CN109364141A - A kind of dark plum compound and preparation method thereof - Google Patents
A kind of dark plum compound and preparation method thereof Download PDFInfo
- Publication number
- CN109364141A CN109364141A CN201811323509.4A CN201811323509A CN109364141A CN 109364141 A CN109364141 A CN 109364141A CN 201811323509 A CN201811323509 A CN 201811323509A CN 109364141 A CN109364141 A CN 109364141A
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- dark plum
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- powder
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Abstract
Dark plum compound is prepared using classification ultrafiltration, ultramicro grinding method for combined use the invention discloses a kind of, it belongs to traditional Chinese medicine and field of food industry.A kind of dark plum compound, it is mainly prepared by following raw materials by the parts by weight: 40-60 parts of dark plum, 15-35 parts of hawthorn, 14-34 parts of dried orange peel, 0.5-1.5 parts of wrinkled giant hyssop.It is raw material that the present invention, which selects the Chinese medicine of integration of drinking and medicinal herbs, has the function of replenishing qi to invigorate the spleen, dampness elimination helps digestion, relieves summer heat and helps fortune, without any side effects.Preparation method of the invention, it prepares dark plum 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, dark plum compound combination ultra-micro powder obtained is enable to play curative effect quickly.
Description
Technical field
The present invention relates to a kind of using classification ultrafiltration, pulverizes the dark plum compound of method for combined use preparation, it belongs to
In traditional Chinese medicine and field of food industry.
Background technique
There are many toxin in human body, it is all to excrete in time, bad work can produce to our body & mind
Substance can be referred to as " poison ".The intracorporal moisture of people exactly obtains for various subtle toxin buildups, so toxin expelling is
It is basic.
Into after summer, temperature is high, rainwater increases, atmospheric moisture is big, is influenced by temperature and moisture, people often have
The light dull, loss of appetite of limbs fatigue, fatigue, apathetic and mouth, lean body mass or loose watery stool, abdomen have one's mind filled with the diseases such as rise
Shape.Chinese medicine says that summer focuses on nourishing heart spleen, and The spleen has the function to transport and transform nutrients, like dryness and hate wetness, is stranded if wet, then dysfunction of the spleen in transportation and transformation, shows as defecating dilute
Half congealed, abdomen have one's mind filled with rise, do not feel like eating, rotten acid regurgitation etc., so wanting invigorating the spleen to clear away damp pathogen in summer, improve mood, toxin be discharged.
General western medical treatment summer symptom commonly uses clear, clearing heat and expelling damp grain of wet poison etc., only mitigates and eliminate symptom, do not control
It is basic to treat, it is possible to can also aggravate the state of an illness.Chinese medicine conditioning invigorating the spleen to clear away damp pathogen can from human body it is basic from start with, comply with summer feature and
The medicinal materials such as Poria cocos, radix fici simplicissimae, rhizoma atractylodis, cortex acanthopanacis, dark plum, Chinese yam are commonly used in the variation of body internal organs, and temporary solution is effected a permanent cure again, sick thus
The common basic therapy of disease.
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, the dark plum that an object of the present invention is to provide a kind of invigorating the spleen to clear away damp pathogen toxin expelling is multiple
Square composition, it is raw material that it, which selects the Chinese medicine of integration of drinking and medicinal herbs, has the function of replenishing qi to invigorate the spleen, dampness elimination helps digestion, relieves summer heat and helps fortune, nothing
Any toxic side effect.
It is a further object of the present invention to provide the preparation methods of above-mentioned dark plum compound, it uses classification ultrafiltration, surpasses
Crushing of Ultrafine joint technology prepares dark plum complex composition, it destroys raw material cell wall using classification ultrafiltration, ultramicro grinding and makes thin
Effective component is precipitated in born of the same parents, while will not damage to effective component structure, makes dark plum compound combination ultra-micro powder obtained
Curative effect can be played quickly.
To achieve the above object, the present invention is achieved through the following technical solutions:
A kind of dark plum compound, it is mainly prepared by following raw materials by the parts by weight: dark plum 40-60
Part, 15-35 parts of hawthorn, 14-34 parts of dried orange peel, 0.5-1.5 parts of wrinkled giant hyssop.
