CN106420834A - Deep processing preparation and quality control method of propolis composite - Google Patents

Deep processing preparation and quality control method of propolis composite Download PDF

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CN106420834A
CN106420834A CN201610967859.9A CN201610967859A CN106420834A CN 106420834 A CN106420834 A CN 106420834A CN 201610967859 A CN201610967859 A CN 201610967859A CN 106420834 A CN106420834 A CN 106420834A
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propolis
powder
preparation
raw material
thick paste
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CN106420834B (en
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何健
黄远英
殷光玲
张铭辉
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BY Health Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/63Arthropods
    • A61K35/64Insects, e.g. bees, wasps or fleas
    • A61K35/644Beeswax; Propolis; Royal jelly; Honey
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/16Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing nitrogen, e.g. nitro-, nitroso-, azo-compounds, nitriles, cyanates
    • A61K47/18Amines; Amides; Ureas; Quaternary ammonium compounds; Amino acids; Oligopeptides having up to five amino acids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity

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Abstract

The invention relates to a processing field of a propolis product, and particularly relates to a deep processing preparation method of the propolis powder and its product. The propolis composite is prepared by hardening and crushing the propolis raw material, and obtaining the propolis raw material powder; performing alcohol extraction on the propolis raw material powder, and obtaining the thick paste of the propolis extractive; mixing the propolis extractive thick paste with amino acid; grinding, cooling and drying, crushing and obtaining the propolis powder. The preparation method adds amino acid to the propolis extractive thick paste, thus the propolis and the amino acid can form an uniform system, thus the propolis can be smoothly dried, and the propolis powder with good powder property is obtained; meanwhile, the propolis powder prepared by the process is applicable to the propolis capsule (including hard capsule and soft capsule), propolis slice and others; the method can significantly improve the collapse problem of the propolis product.

Description

A kind of deep processing preparation of propolis complex and method of quality control
Technical field
The present invention relates to propolis manufacture field, particularly to a kind of deep processing preparation method and products thereof of propolis product.
Background technology
Propolis is the resin that Apiss gather from plant spore or trunk, is mixed into the secretions of palatine gland, wax gland thereon A kind of colloidal solid thing with aromatic odor processing.It is that Apidae animal apis cerana etc. is repaired secreted by Nidus Vespae Yellowish-brown or the stickum of pitchy, can be used as medicine.It is mild-natured, bitter in the mouth, pungent, micro-sweet, has skin moistening granulation promoting, the work(of anti-inflammatory analgetic Effect, can treat gastric ulcer, oral ulcer, burn and scald, skin splitting pain, the disease such as radioprotective.For many years, clinic is mainly used in capillary Vascular hemorrhage and secondary buck medicine.Except flavonoid beyond the region of objective existence, propolis also has fragrant volatile oil, alkene terpenoid, has Machine acids, flavanol compound, alcohol, phenol, aldehyde, ketone, ester, ether compound, enzyme and inorganic salt etc., propolis is natural just as one " Drug Storage ".Propolis has the good effect strengthening human immunity.With the increase of people's operating pressure and age, meanwhile, in Society of state enters the aging stage, and the physical function of people and immune level all begin to decline, and exploitation has increasing containing propolis The product of strong human immunity has large market prospect and social value.
Propolis through ethanol extraction, concentrate after, the extractum obtaining is very sticky, is generally difficult to drying, in order to allow extractum energy Smoothly it is dried, needs to add adjuvant inside, such as starch, maltodextrin, Lactose etc., but a large amount of due to also having inside propolis extractum The tannin constituents such as natural gum, resin, its Polarity comparision is weak, and bonding is agglomerating, tends not to mix homogeneously with adjuvant, and then can not obtain Carry out next step drying process to homogeneous system, the powder characteristicss leading to propolis powder poor it is impossible to formula for a product other Raw material uniformly mixes, final impact product formulation technique;Simultaneously as contain inside propolis carrying aldehyde, ketone, phenolic hydroxyl group in a large number Deng the compound of group, it is each other, can occur mutual condensation, friendship with amine groups of gelatin etc. in soft capsule dosage form Connection reaction, leads to the propolis powder that traditional handicraft is obtained to make tablet, hard capsule, after soft capsule, occur within the shelf-life Disintegrate exceeds the problem that Chinese Pharmacopoeia requires, and leads to product to be judged to unqualified.
