CN106361980A - Polygonatum kingianum lozenge and preparation method thereof - Google Patents
Polygonatum kingianum lozenge and preparation method thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8969—Polygonatum (Solomon's seal)
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- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
- A61K9/0056—Mouth soluble or dispersible forms; Suckable, eatable, chewable coherent forms; Forms rapidly disintegrating in the mouth; Lozenges; Lollipops; Bite capsules; Baked products; Baits or other oral forms for animals
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- A61K2236/30—Extraction of the material
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- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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Abstract
The invention discloses a polygonatum kingianum lozenge and a preparation method thereof. The method comprises the following steps that S1, fresh polygonatum kingianum freeze-dried powder is prepared; S2, polygonatum kingianum extract freeze-dried powder is prepared; S3, tabletting is performed: the fresh polygonatum kingianum freeze-dried powder and the polygonatum kingianum extract freeze-dried powder are mixed and are then subjected to tabletting to prepare the polygonatum kingianum lozenge. The step S1 has a concrete operation mode that fresh polygonatum kingianum is taken and is subjected to freeze drying, and the temperature is -35 to -45 DEG C, so that the water content of the fresh polygonatum kingianum is lower than 10 percent; the fresh polygonatum kingianum is ground into powder to obtain the fresh polygonatum kingianum freeze-dried powder. The step S2 has a concrete operation mode that S2-1, pretreatment is performed: the fresh polygonatum kingianum is pulverized; enzymatic hydrolysate is added; enzymolysis is performed to obtain a solid and liquid mixture A; S2-2, the effective ingredients in the solid and liquid mixture A are effectively extracted to obtain effective ingredient liquid; S2-3, the effective ingredient liquid is concentrated to obtain concentrated liquid; S2-4, the concentrated liquid is subjected to freeze drying to obtain the polygonatum kingianum extract freeze-dried powder. After the preparation method is used, the activity of all effective ingredients of the polygonatum kingianum is reserved to a great degree; the medicine effect is improved.
Description
Technical field
The present invention relates to a kind of tablet and preparation method thereof is and in particular to a kind of P. kingianum buccal tablet and preparation method thereof.
Background technology
P. kingianum Liliaceae Polygonatum herbaceous plant, root stock closely cylinder or nearly beaded, tuberosity is made irregularly sometimes
Pedicellus et Pericarpium Trapae shape is plump.Produce Chinese yunnan, Sichuan, Guizhou.Raw sylvan life, shrubbery or dark and damp grass slope, give birth on rock, height above sea level 700- sometimes
3600 meters.P. kingianum rhizome can control pulmonary tuberculosis, dry cough without phlegm, and xerostomia, fatigue and weakness, diabetes, hypertension are done in prolonged illness Tianjin；Can
Control prolonged illness physical weakness, lumbago, dry cough, sweating due to debility, conjunctival congestion etc..
It is rich in the active substance such as polysaccharide, aminoacid, Flavonoid substances, saponin in P. kingianum, effective to it in prior art
The extraction process of material is not good, easily causes the loss of active substance, when preparing P. kingianum buccal tablet, needs to add releasing agent simultaneously,
Cause the chemical contamination to medicine；All using the polysaccharide in P. kingianum or saponin extract as raw material in another existing process, not
Fresh P. kingianum can be added as raw material, cause drug effect not good and single.
Content of the invention
It is an object of the invention to not good to the extraction process of P. kingianum active substance in solution prior art, easily cause
The loss of effect material, when preparing P. kingianum buccal tablet simultaneously, needs to add releasing agent, causes the chemical contamination to medicine；Separately existing
All using the polysaccharide in P. kingianum or saponin extract as raw material in technique, have not been able to add fresh P. kingianum as raw material, make
Become the good and not single problem of drug effect.