A kind of above-mentioned dark plum compound, it is mainly prepared by following raw materials by the parts by weight: crow
50 parts of plum, 25 parts of hawthorn, 24 parts of dried orange peel, 1 part of wrinkled giant hyssop.
The preparation method of above-mentioned dark plum compound, its step are as follows:
(1) dark plum and hawthorn for meeting the parts by weight, dried orange peel, wrinkled giant hyssop are weighed, through co-grinding to 10-40 mesh, is obtained slightly
Medicinal powder is spare；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 6-10 times of thick medicinal powder weight, and it is small to impregnate 0.5-1.5
When, the cellulase of 0.06-0.18 parts by weight is added, citric acid-sodium citrate tune pH value is 4.0-6.0, in 40 DEG C of -60 DEG C of enzymes
It solves constant temperature in pot to digest 2-4 hours, after enzymatic hydrolysis, is warming up to 93-97 DEG C of enzyme deactivation；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled decoction 0.5-1.5 hours, is filtered, collect filtrate；Filter residue second
Secondary amount of water is 6-10 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 twice 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 0.1-0.3 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 the combination of dark plum compound
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 8 times of thick medicinal powder weight in above-mentioned steps (2), and soaking time preferably 1 hour, fiber
Plain enzyme additional amount preferably 0.12 parts by weight, pH value is preferably 5.0, preferably 50 DEG C of hydrolysis temperature, enzymolysis time preferably 3 hours, is gone out
Preferably 95 DEG C of enzyme temperature.
Enzymatic hydrolysis decocting time is preferably 1 hour in above-mentioned steps (3), and second of amount of water is preferably the 8 of thick medicinal powder weight
Times, decocting time is preferably 1 hour.
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 0.18 times of concentrate weight in above-mentioned steps (7)；Spray drying air inlet temperature
Preferably 120 DEG C of degree, preferably 90 DEG C of leaving air temp, the preferred 800Pa of atomizing pressure, hydrojet speed preferably 10%.
The preferred 10min of grinding 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 have following features and the utility model has the advantages that
It is as follows the effect of Chinese medicine material used in the present invention: dark plum: Ji Yuan: the drying almost ripe fruit of rose department plant plum.
Nature and flavor: it is sour, puckery, it puts down；Channel tropism: return liver, spleen, lung, large intestine channel；Effect: astringing lung-QI, puckery intestines promote the production of body fluid, claming ascaris；For chronic cough of deficiency lung, long
Protracted dysentery is rushed down, abnormal heat is quenched one's thirst, and the ascariasis of biliary tract vomits abdominal pain.Hawthorn: Ji Yuan: the fruit of rosaceous plant hawthorn or fructus crataegi cuneatae.Property is sour, sweet,
Tepor.Channel tropism: returns spleen, stomach, Liver Channel；Effect: food digesting stomach fortifying, scattered stasis change turbid lipid-loweringing；For meat stagnation, gastral cavilty turgor,
Diarrhea dysentery abdominal pain, blood stasis closed, postpartum stasis, confidant sting, chest impediment and cardialgia, hernia pain, hyperlipidemia.Dried orange peel: Ji Yuan: rue
Section's plant tangerine and its dry mature skin of variety；Nature and flavor: bitter, acrid in flavour and warm in nature.Channel tropism: return lung, the spleen channel；Effect: qi-regulating is strong
Spleen is eliminating dampness and eliminating phlegm.For chest gastral cavity turgor, deficiency of food is vomited and diarrhoea, coughing with a lot of sputum.Wrinkled giant hyssop: Ji Yuan: Lamiaceae plant Pogostemon cablin or wrinkled giant hyssop
Herb；Nature and flavor: pungent, tepor；Channel tropism: return lung, the spleen channel；Effect: eliminating dampness with aromatics, and whet the appetite preventing or arresting vomiting, delivers relieving summer-heat；For it is wet it is turbid in
Resistance, the vomiting of gastral cavity ruffian, summer-heat and damp burnout, not easypro, cold-dampness uncomfortable in chest closes heat, abdominal pain is vomited and diarrhoea, nasosinusitis headache.