Content of the invention
In view of this, the invention provides deep processing preparation method of a kind of propolis powder and products thereof.This preparation method is led to Cross and aminoacid is added in propolis extract thick paste, propolis and aminoacid can form homogeneous system, so that propolis energy Enough smoothly it is dried, obtains the good propolis powder of powder characteristicss, thus avoiding propolis powder and aminoacid incomplete mixing, preparation process Difficulty and tablet, capsule (including hard capsule and soft capsule) the underproof problem of disintegrate.
In order to realize foregoing invention purpose, the present invention provides technical scheme below:
The invention provides a kind of preparation method of propolis powder, comprise the steps:
Step 1:Propolis raw material is hardened, pulverizes, obtain propolis raw material powder;Described propolis raw material powder is carried out alcohol extraction, obtains To ethanol extracts of propolis;
Step 2:Ethanol extracts of propolis is carried out concentrating under reduced pressure, is centrifuged after cooling, extracting centrifugal liquid concentrating under reduced pressure, obtains propolis and carry Take thing thick paste.
Step 3:Described propolis extract thick paste is mixed with aminoacid, grinds, lyophilization, pulverize, obtain propolis powder.
This technique is passed through to add aminoacid (arginine, lysine, tryptophan etc.) in propolis production process, can make honeybee Glue extractum can be mixed with aminoacid, and using freeze drying process, thick paste is dried well, finally gives powder characteristicss Good propolis powder, this product avoids propolis extractum and adjuvant mixes irregular problem, and the problem being dried.
Preferably, aminoacid is selected from arginine, lysine, tryptophan, alanine, L-Valine, leucine, different bright ammonia Acid, Methionine, aspartic acid, glutamic acid, glycine, serine, threonine, cysteine, agedoite propylhomoserin, glutamy One or more of amine, Phenylalanine, tyrosine or proline.
Preferably, aminoacid is selected from one or more of Methionine, arginine, cysteine, lysine or histidine.
Preferably, the ratio of aminoacid and propolis extract thick paste is 0.2~1:1;
Preferably, the ratio of aminoacid and propolis extract thick paste is 0.3~0.8:1;
It is highly preferred that the ratio of aminoacid and propolis extract thick paste is 0.4~0.6:1;
In the embodiment that the present invention provides, step 1 is specially:Propolis raw material powder is mixed with the first ethanol water, Stirring is extracted;Gained filtering residue is mixed with the second ethanol water, stirring is extracted, merging filtrate obtains propolis extracted with alcohol.
Preferably, in terms of g/mL, the mass volume ratio of propolis raw material powder and the first ethanol water is 1:(4~20).
Preferably, in terms of g/mL, the mass volume ratio of propolis raw material powder and the first ethanol water is 1:(6~16).
Preferably, in terms of g/mL, the mass volume ratio of filtering residue and the second ethanol water is 1:(4~20).
Preferably, in terms of g/mL, the mass volume ratio of filtering residue and the second ethanol water is 1:(6~16).
Preferably, the volumetric concentration of the first ethanol water or the second ethanol water is 40%~85%.
Preferably, the volumetric concentration of the first ethanol water or the second ethanol water is 60%~80%.
Preferably, the temperature that stirring is extracted is 15~30 DEG C, the time is 1~3h.
Preferably, the step that step 2 is centrifuged after including concentrating and cooling down.
Preferably, concentrating as concentrating under reduced pressure, it is centrifuged as high speed centrifugation.
Preferably, the vacuum of concentrating under reduced pressure is -0.01~-0.1MPa, temperature is 50-80 DEG C, is concentrated into propolis former 3~5 times of volumes of material;After being cooled to 10-15 DEG C, it is centrifuged 5-10min under 1000-2000r/min rotating speed.
Preferably, the vacuum of concentrating under reduced pressure is -0.06~-0.1MPa, and temperature is 60-70 DEG C, is concentrated into propolis raw material 3~5 times of volumes;It is subsequently cooled to 10-12 DEG C, be centrifuged 8-10min under 2000r/min rotating speed;Take interlude centrifugal liquid, Vacuum is -0.06~-0.1MPa, and temperature is 60-70 DEG C, and being concentrated into relative density is 1.02-1.10.
Preferably, the revolution of the grinding of step 3 is 2000r/min, the time of grinding is 5~30min.
In some embodiments that the present invention provides, propolis raw material is Brazilian apiario silvestre raw material.
Preferably, hardening is by the way of freezing in step 1.The temperature of freezing is -20 DEG C -0 DEG C, and the time of freezing is More than 3 hours.