For solving above-mentioned technical problem, the present invention employs the following technical solutions: a kind of P. kingianum process for preparing buccal lozenge, bag
Containing following steps:
S1 is obtained fresh P. kingianum lyophilized powder；
S2 is obtained P. kingianum extract freeze-drying powder；
S3 tabletting: carry out tabletting with P. kingianum extract freeze-drying powder after described fresh P. kingianum lyophilized powder is mixed, prepared Yunnan is yellow
Smart buccal tablet.
P. kingianum buccal tablet is obtained for raw material using fresh P. kingianum lyophilized powder and P. kingianum extract freeze-drying powder, fresh P. kingianum freezes
Dry powder greatly remains various effective ingredient in fresh P. kingianum, rather than single using certain extract, various components matching
Use, drug effect is more preferably；Add P. kingianum extract freeze-drying powder so as to certain active constituent content increases, increase its property of medicine.
Preferably, fresh P. kingianum lyophilized powder is prepared from using following methods in s1 step: take fresh P. kingianum to carry out cold
Lyophilizing is dry, temperature be -35～-45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into powder and obtain fresh P. kingianum
Lyophilized powder.Fresh P. kingianum will be contained and be chilled to below freezing, and make water be changed into ice, then under high vacuum, ice is changed into steam
And remove, targetedly select temperature to be -35～-45 DEG C, make fresh P. kingianum water content be less than 10% simultaneously, beneficial to fresh P. kingianum
The preservation of lyophilized powder, is beneficial to compression molding below simultaneously.
Preferably, P. kingianum extract freeze-drying powder is prepared from using following methods in s2 step:
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting: the effective ingredient in solidliquid mixture a is extracted, obtains effective ingredient liquid；
S2-3 concentrates: effective ingredient liquid is concentrated, obtains concentrated solution；
S2-4 powder: concentrated solution is carried out lyophilization, obtains P. kingianum extract freeze-drying powder.
First add enzymolysis solution to be digested so as to active substance flows out from cell wall by after the pulverizing of fresh P. kingianum, be beneficial to
Effective ingredient liquid is first concentrated by the extraction of effective ingredient, on the one hand makes active substance content in tablet higher, on the other hand
It is dried after concentration, it is possible to reduce the time needed for lyophilization again, while energy saving, the lyophilization energy of short time
The activity of the holding active substance of high degree, it is to avoid low temperature damages to active substance for a long time.
Preferably, described step s2-2 effective component extracting comprises the following steps:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Obtaining solid-to-liquid ratio is 1:10～20, and cold water temperature is 20～30 DEG C, separates and obtains liquid phase part b and solid fraction b；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:8～18, and hot water temperature is 60～80 DEG C, separates and obtains liquid phase part c and solid fraction c；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:8～15, and ethanol temperature is 70～85 DEG C, separates and obtains liquid phase part d and solid fraction d；
Liquid phase part b, liquid phase part c, liquid phase part d are effective ingredient liquid, and liquid phase part b, liquid phase part c, liquid phase part d divide
Not after s2-3 concentration and s2-4 powder, then carry out being mixed to get P. kingianum extract freeze-drying powder.
Adopt 20～30 DEG C of cold water extraction for the first time, by the volatile material in fresh P. kingianum and the many of cold water can be soluble in
The materials such as sugar, aminoacid extract；Adopt for second 60～80 DEG C of hot water to extract, the Saponin in fresh P. kingianum can be extracted
With Rhizoma Polygonati composition；Third time adopts 70～85 DEG C of hot ethanol to extract, and further the Saponin in fresh P. kingianum is extracted, with
When Flavonoid substances are extracted.Using three step extracting modes, adopt different Extraction solvent for different extracts, greatly
The activity saving effective ingredient of degree, extracts so that extraction degree is higher for three times, extraction efficiency is higher simultaneously.