The present invention improves Chinese medicine used in the dark plum compound of invigorating the spleen to clear away damp pathogen toxin expelling, selects national integration of drinking and medicinal herbs mesh
Medicinal material is the raw material often selected in raw material, and traditional herbal cuisine in recording.Based on TCM theory, the traditional Chinese medicine preventiveed treatment of disease is adhered to
Say, by monarch be principle carry out prescription, the proportion of strict control each component, have replenish qi to invigorate the spleen, dampness elimination helps digestion, relieves summer heat and helps
The effect of fortune carries out daily conditioning and maintenance to body, complies with summer climate Variation Features and the variation of corresponding body, prevents disease
Feelings occur and development, achieve the purpose that treating both manifestation and root cause of disease.The present invention is carried out above-mentioned dark plum and hawthorn, dried orange peel, wrinkled giant hyssop by the dosage
Combination, so that each raw material generates synergistic function, using citric acid in dark plum as index ingredient in compound, content is more single
Content improves 100.98% in one dark plum.Huangdi's Internal Classics have cloud, when human body will follow the mandate of heaven, i.e., along the variation of five elements' motion and six kinds of natural factors,
Secret key is to comply with the variation of the gas of YIN YANG in four seasons, and human body could muchly keep fit.Summer, The sun is shining fiercely, and rainwater fills
Abundant, the competing length of all things on earth is maked rapid progress.Anode yin is raw, all things on earth at reality, so, Summertime will comply with the summer overabundance of yang in outer feature,
Pay attention to conserving yang-energy, is conceived to " length " word.Dark plum compound is using dark plum as monarch drug in a prescription, and hawthorn, dried orange peel, wrinkled giant hyssop are as minister
Adjutant enhances tonifying lung strengthening the spleen and replenishing qi, mitigates taste burden, while being equipped with and eliminating dampness with aromatics, and removing summer-heat is damp and hot, prevention conditioning summer summer-heat and damp
Gas take advantage of a weak point, prevent obvious out of strength, dizzy, the uncomfortable in chest, palpitaition of whole body, attention cannot be concentrated, largely perspire, four limbs
It is numb, thirsty, the summer-heat and damps symptom such as nausea.Summer-heat and damp indication is alleviated, body mind clean air and, it is energetic, conducive to the logical of mechanism of qi
It lets out, in order to avoid helping heat with heat, pours oil on the fire, be relatively beneficial to the health care of summer heart.
Present invention application classification ultrafiltration, ultramicro grinding joint technology prepare dark plum compound, and traditional Chinese medicine is extracted
Technique is combined with modern biotechnology technique, retains the extracting mode of traditional water decoction decoction, will using enzymatic hydrolysis pre-treating technology
Protein, cellulose, pectic substance on cell wall etc. hinder the main barrier degradation of effective component dissolution intracellular, to make cell
Wall is loose, ruptures, and reduces diffusion of active ingredient resistance intracellular, improves recovery rate.The present invention is adopted for raw material sources in composition
Equal ingredients between cell wall and cell wall can be effectively decomposed with cellulase, it is more abundant compared with other enzyme effects.Cellulase activity one
As optimum temperature mostly between 45-65 DEG C, hydrolysis temperature increases, and enzymatic activity rises, and reactant energy increases, and makes reaction speed
Accelerate.After temperature is more than 60 DEG C, zymoprotein can be caused to be denaturalized, weaken enzyme activity significantly, reaction speed decline, so enzymatic hydrolysis
Temperature selects between 40 DEG C -60 DEG C.Because raw material is mainly fruit class, broken time is longer, therefore to be set to 2-4 small for enzymolysis time
When, enzyme dosage is between 0.06-0.18 parts by weight.It finds in the course of the research, enzymatic hydrolysis acidity has one to index ingredient yield
Fixing is rung, and when pH value is between 4.0-6.0, yield reaches peak value, and pH value increases again, and yield declines instead.Joined by enzymatic hydrolysis
After number optimization, general flavone index content promotes 176.85%.Using starch, protein in biological hyperfiltration technique removal aqueous extract
Etc. macromoleculars inert substance, while reducing loss of effective components, recycle the filtration water removal of nanofiltration biotechnology, enrichment effectively at
Point, while can avoid thermophilic digestion feed liquid in concentrated extracting solution, effective component retention rate is improved, heat energy loss is reduced.It obtains
Ultramicro-powder after water dissolves, liquid clear, no residue deposited phenomenon.The present invention is not introduced into preparation process simultaneously
Organic solvent and chemical reagent do not destroy medicinal material internal component structure, protect character of medicinal material, preferably performance health care curative effect.