In some embodiments that the present invention provides, the temperature of freezing is -20 DEG C, and the time of freezing is 3 hours.
Preferably, the temperature of freezing is -15~-20 DEG C, the time is 2.5~3h.
Preferably, the mesh number pulverized in step 3 is 20~40 mesh.
Present invention also offers the propolis powder being obtained by preparation method of the present invention.
Present invention also offers a kind of bee glue preparation, the propolis powder being obtained including preparation method of the present invention.
Preferably, the dosage form of bee glue preparation is tablet, hard capsule, soft capsule, oral liquid.
The invention provides a kind of preparation method of propolis powder and products thereof.This preparation method includes:Propolis raw material is hard Change, pulverize, obtain propolis raw material powder;Propolis raw material powder is carried out the steps such as alcohol extraction, concentrating under reduced pressure, centrifugation and obtains propolis extract Thick paste;Propolis extract thick paste is mixed with aminoacid, grinds, lyophilization, pulverize, obtain propolis powder.The present invention at least has There is one of following advantage:
1st, by being added to aminoacid in propolis extract thick paste, propolis can be formed preparation method of the present invention with aminoacid Homogeneous system, so that propolis can smoothly be dried, obtains the good propolis powder of powder characteristicss;Decrease adjuvant in formula Consumption.
2nd, the present invention provide propolis powder good fluidity, be conducive to preparation process, can make further tablet, capsule, The products such as oral liquid.
3rd, the function that this product has antioxidation and strengthens immunity.
4th, compared with the propolis powder of traditional handicraft, this technique be obtained propolis powder can significantly improve propolis product dissolution and Disintegration time, reaches improve product quality and the purpose of product curative effect.
Specific embodiment
The invention discloses a kind of preparation method of propolis powder and products thereof, those skilled in the art can use for reference interior herein Hold, be suitably modified technological parameter and realize.Specifically, all similar replacements and change are to those skilled in the art For be it will be apparent that they are considered as including in the present invention.Preferable enforcement has been passed through in the method for the present invention and application Example is described, related personnel substantially can in without departing from present invention, spirit and scope to method described herein and Application is modified or suitably changes and combine, and to realize and to apply the technology of the present invention.
In preparation method of propolis powder and products thereof that the present invention provides, raw materials used or adjuvant all can be buied by market.
With reference to embodiment, the present invention is expanded on further:
The preparation of embodiment 1 propolis powder
1st, pre-treatment
Brazilian apiario silvestre raw material is freezed 3 hours at -20 DEG C, so that propolis is hardened;Then pulverized using pulverizer, obtained To propolis powder raw material;
2nd, extract
Take the propolis raw material after pulverizing, put in extraction pot, add 85% alcohol at normal temperature stirring of medical material weight 4 times amount volume Extract 3 hours, filter, filtrate is separately deposited;Medicinal residues add the stirring of 4 times amount 85% alcohol at normal temperature and extract 3 hours, filter, take filtrate, merge Extracting solution.
3rd, concentrate and grind
Test group:Take propolis ethanol extract to concentrating under reduced pressure in concentrator, vacuum degree control is -0.01MPa, temperature is 50 DEG C, it is evaporated to when being equivalent to 3 times of volumes of inventory, feed liquid is cooled to 15 DEG C, be centrifuged under 2000r/min speed 5min, after removing upper strata float, extracting centrifugal liquid continues concentrating under reduced pressure, is 1.10 to relative density, obtains propolis extract thick paste; By every part of propolis and amino acid/11:0.2 ratio adds arginine;With colloid mill, thing mixed above is carried out with 5 points of speed lapping Clock, obtains mixing homogeneous propolis extracted with alcohol thick paste.
Matched group:Do not add aminoacid, the same test group of other operation.
4th, it is dried
Take the propolis extracted with alcohol thick paste after grinding, be laid in pallet, carry out lyophilization.
5th, pulverize
When drying to moisture is less than 6%, take out propolis dry extract, pulverized with pulverizer, obtain propolis powder finished product.
6th, powder characteristicss detection
Table 1 powder characteristicss testing result
Result of the test shows, same specification (the aminoacid addition of test group is identical with the adjuvant addition of matched group) Under, the powder fluidity of test group is significantly better than matched group;And, under same environmental condition, the hygroscopicity of matched group is bright Aobvious, it is heated and lump.
