinese medicine
It extracts more and more important.
Summary of the invention
In view of the deficienciess of the prior art, an object of the present invention is to provide a kind of Sessileflower Acanthopanax Bark that kidney tonifying is antifatigue
Compound, it is raw material that it, which selects the Chinese medicine of positive, nourishing kidney-yin the integration of drinking and medicinal herbs of kidney tonifying gas, warm kidney, has nourishing liver and kidney, reason
Gas invigorating the spleen, warm kidney controlling nocturnal emission with astringent drugs, the effect relieved fatigue, can be prepared into series beverage, safely and effectively, without any toxicity and side effects.
It is a further object of the present invention to provide the preparation methods of above-mentioned Sessileflower Acanthopanax Bark compound, it is super using classification
Filter, ultramicro grinding method for combined use prepare Sessileflower Acanthopanax Bark complex composition, it destroys raw cell using classification ultrafiltration, ultramicro grinding
Wall and effective component is precipitated, while effective component structure will not be damaged, make Sessileflower Acanthopanax Bark compound obtained
Combination ultra-micro powder can play curative effect quickly.
To achieve the goals above, the present invention is to provide following technical solution:
A kind of Sessileflower Acanthopanax Bark compound, it is mainly prepared by following raw materials by the parts by weight: short stalk
10-20 parts of slender acanthopanax, 7-8 parts of dried orange peel, 4-8 parts of mulberry fruit, 1-2 parts of fructus alpiniae oxyphyllae.
A kind of above-mentioned Sessileflower Acanthopanax Bark compound, it mainly by following raw materials by the parts by weight prepare and
At: 15 parts of Sessileflower Acanthopanax Bark, 7.5 parts of dried orange peel, 6 parts of mulberry fruit, 1.5 parts of fructus alpiniae oxyphyllae.
The preparation method of above-mentioned Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) Sessileflower Acanthopanax Bark for meeting the parts by weight, dried orange peel, mulberries, fructus alpiniae oxyphyllae are weighed, through co-grinding to 10-40
It is spare to obtain thick medicinal powder for mesh；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 18-22 times of thick medicinal powder weight, and it is small to impregnate 0.5-1.5
When, 0.35-0.55 parts by weight pectase is added, citric acid tune pH value is 3.0-5.0, the constant temperature enzyme in 30 DEG C of -50 DEG C of enzymatic hydrolysis pots
Solution 1-3 hours, after enzymatic hydrolysis, is warming up to 93-97 DEG C of enzyme deactivation；
(3) after enzyme deactivation, after enzymatic treatment system is boiled, filtrate is collected in slightly boiled decoction 1-3 hours, filtration；Second of filter residue
Amount of water is 18-22 times of thick medicinal powder weight, and after boiling, filtrate is collected in slightly boiled decoction 1-3 hours, filtration；Filter residue third time adds
Water is 18-22 times of thick medicinal powder weight, and after boiling, filtrate is collected in slightly boiled decoction 0.5-1.5 hours, filtration；
(4) the resulting filtrate three times of step (3) is merged, 4000-6000r/min is centrifuged 10-20min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) by step (5) resulting ultrafiltrate, under the conditions of 40-50 DEG C, relative molecular mass 300- is retained using film
600Da carries out nanofiltration concentration, and the volume of the concentrated liquid is the 1/4-3/4 of stoste volume, obtains concentrate；
(7) it to the maltodextrin of 0.2-0.4 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly
After be spray-dried, spray drying condition is as follows: 110-130 DEG C of inlet air temperature, 80-100 DEG C of leaving air temp, atomizing pressure
750-850Pa, hydrojet speed 8-12%, obtains dried powder；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 5-15min of tank, makes the average grain diameter of Ultramicro-powder reach 900-1500nm to get Sessileflower Acanthopanax Bark compound
Combine ultra-micro powder.
20 mesh are crushed to after the mixing of above-mentioned steps (1) raw material.
First time amount of water is preferably 20 times of thick medicinal powder weight in above-mentioned steps (2), and soaking time preferably 1 hour, fruit
Glue enzyme additional amount preferably 0.45 parts by weight, pH value is preferably 4.0, preferably 40 DEG C of hydrolysis temperature, enzymolysis time preferably 2 hours, is gone out
Preferably 95 DEG C of enzyme temperature.
Enzymatic hydrolysis decocting time is preferably 2 hours in above-mentioned steps (3)；Second of amount of water is preferably the 20 of thick medicinal powder weight
Times, decocting time is preferably 2 hours；Third time amount of water is preferably 20 times of thick medicinal powder weight, and decocting time is preferably 1 small
When.
Centrifugation rate is preferably 5000r/min in above-mentioned steps (4), and centrifugation time is preferably 15min.
Nanofiltration temperature is preferably 45 DEG C in above-mentioned steps (6), and retaining molecular weight is preferably 450Da.