The dark plum compound that the present invention improves invigorating the spleen to clear away damp pathogen toxin expelling can be used for preparing alternative tea.
Present invention application classification ultrafiltration, ultramicro grinding joint technology prepare dark plum compound, super through what is be prepared
Micro mist can be used for preparing dark plum compound combined beverage series of products.
Present invention application classification ultrafiltration, ultramicro grinding joint technology prepare dark plum compound and dispel in conditioning engine body invigorating the spleen
The effect of wet aspect is preferable, and it is obvious to alleviate symptom effect, prevention, alleviate because body toxin accumulation caused by summer summer-heat and damp, burnout,
Out of strength, do not feel like eating or stool malt sugar etc. symptoms and its bring other health problems.Selected materials are all integration of drinking and medicinal herbs Chinese medicine,
Raw material is easy to get, without any side effects, can reduce the body liver kidney burden and financial burden of user.After body is taken, warp
There is appetite increase, energetic external manifestation in the Absorption And Metabolism of a period of time, body.In animal experiments, it gives by oral administration
After medicine, blood, liver, dark plum organic acid content in kidney are detected in different time points, and result of study shows organic acid in blood
In 4 hours content highests, 1 hour content highest in liver and kidney can be very after illustrating that dark plum compound enters body
It is absorbed by organisms metabolism fastly, plays curative effect.
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
Dark plum 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 dark plum compound, it is to be prepared by following raw materials by the parts by weight: 40 parts of dark plum, hawthorn
35 parts, 34 parts of dried orange peel, 1.5 parts of wrinkled giant hyssop.
The preparation method of dark plum compound, steps are as follows:
(1) 40 parts by weight dark plums, 35 parts by weight hawthorn, 34 parts by weight dried orange peels, 1.5 parts by weight wrinkled giant hyssops are weighed, through mixed powder
10 mesh are broken to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 6 times of thick medicinal powder weight, is impregnated 0.5 hour, is added
The cellulase of 0.06 parts by weight, citric acid-sodium citrate tune pH value are 4.0, and constant temperature digests 2 hours in 40 DEG C of enzymatic hydrolysis pots,
After enzymatic hydrolysis, it is warming up to 93 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 0.5 hour, filtrate is collected in filtration；Filter residue adds for the second time
Water is 6 times of thick medicinal powder weight, slightly boiled to decoct 0.5 hour after boiling, and filtrate is collected in filtration；
(4) the resulting filtrate twice 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 0.1 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 Ultramicro-powder to get dark plum compound
End.
Embodiment 2
A kind of dark plum compound, it is to be prepared by following raw materials by the parts by weight: 45 parts of dark plum, hawthorn
30 parts, 30 parts of dried orange peel, 1.2 parts of wrinkled giant hyssop.
The preparation method of dark plum compound, steps are as follows:
(1) 45 parts by weight dark plums, 30 parts by weight hawthorn, 30 parts by weight dried orange peels, 1.2 parts by weight wrinkled giant hyssops are weighed, through mixed powder
16 mesh are broken to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 7 times of thick medicinal powder weight, is impregnated 0.8 hour, is added
The cellulase of 0.08 parts by weight, citric acid-sodium citrate tune pH value are 4.5, and constant temperature enzymatic hydrolysis 2.5 is small in 45 DEG C of enzymatic hydrolysis pots
When, after enzymatic hydrolysis, it is warming up to 94 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 0.7 hour, filtrate is collected in filtration；Filter residue adds for the second time
Water is 7 times of thick medicinal powder weight, slightly boiled to decoct 0.7 hour after boiling, and filtrate is collected in filtration；
(4) the resulting filtrate twice 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 0.15 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 and combines Ultramicro-powder to get dark plum compound
End.