The preparation of embodiment 2 propolis powder
1st, pre-treatment
Brazilian apiario silvestre raw material is freezed 3 hours at -20 DEG C, so that propolis is hardened;Then pulverized using pulverizer, obtained To propolis powder raw material;
2nd, extract
Take the propolis raw material after pulverizing, put in extraction pot, add 75% alcohol at normal temperature of medical material weight 10 times amount volume to stir Mix extraction 2 hours, filter, filtrate is separately deposited;Medicinal residues add the stirring of 10 times amount 75% alcohol at normal temperature and extract 2 hours, filter, take filtrate, United extraction liquid.
3rd, concentrate and grind
Test group:Take propolis ethanol extract to concentrating under reduced pressure in concentrator, vacuum degree control is -0.03MPa, temperature is 60 DEG C, it is evaporated to when being equivalent to 4 times of volumes of inventory, feed liquid is cooled to 10 DEG C, be centrifuged under 1500r/min speed 8min, after removing upper strata float, extracting centrifugal liquid continues concentrating under reduced pressure, is 1.08 to relative density, obtains propolis extract thick paste; By every part of propolis and amino acid/11:0.4 ratio adds kilnitamin (lysine:Histidine=1:1), with colloid mill to Upper mixture carries out speed lapping 10 minutes, obtains mixing homogeneous propolis extracted with alcohol thick paste.
Matched group:Do not add aminoacid, the same test group of other operation.
4th, it is dried
Take the propolis extracted with alcohol thick paste after grinding, be laid in pallet, carry out lyophilization.
5th, pulverize
When drying to moisture is less than 6%, take out propolis dry extract, pulverized with pulverizer, obtain propolis powder finished product.
6th, powder characteristicss detection
Table 2 powder characteristicss testing result
Result of the test shows, same specification (the aminoacid addition of test group is identical with the adjuvant addition of matched group) Under, the powder fluidity of test group is significantly better than matched group;And the material propertiess of matched group are gently steeped, there are hygroscopic effect, mobility Very poor, be not suitable for direct compression or filled hard capsules;And the good fluidity of test group, can be with direct compression or filled hard Capsule.
The preparation of embodiment 3 propolis powder
1st, pre-treatment
Brazilian apiario silvestre raw material is freezed 3 hours at -20 DEG C, so that propolis is hardened;Then pulverized using pulverizer, obtained To propolis powder raw material;
2nd, extract
Take the propolis raw material after pulverizing, put in extraction pot, add 40% alcohol at normal temperature of medical material weight 20 times amount volume to stir Mix extraction 1.5 hours, filter, filtrate is separately deposited;Medicinal residues add the stirring of 20 times amount 40% alcohol at normal temperature and extract 1.5 hours, filter, take filter Liquid, united extraction liquid.
3rd, concentrate and grind
Test group:Take propolis ethanol extract to concentrating under reduced pressure in concentrator, vacuum degree control is -0.06MPa, temperature is 70 DEG C, it is evaporated to when being equivalent to 3 times of volumes of inventory, feed liquid is cooled to 15 DEG C, be centrifuged under 1000r/min speed 10min, after removing upper strata float, extracting centrifugal liquid continues concentrating under reduced pressure, is 1.06 to relative density, obtains propolis extract thick paste; By every part of propolis and amino acid/11:1 ratio adds kilnitamin (arginine:Methionine:Cysteine=1:1:1)), use Colloid mill carries out speed lapping 20 minutes to thing mixed above, obtains mixing homogeneous propolis extracted with alcohol thick paste.
Matched group:Do not add aminoacid, the same test group of other operation.
4th, it is dried
Take the propolis extracted with alcohol thick paste after grinding, be laid in pallet, carry out lyophilization.
5th, pulverize
When drying to moisture is less than 6%, take out propolis dry extract, pulverized with pulverizer, obtain propolis powder finished product.
6th, powder characteristicss detection
Table 3 powder characteristicss testing result
Result of the test shows, same specification (the aminoacid addition of test group is identical with the adjuvant addition of matched group) Under, the powder fluidity of test group is significantly better than matched group;Matched group material seems and gentlier steeps, and is not suitable for direct compression or fills out Fill hard capsule.
The preparation of embodiment 4 bee glue soft capsule and nature examination
Test group product content composition formula:
Table 4 propolis soft capsule content formula
Raw material Ratio
The propolis powder of embodiment 1 5 parts
Soybean oil 4.8 part
Natural Vitamin E 0.1 part
Cera Flava 0.1 part
Test set product rubber formula:
Table 5 bee glue soft capsule rubber formula
Raw material Ratio
Gelatin 4.4 part
Water 3 parts
Glycerol 2.5 part
Caramel color 0.1 part
Matched group:Using the matched group propolis powder in embodiment 1, other components and operate same test group.