The additive amount of maltodextrin is preferably 0.3 times of concentrate weight in above-mentioned steps (7)；Spray drying EAT
It is preferred that 120 DEG C, preferably 90 DEG C of leaving air temp, the preferred 800Pa of atomizing pressure, hydrojet speed preferably 10%.
Impacting time preferred 10min in above-mentioned steps (8), the average grain diameter of Ultramicro-powder are 1200nm.
Due to the adoption of the above technical scheme, so that compared with prior art, the present invention having following features and effect:
It is as follows the effect of Chinese medicine material used in the present invention: Sessileflower Acanthopanax Bark: Ji Yuan: Araliaceae wilsonii and Panax sessiliflorus
Root skin；Nature and flavor: pungent, bitter, micro-sweet；Temperature；Channel tropism: enter liver and kidney channel.Major function: wind-damp dispelling, nourishing liver and kidney, strengthening the bones and muscles, promoting blood circulation
Arteries and veins；It is used for treating arthralgia due to cold and dampness, lumbocrural pain, muscles and bones impotence, the retardation of walking of decimal a little, physically weak frail, bruise wound, fracture, oedema, foot
Gas, uncontrolled urination.Dried orange peel: Ji Yuan: rutaceae orange and its dry mature skin of variety；Nature and flavor: bitter, acrid in flavour and warm in nature；Return
Through: enter lung, the spleen channel.Major function: regulating qi-flowing for strengthening spleen, eliminating dampness and eliminating phlegm；For abdominal fullness and distention, deficiency of food is vomited and diarrhoea, coughing with a lot of sputum.Mulberry fruit:
The drying fruit ear of moraceae plants mulberry；Nature and flavor: it is sweet, sour, it trembles with fear；Channel tropism: enter the heart, liver and kidney channel.Major function: enriching yin of enriching blood, profit of promoting the production of body fluid
It is dry；For dizziness and tinnitus, palpitation and insomnia, poliosis, injury thirst, Heat Diabetes, blood deficiency and constipation.Fructus alpiniae oxyphyllae: Ji Yuan: Zingiber
The fruit of plant intelligence development；Nature and flavor: acrid in flavour and warm in nature；Channel tropism: enter spleen, kidney channel；Major function: warming spleen and stopping diarrha take the photograph saliva, kidney reducing urination controlling nocturnal emission with astringent drugs is warmed up；
For it is cold in deficiency-cold in spleen and stomach, vomiting, diarrhea, abdomen educate, the more salivas of mouth, enuresis with renal asthenia, frequent micturition, spermatorrhea, gonorrhoea.
The antifatigue Sessileflower Acanthopanax Bark compound combination of kidney tonifying of the present invention Chinese medicine used, is selected in national integration of drinking and medicinal herbs catalogue
Medicinal material is raw material, based on TCM theory, adheres to the theory of TCM preventiveed treatment of disease, and is that principle carries out prescription, symbol by monarch
It closes the five colors and enters the five internal organs theory of traditional Chinese medical science, the proportion of strict control each component has nourishing liver and kidney, regulating qi-flowing for strengthening spleen, warm kidney controlling nocturnal emission with astringent drugs, alleviates
The effect of fatigue, kidney qi benefit are supplemented nutrition, and organism metabolism circulation is smooth, and the invasive ability of exopathogen is defendd to improve, and body recovery is cured
Ability enhancing carries out daily conditioning and maintenance to human kidney, complies with kidney characteristic and variation carries out correspondingly prevention and conditioning.
Above-mentioned Sessileflower Acanthopanax Bark, dried orange peel, mulberry fruit and fructus alpiniae oxyphyllae are combined by the present invention by the dosage, so that each raw material generates collaboration and increases
Effect acts on, and using slender acanthopanax polysaccharide in Sessileflower Acanthopanax Bark as index ingredient in compound, content is mentioned in the more single Sessileflower Acanthopanax Bark of content
It has risen twice.Body system's organ is closely coupled, and single raw material covering surface is limited, and monarch, which is mutually arranged in pairs or groups, facilitates compound hair
Wave ultimate attainment effect.Using Sessileflower Acanthopanax Bark as monarch drug in a prescription, dried orange peel, mulberry fruit, fructus alpiniae oxyphyllae have nourishing and push each internal organs function as minister adjutant
Can, deficiency of kidney-essence is filled up, spleen transporting is warmed up, helps pulmonary aspiration, adjusts internal aqueous balance.Organism balance, biochemical active, function operating
Restore fast, energetic, bone is firm strong, relieves fatigue sense out of strength, prevents senilism early ageing, decreased energy.