Embodiment 3
A kind of dark plum compound, it is to be prepared by following raw materials by the parts by weight: 50 parts of dark plum, hawthorn
25 parts, 24 parts of dried orange peel, 1 part of wrinkled giant hyssop.
The preparation method of dark plum compound, steps are as follows:
(1) 50 parts by weight dark plums, 25 parts by weight hawthorn, 24 parts by weight dried orange peels, 1 parts by weight wrinkled giant hyssop are weighed, through co-grinding
To 20 mesh, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 8 times of thick medicinal powder weight, is impregnated 1 hour, is added
The cellulase of 0.12 parts by weight, citric acid-sodium citrate tune pH value are 5.0, and constant temperature digests 3 hours in 50 DEG C of enzymatic hydrolysis pots,
After enzymatic hydrolysis, it is warming up to 95 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 8 times of thick medicinal powder weight, slightly boiled to decoct 1 hour after boiling, and filtrate is collected in filtration；
(4) the resulting filtrate twice 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 0.2 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: 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 and combines Ultramicro-powder to get dark plum compound
End.
Embodiment 4
A kind of dark plum compound, it is to be prepared by following raw materials by the parts by weight: 55 parts of dark plum, hawthorn
20 parts, 20 parts of dried orange peel, 0.8 part of wrinkled giant hyssop.
The preparation method of dark plum compound, steps are as follows:
(1) 55 parts by weight dark plums, 20 parts by weight hawthorn, 20 parts by weight dried orange peels, 0.8 parts by weight wrinkled giant hyssop are weighed, through mixed powder
30 mesh are broken to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 9 times of thick medicinal powder weight, is impregnated 1.2 hours, is added
The cellulase of 0.16 parts by weight, citric acid-sodium citrate tune pH value are 5.5, and constant temperature enzymatic hydrolysis 3.5 is small in 55 DEG C of enzymatic hydrolysis pots
When, after enzymatic hydrolysis, it is warming up to 96 DEG C of enzyme deactivations；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled to decoct 1.2 hours, filtrate is collected in filtration；Filter residue adds for the second time
Water is 9 times of thick medicinal powder weight, slightly boiled to decoct 1.2 hours after boiling, and filtrate is collected in filtration；
(4) the resulting filtrate twice 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 0.25 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: 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 and combines Ultramicro-powder to get dark plum compound
End.
Embodiment 5
A kind of dark plum compound, it is to be prepared by following raw materials by the parts by weight: 60 parts of dark plum, hawthorn
15 parts, 14 parts of dried orange peel, 0.5 part of wrinkled giant hyssop.
The preparation method of dark plum compound, steps are as follows:
(1) 60 parts by weight dark plums, 15 parts by weight hawthorn, 14 parts by weight dried orange peels, 0.5 parts by weight wrinkled giant hyssop are weighed, through mixed powder
40 mesh are broken to, it is spare to obtain thick medicinal powder；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 10 times of thick medicinal powder weight, is impregnated 1.5 hours, is added
The cellulase of 0.18 parts by weight, citric acid-sodium citrate tune pH value are 6.0, and constant temperature digests 4 hours in 60 DEG C of enzymatic hydrolysis pots,
After enzymatic hydrolysis, it is warming up to 97 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 10 times of thick medicinal powder weight, slightly boiled to decoct 1.5 hours after boiling, and filtrate is collected in filtration；
(4) the resulting filtrate twice 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 0.3 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: 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 and combines Ultramicro-powder to get dark plum compound
End.
Thick medicinal powder obtained by step (1) can be applied to prepare dark plum compound alternative tea in embodiment 1,2,3,4,5.