It is that liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μ as preferential, described step s2-3 concentration step
M, liquid phase part c and liquid phase part d adopt negative pressure evaporation to concentrate, and described negative pressure evaporation concentrates in the following ways: first will
The pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01～0.05mpa 20～60 minutes, then keeps pressure to exist
0.05～0.1mpa reduces 10～20 times to liquid volume, and described negative pressure evaporation concentrates overall process liquid and all keeps less than 80 DEG C.
Membrance concentration technology is adopted for the liquid phase part b being obtained using cold water extraction, can at utmost retain volatility thing therein
Material, mainly fragrance class material are so that the former P. kingianum taste of buccal tablet is stronger.Liquid phase part c and liquid phase part d is using negative
Pressure evaporation and concentration, reaches extraction and requires, consider while reduces cost, most effective.
Preferably, described s2-4 milling step be liquid phase part b concentrated after carry out lyophilization, temperature be -35
～-45 DEG C, it is less than 10% to water content；Carry out atomization drying after liquid phase part c and liquid phase part d is concentrated, be less than to water content
10%.It is rich in polysaccharide and aminoacid, lyophilization is carried out at low temperature, therefore in the thing for many thermal sensitivitys in liquid phase part b
Matter is particularly suitable, such as polysaccharide and aminoacid, degeneration will not occur or lose biologos, avoid oxidation simultaneously.Liquid phase part c
And liquid phase part d adopts atomization drying speed fast, efficiency can be improved.
Preferably, calculating by weight, fresh P. kingianum lyophilized powder is 85～95 parts, and P. kingianum extract freeze-drying powder is
5～15 parts.In P. kingianum buccal tablet, predominant amount is fresh P. kingianum lyophilized powder, accounts for larger specific gravity, P. kingianum extract freeze-drying powder contains
Amount is less, is to make various components matching in P. kingianum use using this proportioning purpose, then to add P. kingianum extract lyophilizing
Powder, increases the property of medicine, and drug effect is higher.
Preferably, mix described fresh P. kingianum lyophilized powder with P. kingianum extract freeze-drying powder after, only spray water is just
Carry out tabletting, injection flow rate mix with P. kingianum extract freeze-drying powder for P. kingianum lyophilized powder after weight 0.1～0.3%.Using this
Invention preparation method, releasing agent need not be added in tabletting it is only necessary to spray 0.1～0.3% water, fresh P. kingianum lyophilized powder with
Form lubricating layer in tablet surface after the water suction of P. kingianum extract freeze-drying powder, play the effect of assisted demoulding.
Preferably, in described s2-2-1 step, circulate this process 2～8 times, control total time during circulation 0.5～
8h；In described s2-2-2 step, circulate this process 2～4 times, during circulation, total time controls in 0.1～4h.S2-2-1 and s2-
2-2 step is extracted using multiple circulation, but is controlled the total time it circulated during extraction, and long soaking time easily becomes
Matter, reduces production efficiency, and the time is too short simultaneously, and its interior active substance leaches not exclusively, therefore control this time period
Good.
A kind of P. kingianum buccal tablet, is prepared from using any one preparation method above-mentioned.Its interior effective ingredient species is relatively
Many, active constituent content is more, the activity saving effective ingredient of high degree, and drug effect is more preferably.
Compared with prior art, the present invention at least can produce a kind of following beneficial effect: it is many that the present invention contains P. kingianum
Plant effective ingredient, each composition cooperates, improve the property of medicine；The work saving each effective ingredient of P. kingianum of high degree of the present invention
Property, increase drug effect；The present invention is in tableting processes it is not necessary to add releasing agent, it is to avoid chemical contamination；Saving money of the present invention
Source, comprehensive benefit is high.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Embodiment 1:
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -35 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Obtaining solid-to-liquid ratio is 1:10, and cold water temperature is 20 DEG C, separates and obtains liquid phase part b and solid fraction b；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:8, and hot water temperature is 60 DEG C, separates and obtains liquid phase part c and solid fraction c；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:8, and ethanol temperature is 70 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01mpa 20 minutes, so
Keep pressure to reduce 10 times in 0.05mpa to liquid volume afterwards, described negative pressure evaporation concentrate overall process liquid all keep 80 DEG C with
Under, obtain concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -35 DEG C, be less than 10% to water content；Liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 85 parts, take P. kingianum extract freeze-drying powder to be 15
Part, carry out tabletting, prepared P. kingianum buccal tablet after mixing.