Present invention application classification ultrafiltration, ultramicro grinding method for combined use prepare Sessileflower Acanthopanax Bark compound, by traditional Chinese medicine
Extraction process is combined with modern biotechnology technique, retains the extracting mode of traditional water decoction decoction, utilizes enzymatic hydrolysis pre-treatment work
Protein, cellulose, pectic substance etc. on cell wall is hindered the main barrier of effective component dissolution intracellular to degrade by skill, to make
Cell wall is loose, ruptures, and reduces diffusion of active ingredient resistance intracellular, improves recovery rate.
The present invention is for raw material sources, predominantly fruit class in composition, so can effectively hydrolyze destruction using pectase
The pectic substance ingredient of fruit cell wall reduces viscosity, retains the functional components of raw material in compound in a higher degree.Enzymatic hydrolysis temperature
Degree has important influence to enzymolysis efficiency and active principle recovery rate, to protect polysaccharide component in fruit not to be destroyed, starting temperature
Degree be set as 30 DEG C, as hydrolysis temperature gradually rises, enzymolysis efficiency and recovery rate are quickly increased, when temperature be increased to 40 DEG C by
Gradually stable, enzymatic hydrolysis preference temperature is 30 DEG C -50 DEG C, and best hydrolysis temperature is 40 DEG C.Because fruit class contains there are many phenolic acid substance,
With the similar principle to mix, enzymatic hydrolysis appropriate pH is 3.0-5.0, and the best pH that digests is 4.0.Enzymolysis time is unsuitable too long, through investigating,
Between 1-3 hours, Best Times are 2 hours.It is inadequate to the natural barrier destructive power of cell when enzyme dosage is less, with
Enzyme dosage when gradually increasing, the dissolution of active principle can be increased, when position reaches saturation state, enzyme dosage is in 0.35-
When within the scope of 0.55 parts by weight, recovery rate reaches balance.After enzymatic hydrolysis parameter optimization, slender acanthopanax polysaccharide index content is more traditional to be mentioned
Method is taken to be promoted twice.Using macromoleculars inert substances such as starch, protein in biological hyperfiltration technique removal aqueous extract, simultaneously
Loss of effective components is reduced, the filtration water removal of nanofiltration biotechnology is recycled, it is active constituent-enriched, while can in concentrated extracting solution
Thermophilic digestion feed liquid is avoided, effective component retention rate is improved, reduces heat energy loss.Obtained Ultramicro-powder is after water dissolves, liquid
Clear, no residue deposited phenomenon.The present invention is not introduced into organic solvent and chemical reagent, does not break in preparation process simultaneously
Bad medicinal material internal component structure protects character of medicinal material, preferably performance health care curative effect.
The antifatigue Sessileflower Acanthopanax Bark compound of kidney tonifying of the present invention can be used for preparing alternative tea.
Present invention application classification ultrafiltration, ultramicro grinding method for combined use prepare Sessileflower Acanthopanax Bark compound, through being prepared
Ultramicro-powder can be used for preparing Sessileflower Acanthopanax Bark compound combined beverage series of products.
Present invention application classification ultrafiltration, pulverizing method for combined use, to prepare Sessileflower Acanthopanax Bark compound antifatigue in kidney tonifying
The effect of aspect is preferable, supplements human body kidney qi, takes into account conscience spleen and lung fortune function, body tolerance enhancing, and resume speed is promoted,
Internal organs qi-blood circulating is orderly, in health problems such as balances in conditioning human body.Selected materials are all integration of drinking and medicinal herbs Chinese medicine, and raw material is easy
, the pharmacological property of natural herbs is taken, without any side effects, body liver kidney burden and the economy that can reduce user are negative
Load.The method of the present invention prepares Sessileflower Acanthopanax Bark compound, full of vitality after taking orally, and activity increases, and body recovery is very fast.It is logical
Pharmacokinetics Observation is crossed, Sessileflower Acanthopanax Bark polyoses content peak time is shorter in rat blood, and peak is reached within 0.5 hour
It is very fast to illustrate that body absorbs for value.And content is higher in kidney, and retention time is longer in vivo, can effectively be inhaled by body
Receive metabolism.
Preparation method of the invention, medicinal ingredient is precipitated completely in it, and low energy consumption, it is using classification ultrafiltration, ultramicro grinding
It destroys raw material cell wall and effective component in cell is precipitated, while effective component structure will not be damaged, made obtained
Sessileflower Acanthopanax Bark compound combination ultra-micro powder can play curative effect quickly.
Specific embodiment
Below with reference to embodiment, the present invention is described further.Following embodiment is only several specific realities of the invention
Example is applied, but the design concept of the present invention is not limited to this, it is all to be made a non-material change to the present invention using this design,
It should belong to the behavior for invading the scope of the present invention.
Method in following embodiments is unless otherwise instructed conventional method.
Percentage composition in following embodiments is unless otherwise instructed mass percentage.
Number in following embodiments is parts by weight.