The combination of dark plum compound obtained by step (8) ultra-micro powder can be used for dark plum compound combination drink in embodiment 1,2,3,4,5
Expect series of products.
Test example 1
The detection and content point of the dark plum compound combination ultra-micro powder ingredient of 1,2,3,4,5 method of embodiment of the present invention preparation
Analysis method and result are as follows:
(1) prepared by reference substance solution: precision weighs citric acid reference substance 10mg, sets in 10mL measuring bottle, and mobile phase, which is added, to be made
Dissolution is diluted to scale, and precision is drawn 2.5mL, set in 10mL measuring bottle, and mobile phase, which is added, to be made to dissolve, and is diluted to scale, obtains
The citric acid reference substance solution of 0.25mg/mL.
(2) chromatographic condition: mobile phase 0.8%NH4H2PO4Solution (uses H3PO4Adjust pH 2.2), flow velocity 1.0mL/min,
Column temperature is 25 DEG C, Detection wavelength 214nm, and sample volume is 20 μ L.
(3) drafting of standard curve: precision draws 1,2,5,10,15,20 μ L of reference substance solution, sample introduction measurement.With lemon
Sour sample volume be abscissa, peak area integrated value be ordinate, draw standard curve.
(4) prepared by test solution: precision weighs the dark plum compound combination Ultramicro-powder of 1,2,3,4,5 method of embodiment preparation
Each 1.0g in end, is respectively placed in 50mL stuffed conical flask, and after methanol 25mL is added in precision, weighed weight, ultrasonic extraction 1h is put
It is cold, then weighed weight, less loss weight is supplied with methanol, is shaken up, is filtered.Precision measures subsequent filtrate 2mL, after volatilizing methanol, with stream
Dynamic phase is settled in 10mL measuring bottle, is shaken up, through 0.45 μm of miillpore filter filtration to get test solution.
The preparation of dark plum simple: precision weighs dark plum, extracts by 3 extracting method of embodiment, by test solution method system
For to get dark plum single drug solns.
Traditional water decoction agent group sample preparation: 50 parts of dark plum, 25 parts of hawthorn, dried orange peel 24 are weighed in 3 step of embodiment (1) ratio
Part, 1 part of wrinkled giant hyssop, carry out being crushed to 20 mesh after mixing.First time amount of water is 8 times of medicinal material amount, is impregnated 1 hour, slightly boiled to decoct 1
Hour, filtrate is collected in filtration；Second of amount of water of filter residue is 8 times of medicinal material amount, slightly boiled to decoct 1 hour after boiling, and filters, receives
Collect filtrate.Filtrate, moisture volatilize twice for merging.Precision weighs 1.0g medicinal extract, prepares by test solution method to get traditional water
Decoction group sample solution
(5) experimental result
1 reference substance sample volume of table and peak area
| Reference substance/μ L | 1 | 2 | 5 | 10 | 15 | 20 |
| Peak area | 17373 | 32051 | 79059 | 162404 | 253216 | 308310 |
Calibration curve equation is Y=15813X+2390.2, coefficient R=0.9978
The measurement comparison of 2 citric acid content of table
| Grouping | Citric acid content % |
| Example 1 group | 23.91 |
| 2 groups of embodiment | 25.13 |
| 3 groups of embodiment | 26.55 |
| 4 groups of embodiment | 26.22 |
| 5 groups of embodiment | 25.90 |
| Dark plum simple group | 13.21 |
| Traditional water decoction agent group | 9.59 |
The comparison of 3 nutrient component determining of table
Test example 2
The dark plum compound combination Ultramicro-powder of 1,2,3,4,5 method of embodiment of the present invention preparation is used for taste summer-heat and damp animal model
Test.