Embodiment 2:
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Obtaining solid-to-liquid ratio is 1:20, and cold water temperature is 30 DEG C, separates and obtains liquid phase part b and solid fraction b；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:18, and hot water temperature is 80 DEG C, separates and obtains liquid phase part c and solid fraction c；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:15, and ethanol temperature is 85 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.05mpa 60 minutes, so
Keep pressure to reduce 20 times in 0.1mpa to liquid volume afterwards, described negative pressure evaporation concentrate overall process liquid all keep 80 DEG C with
Under, obtain concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -45 DEG C, be less than 10% to water content, liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 95 parts, take P. kingianum extract freeze-drying powder to be 5
Part, carry out tabletting, prepared P. kingianum buccal tablet after mixing.
Embodiment 3:
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Solid-to-liquid ratio is 1:20, cold water temperature is 30 DEG C, separates and obtains liquid phase part b and solid fraction b, circulates this process 2 times, circulation
When control in 0.5h total time；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:18, and hot water temperature is 80 DEG C, separates and obtains liquid phase part c and solid fraction c, circulates this process 2 times, during circulation
Total time controls in 0.1h；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:15, and ethanol temperature is 85 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01mpa 20 minutes, so
Keep pressure to reduce 10 times in 0.05mpa to liquid volume afterwards, described negative pressure evaporation concentrate overall process liquid all keep 80 DEG C with
Under, obtain concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -40 DEG C, be less than 10% to water content, liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 95 parts, take P. kingianum extract freeze-drying powder to be 5
Part, sprayed water after mixing, injection flow rate mix with P. kingianum extract freeze-drying powder for P. kingianum lyophilized powder after weight 0.1%, enter
Row tabletting, prepared P. kingianum buccal tablet.
Embodiment 4
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Solid-to-liquid ratio is 1:10, cold water temperature is 30 DEG C, separates and obtains liquid phase part b and solid fraction b, circulates this process 8 times, circulation
When control in 8h total time；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:18, and hot water temperature is 80 DEG C, separates and obtains liquid phase part c and solid fraction c, circulates this process 4 times, during circulation
Total time controls in 4h；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:15, and ethanol temperature is 85 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01mpa 40 minutes, so
Pressure is kept to reduce 15 times in 0.05mpa to liquid volume afterwards, described negative pressure evaporation concentrates overall process liquid and all keeps 60 DEG C, obtains
To concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -40 DEG C, be less than 10% to water content, liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 95 parts, take P. kingianum extract freeze-drying powder to be 5
Part, sprayed water after mixing, injection flow rate mix with P. kingianum extract freeze-drying powder for P. kingianum lyophilized powder after weight 0.3%, enter
Row tabletting, prepared P. kingianum buccal tablet.
Embodiment 5:
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Solid-to-liquid ratio is 1:10, cold water temperature is 20 DEG C, separates and obtains liquid phase part b and solid fraction b, circulates this process 8 times, circulation
When control in 8h total time；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:18, and hot water temperature is 70 DEG C, separates and obtains liquid phase part c and solid fraction c, circulates this process 4 times, during circulation
Total time controls in 4h；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:10, and ethanol temperature is 75 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01mpa 40 minutes, so
Pressure is kept to reduce 15 times in 0.05mpa to liquid volume afterwards, described negative pressure evaporation concentrates overall process liquid and all keeps 60 DEG C, obtains
To concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -40 DEG C, be less than 10% to water content, liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 85 parts, take P. kingianum extract freeze-drying powder to be 15
Part, sprayed water after mixing, injection flow rate mix with P. kingianum extract freeze-drying powder for P. kingianum lyophilized powder after weight 0.3%, enter
Row tabletting, prepared P. kingianum buccal tablet.