Embodiment 1
A kind of Sessileflower Acanthopanax Bark compound, it is to be prepared by following raw materials by the parts by weight: Sessileflower Acanthopanax Bark
10 parts, 8 parts of dried orange peel, 8 parts of mulberry fruit, 2 parts of fructus alpiniae oxyphyllae.
The preparation method of Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) 10 parts by weight Sessileflower Acanthopanax Barks, 8 parts by weight dried orange peels, 8 parts by weight mulberry fruits, 2 parts by weight fructus alpiniae oxyphyllaes are weighed, through mixing
10 mesh are crushed to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 18 times of thick medicinal powder weight, is impregnated 0.5 hour, is added
0.35 parts by weight pectase, citric acid tune pH value are 3.0, and constant temperature digests 1 hour in 30 DEG C of enzymatic hydrolysis pots, after enzymatic hydrolysis, are risen
Temperature is to 93 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 1 hour, filtrate is collected in filtration；Filter residue adds water for the second time
Amount is 18 times of thick medicinal powder weight, slightly boiled to decoct 1 hour after boiling, and filtrate is collected in filtration；Filter residue third time amount of water is thick
18 times of medicinal powder weight, slightly boiled to decoct 0.5 hour after boiling, filtrate is collected in filtration；
(4) the resulting filtrate three times of step (3) is merged, 4000r/min is centrifuged 10min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) it by step (5) resulting ultrafiltrate, under the conditions of 40 DEG C, is carried out using film retention relative molecular mass 300Da
Nanofiltration concentration, the volume of the concentrated liquid are the 1/4 of stoste volume, obtain concentrate；
(7) it to the maltodextrin of 0.2 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, obtains dried powder；Spray drying condition is as follows: 110 DEG C of inlet air temperature, 80 DEG C of leaving air temp, and atomizing pressure
750Pa, hydrojet speed 8%；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 5min of tank makes the average grain diameter of Ultramicro-powder reach 900nm and combines ultra micro to get Sessileflower Acanthopanax Bark compound
Powder.
Embodiment 2
A kind of Sessileflower Acanthopanax Bark compound, it is to be prepared by following raw materials by the parts by weight: Sessileflower Acanthopanax Bark
12 parts, 7.7 parts of dried orange peel, 7 parts of mulberry fruit, 1.8 parts of fructus alpiniae oxyphyllae.
The preparation method of Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) 12 parts by weight Sessileflower Acanthopanax Barks, 7.7 parts by weight dried orange peels, 7 parts by weight mulberry fruits, 1.8 parts by weight fructus alpiniae oxyphyllaes are weighed, are passed through
It carries out being crushed to 16 mesh after mixing, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 19 times of thick medicinal powder weight, is impregnated 0.8 hour, is added
0.4 parts by weight pectase, citric acid tune pH value are 3.5, and constant temperature digests 1.5 hours in 35 DEG C of enzymatic hydrolysis pots, after enzymatic hydrolysis, are risen
Temperature is to 94 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 1.5 hours, filtrate is collected in filtration；Filter residue adds for the second time
Water is 19 times of thick medicinal powder weight, slightly boiled to decoct 1.5 hours after boiling, and filtrate is collected in filtration；Filter residue third time amount of water
It is 19 times of thick medicinal powder weight, after boiling, slightly boiled to decoct 0.8 hour, filtrate is collected in filtration；
(4) the resulting filtrate three times of step (3) is merged, 4500r/min is centrifuged 12min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) it by step (5) resulting ultrafiltrate, under the conditions of 43 DEG C, is carried out using film retention relative molecular mass 400Da
Nanofiltration concentration, the volume of the concentrated liquid are the 1/4 of stoste volume, obtain concentrate；
(7) it to the maltodextrin of 0.25 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, obtains dried powder；Spray drying condition is as follows: 115 DEG C of inlet air temperature, 85 DEG C of leaving air temp, and atomizing pressure
780Pa, hydrojet speed 9%；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 8min of tank makes the average grain diameter of Ultramicro-powder reach 1000nm super to get the combination of Sessileflower Acanthopanax Bark compound
Micropowder.
Embodiment 3
A kind of Sessileflower Acanthopanax Bark compound, it is to be prepared by following raw materials by the parts by weight: Sessileflower Acanthopanax Bark
15 parts, 7.5 parts of dried orange peel, 6 parts of mulberry fruit, 1.5 parts of fructus alpiniae oxyphyllae.