Preparation technology:By the being proportionally added into glue tank such as gelatin, water, glycerol, caramel color, by change glue post operation code Operated, prepared glue insulation is standby;Separately take propolis powder, soybean oil, antioxidant, Cera Flava etc. to be mixed in proportion, grind Carry out pelleting by pelleting post operation code afterwards, gained soft capsule is dried by drying process, obtains bee glue soft capsule finished product.
Nature examination:
Study on the stability:By the soft gel products of test group and matched group be placed in 45 DEG C, carry out under conditions of RT75% steady Qualitative investigation, the disintegration time result in contrast 0~March of acceleration.
The disintegration time measurement result that table 6 Stability of Soft Capsules is investigated
Sample 0 month Accelerate January Accelerate 2 months Accelerate March
Experimental group 7min 20min 35min 42min
Matched group 7min 41min > 60min > 60min
Result of the test shows, experimental group bee glue soft capsule accelerate 3 months in disintegration time maintain 60 minutes within, Meet product quality to require;The disintegration time when accelerating 2 months for the matched group bee glue soft capsule was more than 60 minutes;Result illustrates, Propolis powder under this technique can improve the effective ingredient dissolution of soft capsule dosage form, improves the effectiveness of product.
The preparation of embodiment 5 propolis tablet and nature examination
Test group formula for a product:
Table 7 propolis slice prescription
Raw material Ratio
The propolis powder of embodiment 2 4.5 part
Hydroxyl isomaltulose 5.4 part
Magnesium stearate 0.05 part
Silicon dioxide 0.05 part
Matched group:Using the matched group propolis powder in embodiment 2, other components and operate same test group.
Preparation technology:Propolis powder, adjuvant etc. are always mixed, pelletize after pressing blade technolgy carry out tabletting, products obtained therefrom coating or Not coating, obtains propolis tablet finished product.
Nature examination:
Study on the stability:By the tablet of test group and matched group be placed in 45 DEG C, carry out under conditions of RT75% stable Property investigate, contrast 0~March of acceleration disintegration time result.
The disintegration time measurement result of table 8 propolis tablet study on the stability
Sample 0 month Accelerate January Accelerate 2 months Accelerate March
Experimental group 10min 30min 35min 43min
Matched group 10min 41min > 60min > 60min
Result of the test shows, experimental group propolis tablet, within accelerating the disintegration time in 3 months to maintain 60 minutes, meets Product quality requires;The disintegration time when accelerating 2 months for the matched group propolis tablet was more than 60 minutes;Result illustrates, under this technique Propolis powder can improve the effective ingredient dissolution of propolis in propolis tablet, improve the effectiveness of product.
The preparation of embodiment 6 propolis hard capsule and nature examination
Test group formula for a product:
Table 9 propolis ebonite capsule formula
Raw material Ratio
The propolis powder of embodiment 3 9.7 part
Magnesium stearate 0.3 part
Matched group:Using the matched group propolis powder of embodiment 3, other components and operate same test group.
Preparation technology:The adjuvants such as propolis powder, appropriate magnesium stearate are proportionally added into, after mixing, use hard capsule filling machine It is filled in hard capsule case.
Nature examination:
Study on the stability:The tablet of test group and matched group is placed in 45 DEG C, carries out stable under conditions of RT75% Property investigate, contrast 0~March of acceleration disintegration time result.
The disintegration time measurement result of table 10 propolis hard capsule study on the stability
Sample 0 month Accelerate January Accelerate 2 months Accelerate March
Experimental group 12min 24min 25min 24min
Matched group 12min 35min 51min > 60min
Result of the test shows, experimental group propolis hard capsule accelerate 3 months in disintegration time maintain 30 minutes within, Meet product quality to require;Matched group bee glue soft capsule accelerate 3 months when disintegration time more than 60 minutes, and, accelerate 1 When, hard capsule content has conglomeration existing, the dissolution of impact effective ingredient;Result illustrates, the propolis powder under this technique can change The effective ingredient dissolution of kind hard capsule dosage form, improves the effectiveness of product.
Embodiment 7 apiario silvestre Determination Method of Flavone Content (in terms of pinocembrin)
1st, principle:
The flavone compound being dissolved in ethanol, under weak basic condition, is combined generation colored substance with developer trivalent aluminium ion Matter, can produce absorption maximum near 303nm wavelength.In the range of finite concentration, its absorbance is contained with flavone compound Amount is directly proportional.Compare with standard curve, the content of flavone compound can be quantitative determined.