Optimum embodiment:
A kind of P. kingianum buccal tablet and preparation method thereof, comprises the steps of
S1 is obtained fresh P. kingianum lyophilized powder:
Take fresh P. kingianum to carry out lyophilization, temperature be -45 DEG C so that fresh P. kingianum water content is less than 10%, then be ground into
Powder obtains fresh P. kingianum lyophilized powder.
S2 is obtained P. kingianum extract freeze-drying powder；
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Solid-to-liquid ratio is 1:10, cold water temperature is 20 DEG C, separates and obtains liquid phase part b and solid fraction b, circulates this process 4 times, circulation
When control in 5h total time；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:18, and hot water temperature is 70 DEG C, separates and obtains liquid phase part c and solid fraction c, circulates this process 2 times, during circulation
Total time controls in 1h；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:10, and ethanol temperature is 80 DEG C, separates and obtains liquid phase part d and solid fraction d；Liquid phase part b, liquid phase part c,
Liquid phase part d is effective ingredient liquid.
S2-3 concentrates: liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, liquid phase part c and liquid phase part d adopts
Concentrated with negative pressure evaporation, first the pressure of liquid phase part c or liquid phase part d is maintained at vacuum 0.01mpa 40 minutes, so
Pressure is kept to reduce 15 times in 0.05mpa to liquid volume afterwards, described negative pressure evaporation concentrates overall process liquid and all keeps 60 DEG C, obtains
To concentrated solution.
S2-4 powder: carry out lyophilization after liquid phase part b is concentrated, temperature is -40 DEG C, be less than 10% to water content, liquid
Phase part c and liquid phase part d concentrated after carry out atomization drying, be less than 10% to water content, then mixed, obtain P. kingianum
Extract freeze-drying powder.
S3 tabletting: calculate by weight, take fresh P. kingianum lyophilized powder to be 85 parts, take P. kingianum extract freeze-drying powder to be 15
Part, sprayed water after mixing, injection flow rate mix with P. kingianum extract freeze-drying powder for P. kingianum lyophilized powder after weight 0.2%, enter
Row tabletting, prepared P. kingianum buccal tablet.
Spoken of in this manual multiple explanatory embodiment, refers to the concrete grammar bag with reference to the description of this embodiment
Include at least one embodiment of the application generality description.Multiple local appearance statement of the same race in the description is not certain
Refer to same embodiment.Furthermore, it is understood that when describing a method with reference to any one embodiment, to be advocated is to combine
Other embodiment falls within the scope of the present invention realizing this method.
Claims (10)
1. a kind of P. kingianum process for preparing buccal lozenge it is characterised in that: comprise the steps of
S1 is obtained fresh P. kingianum lyophilized powder；
S2 is obtained P. kingianum extract freeze-drying powder；
S3 tabletting: carry out tabletting with P. kingianum extract freeze-drying powder after described fresh P. kingianum lyophilized powder is mixed, prepared Yunnan is yellow
Smart buccal tablet.
2. a kind of P. kingianum process for preparing buccal lozenge according to claim 1 it is characterised in that: in s1 step, fresh P. kingianum freezes
Dry powder is prepared from using following methods: takes fresh P. kingianum to carry out lyophilization, temperature is -35～-45 DEG C so that fresh P. kingianum
Water content is less than 10%, then is ground into powder and obtains fresh P. kingianum lyophilized powder.
3. a kind of P. kingianum process for preparing buccal lozenge according to claim 1 it is characterised in that: in s2 step P. kingianum extract
Thing lyophilized powder is prepared from using following methods:
S2-1 pretreatment: fresh P. kingianum is pulverized, adds enzymolysis solution to be digested afterwards, obtain solidliquid mixture a；
S2-2 effective component extracting: the effective ingredient in solidliquid mixture a is extracted, obtains effective ingredient liquid；
S2-3 concentrates: effective ingredient liquid is concentrated, obtains concentrated solution；
S2-4 powder: concentrated solution is carried out lyophilization, obtains P. kingianum extract freeze-drying powder.