The preparation method of Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) 15 parts by weight Sessileflower Acanthopanax Barks, 7.5 parts by weight dried orange peels, 6 parts by weight mulberry fruits, 1.5 parts by weight fructus alpiniae oxyphyllaes are weighed, are passed through
It carries out being crushed to 20 mesh after mixing, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 20 times of thick medicinal powder weight, is impregnated 1 hour, is added
0.45 parts by weight pectase, citric acid tune pH value are 4.0, and constant temperature digests 2 hours in 40 DEG C of enzymatic hydrolysis pots, after enzymatic hydrolysis, are risen
Temperature is to 95 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 2 hours, filtrate is collected in filtration；Filter residue adds water for the second time
Amount is 20 times of thick medicinal powder weight, slightly boiled to decoct 2 hours after boiling, and filtrate is collected in filtration；Filter residue third time amount of water is thick
20 times of medicinal powder weight, slightly boiled to decoct 1 hour after boiling, filtrate is collected in filtration；
(4) the resulting filtrate three times of step (3) is merged, 5000r/min is centrifuged 15min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) it by step (5) resulting ultrafiltrate, under the conditions of 45 DEG C, is carried out using film retention relative molecular mass 450Da
Nanofiltration concentration, the volume of the concentrated liquid are the 1/2 of stoste volume, obtain concentrate；
(7) it to the maltodextrin of 0.3 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, obtains dried powder；Spray drying condition is as follows: 120 DEG C of inlet air temperature, 90 DEG C of leaving air temp, and atomizing pressure
800Pa, hydrojet speed 10%；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 10min of tank makes the average grain diameter of Ultramicro-powder reach 1200nm super to get the combination of Sessileflower Acanthopanax Bark compound
Micropowder.
Embodiment 4
A kind of Sessileflower Acanthopanax Bark compound, it is to be prepared by following raw materials by the parts by weight: Sessileflower Acanthopanax Bark
18 parts, 7.3 parts of dried orange peel, 5 parts of mulberry fruit, 1.2 parts of fructus alpiniae oxyphyllae.
The preparation method of Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) 18 parts by weight Sessileflower Acanthopanax Barks, 7.3 parts by weight dried orange peels, 5 parts by weight mulberry fruits, 1.2 parts by weight fructus alpiniae oxyphyllaes are weighed, are passed through
It is spare to obtain thick medicinal powder to 30 mesh for co-grinding；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 21 times of thick medicinal powder weight, is impregnated 1.2 hours, is added
0.5 parts by weight pectase, citric acid tune pH value are 4.5, and constant temperature digests 2.5 hours in 45 DEG C of enzymatic hydrolysis pots, after enzymatic hydrolysis, are risen
Temperature is to 96 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 2.5 hours, filtrate is collected in filtration；Filter residue adds for the second time
Water is 21 times of thick medicinal powder weight, slightly boiled to decoct 2.5 hours after boiling, and filtrate is collected in filtration；Filter residue third time amount of water
It is 21 times of thick medicinal powder weight, after boiling, slightly boiled to decoct 1.2 hours, filtrate is collected in filtration；
(4) the resulting filtrate three times of step (3) is merged, 5500r/min is centrifuged 17min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) it by step (5) resulting ultrafiltrate, under the conditions of 47 DEG C, is carried out using film retention relative molecular mass 500Da
Nanofiltration concentration, the volume of the concentrated liquid are the 3/4 of stoste volume, obtain concentrate；
(7) it to the maltodextrin of 0.35 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, obtains dried powder；Spray drying condition is as follows: 125 DEG C of inlet air temperature, 95 DEG C of leaving air temp, and atomizing pressure
830Pa, hydrojet speed 11%；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 12min of tank makes the average grain diameter of Ultramicro-powder reach 1300nm super to get the combination of Sessileflower Acanthopanax Bark compound
Micropowder.
Embodiment 5
A kind of Sessileflower Acanthopanax Bark compound, it is mainly prepared by following raw materials by the parts by weight: short stalk
20 parts of slender acanthopanax, 7 parts of dried orange peel, 4 parts of mulberry fruit, 1 part of fructus alpiniae oxyphyllae.
The preparation method of Sessileflower Acanthopanax Bark compound, steps are as follows:
(1) 20 parts by weight Sessileflower Acanthopanax Barks, 7 parts by weight dried orange peels, 4 parts by weight mulberry fruits, 1 parts by weight fructus alpiniae oxyphyllae are weighed, through mixing
40 mesh are crushed to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 22 times of thick medicinal powder weight, is impregnated 1.5 hours, is added
0.55 parts by weight pectase, citric acid tune pH value are 5.0, and constant temperature digests 3 hours in 50 DEG C of enzymatic hydrolysis pots, after enzymatic hydrolysis, are risen
Temperature is to 97 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 3 hours, filtrate is collected in filtration；Filter residue adds water for the second time
Amount is 22 times of thick medicinal powder weight, slightly boiled to decoct 3 hours after boiling, and filtrate is collected in filtration；Filter residue third time amount of water is thick
22 times of medicinal powder weight, slightly boiled to decoct 1.5 hours after boiling, filtrate is collected in filtration；
(4) the resulting filtrate three times of step (3) is merged, 6000r/min is centrifuged 20min, collects supernatant；
(5) it is super by molecular weight 300K, 100K, 10K doughnut that retention is respectively adopted in the supernatant for collecting step (4)
Filter column carries out ultrafiltration, collects ultrafiltrate；
(6) it by step (5) resulting ultrafiltrate, under the conditions of 50 DEG C, is carried out using film retention relative molecular mass 600Da
Nanofiltration concentration, the volume of the concentrated liquid are the 3/4 of stoste volume, obtain concentrate；
(7) it to the maltodextrin of 0.4 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, obtains dried powder；Spray drying condition is as follows: 130 DEG C of inlet air temperature, 100 DEG C of leaving air temp, and atomizing pressure
850Pa, hydrojet speed 12%；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding
The intracorporal mill Jie impacting 15min of tank makes the average grain diameter of Ultramicro-powder reach 1500nm super to get the combination of Sessileflower Acanthopanax Bark compound
Micropowder.