(1) Animal Model
Select weight for SPF grades of 18-22g BALB/c male mice 120, mouse is common in SPF grades of laboratories
It feed adaptable fed 7 days, after adaptable fed, randomly selects 100 and carries out stomach-filling with 20% folium sennae liquid, it is every small
Mouse stomach-filling volume is 0.3mL, and Normal group mouse carries out the ultrapure water stomach-filling of same volume.Daily stomach-filling 1 time, continuous gavage 7
It, during which conventinal breeding.There is the relevant symptom and sign of taste summer-heat and damp disease, serum, knot in experimental result discovery mouse model
There is significantly raised (P < 0.05) in intestines TNF-α, prompts the success of taste summer-heat and damp disease model modeling.
(2) animal packet and administration
Using 10 healthy kunming mices as blank control group (drinking water), it is small that 80 taste summer-heat and damps model successful Kunming
Mouse is randomly divided into 8 groups, i.e. animal model group, and 1,2,3,4,5 group of embodiment, dark plum simple group and traditional water decoction agent group, every group
10.Each experimental group dosage is 517.76mg/kg, and administration capacity is 10mL/kg.Each group is raised commonly to raise during experiment
Material, and free water, daily stomach-filling 1 time, continuous gavage 7 days.
(3) observation index
Since the 1st day to the state of mind for the mouse all organized, mobility, coat state, weight, anus situation,
Excrement situation is observed, and weight is surveyed weekly once, continuous 7 days, is measured before morning stomach-filling.
(4) experimental result
The weight dynamic change of 4.1 each group mouse
As shown in Table 4, during to drug 7 days, when the 0th day, each experimental mice weight is compared with normal group, as a result
There is no statistical difference (P > 0.05)；When the 7th day, compared with model group, 3 groups of embodiment can improve taste extremely significantly
Summer-heat and damp mouse weight (P < 0.01).The experimental results showed that a kind of dark plum compound for clearing damp of relieving summer heat can be controlled effectively
The indigestion symptoms such as appetite stimulator because of caused by summer hot summer weather are treated, and effect is substantially better than dark plum simple group and traditional water
Decoction group.
4 different time sections each group mouse weight of table compares (g)
Note: compared with blank control group,aP<0.05
Compared with model group,bP < 0.05,cP<0.01
Compared with dark plum simple group,dP < 0.05,eP<0.01
Compared with traditional water decoction agent group,fP < 0.05,gP<0.01
4.2 overview results
The blank control group mouse state of mind is good, and activity is quick, and feed is normal, and coat is fair and clear glossy, and tripe mouth has no
Redness, tripe peritricha is clean, and excrement is brown neither too hard, nor too soft at graininess color, and excrement has no washmarking on filter paper.
Taste summer-heat and damp model group mouse is apathetic depressed, and Teng's contracting, happiness is closed one's eyes, drowsiness lazy move, and feed, which is reduced, even goes on a hunger strike,
Coat is dark and gloomy in a jumble, and anus lipstick swells obviously with rectal prolapse, and paratroch jaundice is stained with excrement, is let out long, and shapeless excrement is watery, filter paper sheet
Washmarking.
The embodiment each group mouse state of mind is good, and activity is sensitive, and feed is normal, and coat is fair and clear glossy, the non-show of anus mouth
Swollen, tripe peritricha is clean, and excrement is brown neither too hard, nor too soft at graininess color, excrement slightly washmarking on filter paper.
The dark plum simple group mouse state of mind is poor, likes poly- heap Teng contracting, drowsiness lazy move, and feed is reduced, and coat is matt, anus
Lipstick is swollen to have rectal prolapse more, and crissum is stained with excrement, is let out long, and excrement is shapeless to filter just for water, filter paper sheet washmarking.
Traditional water decoction agent group mouse rhembasmus likes poly- heap Teng contracting, and drowsiness lazy move, food-intake is few even to go on a hunger strike, and coat is miscellaneous
Disorderly, anus is red and swollen rectal prolapse more, and crissum jaundice is stained with excrement, is let out long, and excrement is shapeless to filter just for water, filter paper sheet washmarking.
Claims (10)
1. a kind of dark plum compound, it is characterised in that it is mainly prepared by following raw materials by the parts by weight:
40-60 parts of dark plum, 15-35 parts of hawthorn, 14-34 parts of dried orange peel, 0.5-1.5 parts of wrinkled giant hyssop.