4. a kind of P. kingianum process for preparing buccal lozenge according to claim 3 it is characterised in that: described step s2-2 is extracted
Effective ingredient comprises the following steps:
S2-2-1 first time effective component extracting: add cold water to be extracted in solidliquid mixture a, the cold water of described addition makes
Obtaining solid-to-liquid ratio is 1:10～20, and cold water temperature is 20～30 DEG C, separates and obtains liquid phase part b and solid fraction b；
Second effective component extracting of s2-2-2: add hot water to be extracted in solid fraction b, the hot water of described addition makes
Solid-to-liquid ratio is 1:8～18, and hot water temperature is 60～80 DEG C, separates and obtains liquid phase part c and solid fraction c；
S2-2-3 third time effective component extracting: add ethanol to be extracted in solid fraction c, the ethanol of described addition makes
Solid-to-liquid ratio is 1:8～15, and ethanol temperature is 70～85 DEG C, separates and obtains liquid phase part d and solid fraction d；
Liquid phase part b, liquid phase part c, liquid phase part d are effective ingredient liquid, and liquid phase part b, liquid phase part c, liquid phase part d divide
Not after s2-3 concentration and s2-4 powder, then carry out being mixed to get P. kingianum extract freeze-drying powder.
5. a kind of P. kingianum process for preparing buccal lozenge according to claim 4 it is characterised in that: described step s2-3 concentrates
Step is that liquid phase part b is carried out membrance concentration, membrane aperture≤0.001 μm, and liquid phase part c and liquid phase part d adopts negative pressure evaporation
Concentrate, described negative pressure evaporation concentrates in the following ways: is maintained at very the pressure of liquid phase part c or liquid phase part d first
Reciprocal of duty cycle 0.01～0.05mpa 20～60 minutes, then keeps pressure to reduce 10～20 in 0.05～0.1mpa to liquid volume
Times, described negative pressure evaporation concentrates overall process liquid and all keeps less than 80 DEG C.
6. a kind of P. kingianum process for preparing buccal lozenge according to claim 4 it is characterised in that: described s2-4 milling step
For liquid phase part b concentrated after carry out lyophilization, temperature be -35～-45 DEG C, to water content be less than 10%；Liquid phase part c and
Carry out atomization drying after liquid phase part d is concentrated, be less than 10% to water content.
7. a kind of P. kingianum process for preparing buccal lozenge according to claim 1 it is characterised in that: in s3 step, by weight
Number calculates, and fresh P. kingianum lyophilized powder is 85～95 parts, and P. kingianum extract freeze-drying powder is 5～15 parts.
8. a kind of P. kingianum process for preparing buccal lozenge according to claim 1 it is characterised in that: in s3 step, will be described
After fresh P. kingianum lyophilized powder is mixed with P. kingianum extract freeze-drying powder, only spray water just carries out tabletting, and injection flow rate freezes for P. kingianum
Dry powder mix with P. kingianum extract freeze-drying powder after weight 0.1～0.3%.
9. a kind of P. kingianum process for preparing buccal lozenge according to claim 4 it is characterised in that:
In described s2-2-1 step, circulate this process 2～8 times, during circulation, total time controls in 0.5～8h；
In described s2-2-2 step, circulate this process 2～4 times, during circulation, total time controls in 0.1～4h.
10. a kind of P. kingianum buccal tablet it is characterised in that: be prepared from using any one preparation method in claim 1 to 9.
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| CN110934837B (en) * | 2019-12-16 | 2021-10-22 | 西藏天虹科技股份有限责任公司 | Polygonatum sibiricum polypeptide composite tablet and preparation method thereof |
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