Thick medicinal powder obtained by step (1) can be applied to prepare Sessileflower Acanthopanax Bark compound alternative tea in embodiment 1,2,3,4,5.
It is multiple to can be used for Sessileflower Acanthopanax Bark for the combination of Sessileflower Acanthopanax Bark compound obtained by step (8) ultra-micro powder in embodiment 1,2,3,4,5
Square combined beverage series of products.
Test example 1
1,2,3,4,5 method of the embodiment of the present invention preparation Sessileflower Acanthopanax Bark compound combination ultra-micro powder ingredient detection with contain
Analysis method and result are as follows:
(1) prepared by reference substance solution: precision weighs that glucose control product are appropriate, and it is the molten of 0.2mg/mL that concentration, which is made, with water
Liquid is to get reference substance solution.
(2) Specification Curve of Increasing: precision draws reference substance solution 0,0.2,0.5,1,1.5,2.0mL, is placed in 6 10mL tools
It fills in scale test tube, adds water polishing to 2mL, each 1mL of 5% phenol solution is added, shakes up, adds each 5mL of the concentrated sulfuric acid, shake rapidly
It is even, cooling is stood, 20min is heated in 40 DEG C of water-baths and carries out chromogenic reaction, is taken out immediately after reaction, flowing is water-cooled to
Room temperature measures absorbance at 490nm wavelength.Using glucose quality as abscissa, absorbance is ordinate, and it is bent to draw standard
Line.
(3) test sample preparation is with measurement: the Sessileflower Acanthopanax Bark compound that precision weighs the preparation of 1,2,3,4,5 methods combines Ultramicro-powder
Last 1.0g, is respectively placed in stuffed conical flask, and 80% ethyl alcohol 100mL, the ultrasound 30min at 40-50 DEG C, in residue is added
After ethyl alcohol volatilizes, add water 100mL, at 40-50 DEG C, ultrasonic extraction 3 times, each 30min, filtration, merging filtrate, then constant volume in
In 50mL measuring bottle, as test solution.By standard curve preparation manipulation step, absorbance is measured at 490nm wavelength, is calculated
Sessileflower Acanthopanax Bark compound polyoses content.
The preparation of Sessileflower Acanthopanax Bark simple: precision weighs Sessileflower Acanthopanax Bark, extracts by 3 extracting method of embodiment, molten by test sample
Liquid method is prepared to get Sessileflower Acanthopanax Bark single drug solns.
Traditional water decoction agent group sample preparation: weighing 15 parts of Sessileflower Acanthopanax Bark in 3 step of embodiment (1) ratio, and 7.5 parts of dried orange peel,
It 6 parts of mulberry fruit, 1.5 parts of fructus alpiniae oxyphyllae, carries out being crushed to 20 mesh after mixing.First time amount of water is 20 times of medicinal material amount, and it is small to impregnate 1
When, slightly boiled to decoct 2 hours, filtrate is collected in filtration；Second of amount of water of filter residue is 20 times of medicinal material amount, after boiling, slightly boiled decoction
2 hours, filtrate was collected in filtration；Filter residue third time amount of water is 20 times of medicinal material amount, slightly boiled to decoct 1 hour after boiling, filtration,
Collect filtrate.Filtrate, moisture volatilize three times for merging.Precision weighs 1.0g medicinal extract, prepares by test solution method to get tradition
Water decoction group sample solution.
(4) experimental result
1 reference substance content of table and absorbance value
| Reference substance/mg | 0.04 | 0.1 | 0.2 | 0.3 | 0.4 |
| Light absorption value | 0.106 | 0.183 | 0.279 | 0.399 | 0.468 |
Calibration curve equation is Y=1.0174X+0.0754, coefficient R=0.9962
The comparison of 2 polysaccharide component assay of table
| Grouping | Polyoses content % |
| Example 1 group | 19.89 |
| 2 groups of embodiment | 23.42 |
| 3 groups of embodiment | 30.74 |
| 4 groups of embodiment | 28.03 |
| 5 groups of embodiment | 25.94 |
| Sessileflower Acanthopanax Bark simple group | 9.69 |
| Traditional water decoction agent group | 9.22 |
The comparison of 3 nutrient component determining of table
Test example 2
The Sessileflower Acanthopanax Bark compound combination ultra-micro powder of 1,2,3,4,5 method of embodiment of the present invention preparation for resist oxygen lack and resists
Tired animal model test.