2. a kind of dark plum compound according to claim 1, it is characterised in that it mainly presses institute by following raw materials
It states parts by weight to be prepared: 50 parts of dark plum, 25 parts of hawthorn, 24 parts of dried orange peel, 1 part of wrinkled giant hyssop.
3. a kind of preparation method of dark plum compound as claimed in claim 1 or 2, it is characterised in that steps are as follows:
(1) dark plum and hawthorn for meeting the parts by weight, dried orange peel, wrinkled giant hyssop are weighed, through co-grinding to 10-40 mesh, obtains thick medicinal powder
It is spare；
(2) thick medicinal powder is placed in medicine pot, first time amount of water is 6-10 times of thick medicinal powder weight, impregnates 0.5-1.5 hours, adds
Enter the cellulase of 0.06-0.18 parts by weight, citric acid-sodium citrate tune pH value is 4.0-6.0, in 40 DEG C of -60 DEG C of enzymatic hydrolysis pots
Middle constant temperature digests 2-4 hours, after enzymatic hydrolysis, is warming up to 93-97 DEG C of enzyme deactivation；
(3) after enzyme deactivation, enzymatic treatment system is boiled, slightly boiled decoction 0.5-1.5 hours, is filtered, collect filtrate；Filter residue adds for the second time
Water is 6-10 times of thick medicinal powder weight, after boiling, slightly boiled decoction 0.5-1.5 hours, and filtration, merging filtrate；
(4) the resulting filtrate twice 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 0.1-0.3 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 and combines ultra micro to get dark plum compound
Powder.
4. the preparation method of dark plum compound according to claim 3, which is characterized in that the mixing of step (1) raw material
After be crushed to 20 mesh.
5. the preparation method of dark plum compound according to claim 3, which is characterized in that in step (2) for the first time
Amount of water is 8 times of thick medicinal powder weight, and soaking time is 1 hour, and cellulase additional amount is 0.12 parts by weight, pH value 5.0,
Hydrolysis temperature is 50 DEG C, and enzymolysis time is 3 hours, and enzyme-removal temperature is 95 DEG C.
6. the preparation method of dark plum compound according to claim 3, which is characterized in that enzymatic hydrolysis is decocted in step (3)
Boiling the time is 1 hour, and second of amount of water is 8 times of thick medicinal powder weight, and decocting time is 1 hour.
7. the preparation method of dark plum compound according to claim 3, which is characterized in that centrifugation speed in step (4)
Rate is 5000r/min, centrifugation time 15min.
8. the preparation method of dark plum compound according to claim 3, which is characterized in that nanofiltration temperature in step (6)
Degree is 45 DEG C, retaining molecular weight 450Da.
9. the preparation method of dark plum compound according to claim 3, which is characterized in that malt is pasted in step (7)
The additive amount of essence is preferably 0.2 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 dark plum compound according to claim 3, which is characterized in that grinding in step (8)
10min, the average grain diameter of Ultramicro-powder are 1200nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116270910A (en) * | 2023-02-21 | 2023-06-23 | 四川德培源中药科技开发有限公司 | Summer heat clearing and fluid supplementing electrolyte anti-fatigue composition and preparation method thereof |
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| CN101850081A (en) * | 2009-03-31 | 2010-10-06 | 北京因科瑞斯医药科技有限公司 | Traditional Chinese medicine composition capable of facilitating digestion and preparation method thereof |
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2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850081A (en) * | 2009-03-31 | 2010-10-06 | 北京因科瑞斯医药科技有限公司 | Traditional Chinese medicine composition capable of facilitating digestion and preparation method thereof |
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| 范青生: "《保健食品工艺学》", 30 November 2006, 中国中医药科技出版社 * |
| 马华，等: "开胃增食灵治疗小儿厌食症临床观察", 《中国中医药信息杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116270910A (en) * | 2023-02-21 | 2023-06-23 | 四川德培源中药科技开发有限公司 | Summer heat clearing and fluid supplementing electrolyte anti-fatigue composition and preparation method thereof |
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