1, mouse resist oxygen lack is influenced
(1) by 80 mouse, weight 18-20g, half male and half female is randomly divided into 10 groups: blank control group, embodiment 1,2,
3,4,5 groups, Sessileflower Acanthopanax Bark simple group and traditional water decoction agent group.Each embodiment group, Sessileflower Acanthopanax Bark simple group and traditional water decoction
Agent group dosage is 599.33mg/kg, stomach-filling volume 0.25mL/kg.Blank control group gives the distilled water of equal capacity, daily
1 time, for three days on end.
(2) observation index: after last dose 45min, mouse is set in batch same specification 250mL ground stuffed conical flask
(the built-in fresh soda lime of fixed weight is with absorbing carbon dioxide and water), bottleneck water shutoff is to check that gas leakage starts timing, until small
Mouse death by suffocation, as hypoxia endurance time.
(3) experimental result
Influence of 4 each group of table to mouse hypoxia endurance time
| Grouping | Hypoxia endurance time (s) |
| Blank control group | 15.32±5.20 |
| Example 1 group | 31.31±6.87★★△# |
| 2 groups of embodiment | 34.42±7.73★★△# |
| 3 groups of embodiment | 42.94±10.23★★△△## |
| 4 groups of embodiment | 38.54±7.69★★△△## |
| 5 groups of embodiment | 32.91±8.49★★△# |
| Sessileflower Acanthopanax Bark simple group | 24.25±8.67★ |
| Traditional water decoction agent group | 22.62±6.79★ |
Note: compared with blank control group,★P < 0.05,★★P<0.01
Compared with Sessileflower Acanthopanax Bark simple group,△P < 0.05,△△P<0.01
Compared with traditional water decoction agent group,#P < 0.05,##P<0.01
As seen from the above table, compared with blank control group, each embodiment group of Sessileflower Acanthopanax Bark can significantly extend the normal pressure of mouse
The resist oxygen lack time-to-live has improvement result to cerebral anoxia or myocardial ischemia, and effect is better than Sessileflower Acanthopanax Bark simple group and tradition
Water decoction group, wherein 3 groups of mouse Hypoxia under normal pressure longests of embodiment.
2, to the influence of mouse physical fatigue
(1) by 80 mouse, weight 18-20g is randomly divided into 10 groups, i.e. blank control group, 1,2,3,4,5 group of embodiment,
Sessileflower Acanthopanax Bark simple group and traditional water decoction agent group.Dosage is tested with resist oxygen lack, stomach-filling volume 0.25mL/kg.Blank pair
The distilled water of equal capacity, one time a day, continuous 7 days are given according to group.
(2) after last dose 60min, groups of animals observation index: is respectively placed in the trip of 25 DEG C of water temperature, depth of water 30cm
In swimming case.Do not refloat after sinking under water 6s to mouse and exhaust death standard as power, record from swimming to death time, work
For mouse swimming time.
(3) experimental result
Influence of 5 each group of table to mouse swimming time
| Grouping | Weight (g) before being administered | Weight (g) after administration | Swimming time (s) |
| Blank control group | 18.10±1.20 | 25.09±2.94 | 99.85±41.83 |
| Example 1 group | 18.19±1.29 | 22.45±2.71 | 159.64±68.75★★△# |
| 3 groups of embodiment | 18.15±1.13 | 23.01±3.21 | 162.79±71.06★★△# |
| 4 groups of embodiment | 18.25±1.23 | 23.28±1.75 | 224.86±90.43★★△△## |
| 6 groups of embodiment | 18.09±1.49 | 22.99±2.64 | 177.44±73.88★★△△## |
| 7 groups of embodiment | 18.12±1.43 | 22.53±3.12 | 159.63±65.47★★△# |
| Sessileflower Acanthopanax Bark simple group | 18.14±1.11 | 22.34±2.36 | 128.20±60.57★ |
| Traditional water decoction agent group | 18.12±1.17 | 22.18±3.09 | 121.63±59.72★ |
Note: compared with blank control group,★P < 0.05,★★P<0.01
Compared with Sessileflower Acanthopanax Bark simple group,△P < 0.05,△△P<0.01
Compared with combining traditional water decoction agent group,#P < 0.05,##P<0.01
As seen from the above table, compared with blank control group, when each embodiment group of Sessileflower Acanthopanax Bark can significantly extend mouse swimming
Between, body movement endurance is improved, tired time of occurrence is postponed, effect is better than Sessileflower Acanthopanax Bark simple group and traditional water decoction agent group,
And 3 groups of effects of embodiment are best.
Claims (10)
1. a kind of Sessileflower Acanthopanax Bark compound, it is characterised in that it mainly by following raw materials by the parts by weight prepare and
At: 10-20 parts of Sessileflower Acanthopanax Bark, 7-8 parts of dried orange peel, 4-8 parts of mulberry fruit, 1-2 parts of fructus alpiniae oxyphyllae.
2. a kind of Sessileflower Acanthopanax Bark compound according to claim 1, it is characterised in that it is mainly by following raw materials
It is prepared by the parts by weight: 15 parts of Sessileflower Acanthopanax Bark, 7.5 parts of dried orange peel, 6 parts of mulberry fruit, 1.5 parts of fructus alpiniae oxyphyllae.
3. a kind of preparation method of Sessileflower Acanthopanax Bark compound as claimed in claim 1 or 2, it is characterised in that preparation method step
It is rapid as follows:
(1) Sessileflower Acanthopanax Bark for meeting the parts by weight, dried orange peel, mulberries, fructus alpiniae oxyphyllae are weighed, through co-grinding to 10-40 mesh, is obtained
Thick medicinal powder is spare；
(2) thick medicinal powder being placed in medicine pot, first time amount of water is 18-22 times of thick medicinal powder weight, it impregnates 0.5-1.5 hours,
0.35-0.55 parts by weight pectase is added, citric acid tune pH value is 3.0-5.0, and constant temperature digests 1- in 30 DEG C of -50 DEG C of enzymatic hydrolysis pots
3 hours, after enzymatic hydrolysis, it is warming up to 93-97 DEG C of enzyme deactivation；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled decoction 1-3 hours, is filtered, collect filtrate；Second of amount of water of filter residue
It is 18-22 times of thick medicinal powder weight, after boiling, filtrate is collected in slightly boiled decoction 1-3 hours, filtration；Filter residue third time amount of water is
18-22 times of thick medicinal powder weight, after boiling, filtrate is collected in slightly boiled decoction 0.5-1.5 hours, filtration；
(4) the resulting filtrate three times of step (3) is merged, 4000-6000r/min is centrifuged 10-20min, collects supernatant；
(5) retention is respectively adopted by molecular weight 300K, 100K, 10K Hollow Fiber Ultrafiltration column in the supernatant for collecting step (4)
Ultrafiltration is carried out, ultrafiltrate is collected；
(6) by step (5) resulting ultrafiltrate, under the conditions of 40-50 DEG C, relative molecular mass 300-600Da is retained using film
Nanofiltration concentration is carried out, the volume of the concentrated liquid is the 1/4-3/4 of stoste volume, obtains concentrate；
(7) it to the maltodextrin of 0.2-0.4 times of concentrate weight of addition in step (6) resulting concentrate, stirs evenly laggard
Row spray drying, spray drying condition are as follows: 110-130 DEG C of inlet air temperature, 80-100 DEG C of leaving air temp, and atomizing pressure 750-
850Pa, hydrojet speed 8-12%, obtains dried powder；
(8) dried powder obtained by step (7) is put into micronizer to pulverize, passes through high energy nanometer impact grinding tank body
Interior mill Jie impacting 5-15min makes the average grain diameter of Ultramicro-powder reach 900-1500nm to get the combination of Sessileflower Acanthopanax Bark compound
Ultra-micro powder.
4. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that step (1) raw material
20 mesh are crushed to after mixing.
5. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that in step (2)
Amount of water is 20 times of thick medicinal powder weight, and soaking time is 1 hour, and pectase additional amount is 0.45 parts by weight, and pH value is
4.0, hydrolysis temperature is 40 DEG C, and enzymolysis time is 2 hours, and enzyme-removal temperature is 95 DEG C.
6. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that enzyme in step (3)
Solving decocting time is 2 hours；Second of amount of water is 20 times of thick medicinal powder weight, and decocting time is 2 hours；Third time amount of water
It is 20 times of thick medicinal powder weight, decocting time is 1 hour.
7. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that in step (4) from
Heart rate is 5000r/min, centrifugation time 15min.
8. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that step is received in (6)
Filtering temperature is 45 DEG C, retaining molecular weight 450Da.
9. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that wheat in step (7)
The additive amount of bud dextrin is 0.3 times of concentrate weight；Spray drying condition is as follows: 120 DEG C of inlet air temperature, leaving air temp 90
DEG C, atomizing pressure 800Pa, hydrojet speed 10%.
10. the preparation method of Sessileflower Acanthopanax Bark compound according to claim 3, which is characterized in that step is hit in (8)
Hitting milling time is 10min, and the average grain diameter of Ultramicro-powder is 1200nm.
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Application publication date: 20190111 |