2nd, instrument and equipment:
XA204 analytical balance, UV2450 spectrophotometer, centrifuge.
3rd, reagent:
Pinocembrin standard substance:National Institute for Food and Drugs Control, content:99.8%.
Aluminum nitrate solution (100g/L):Weigh Al (NO3)3.9H2O 17.60g, is dissolved in water, and constant volume is in 100mL volumetric flask In, shake up;
Liquor kalii acetici (9.8g/100mL):Weigh potassium acetate 9.814g, be dissolved in water, constant volume in 100mL volumetric flask, Shake up;
Pinocembrin standard solution:Weigh 10mg pinocembrin reference substance, plus 80% ethanol dissolves and is settled to 50mL, obtains final product.
Test sample is bee glue soft capsule.
4th, analytical procedure:
4.1 standard curve preparations:
Draw pinocembrin standard solution:0.0th, 0.5,1.0,2.0,3.0,4.0mL, in 50mL volumetric flask, sequentially adds nitre Sour aluminum solutions 1mL, liquor kalii acetici 1mL, shake up, plus 80% ethanol, to scale, shakes up, and stand 1h.With 1cm cuvette in At 303nm, with 0 pipe standards solution as blank, mensuration absorbance.With 50mL pinocembrin concentration (mg) as abscissa, absorbance is Vertical coordinate, draws standard curve.
4.2 sample determination:
Weigh the sample 0.1g product of mix homogeneously, to 50mL volumetric flask, plus the dissolving of 80% appropriate amount of ethanol, ultrasonic 30min is completely loose to sample, fully extracts;Let cool, be settled to scale, shake up, 8000r/min is centrifuged 5min.Accurate absorption Sample supernatant 1.0mL, is placed in 50mL volumetric flask, is operated by 4.1.Use 1cm cuvette, measure at wavelength 303nm The absorbance of sample solution.Look into standard curve, obtain the flavonoid content (mg) in sample solution.
4.3 results calculate:
Table 11 general flavone content testing result
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of propolis powder is it is characterised in that comprise the steps:
Step 1:Propolis raw material is hardened, pulverizes, obtain propolis raw material powder;Described propolis raw material powder is carried out alcohol extraction, obtains honeybee Glue alcohol extract;
Step 2:Ethanol extracts of propolis is carried out concentrating under reduced pressure, is centrifuged after cooling, extracting centrifugal liquid concentrating under reduced pressure, obtains propolis extract Thick paste;
Step 3:Described propolis extract thick paste is mixed with aminoacid, grinds, lyophilization, pulverize, obtain propolis powder.
2. preparation method according to claim 1 is it is characterised in that described aminoacid is selected from arginine, lysine, color ammonia Acid, alanine, L-Valine, leucine, isoleucine, Methionine, aspartic acid, glutamic acid, glycine, serine, threonine, One or more of cysteine, agedoite propylhomoserin, L-Glutamine, Phenylalanine, tyrosine or proline.
3. preparation method according to claim 1 and 2 is it is characterised in that described aminoacid is thick with described propolis extract Cream ratio is 0.2~1:1.
4. preparation method according to any one of claim 1 to 3 is it is characterised in that described step 2 is specially:By honeybee Collagen feed powder is mixed with the first ethanol water, and stirring is extracted;Gained filtering residue is mixed with the second ethanol water, stirring carries Take, merging filtrate, obtain propolis extracted with alcohol.
5. preparation method according to claim 4 is it is characterised in that in terms of g/mL, described propolis raw material powder and described the The mass volume ratio of one ethanol water is 1:(4~20);Described filtering residue and the mass volume ratio of described second ethanol water For 1:(4~20);The volumetric concentration of the first ethanol water or described second ethanol water is 40%~85%;Described stirring The temperature extracted is 15~30 DEG C, and the time is 1~3h.
6. preparation method according to any one of claim 1 to 5 is it is characterised in that concentrating under reduced pressure in described step 2 Vacuum be -0.01~-0.1MPa, temperature be 50-80 DEG C, be concentrated into described propolis raw material 3-5 times of volume when, will concentrate Liquid is cooled to 10~15 DEG C, is then centrifuged 5~10min under 1000~2000r/min speed, and extracting centrifugal liquid continues to be concentrated into phase It is 1.02~1.10 to density, obtain propolis extract thick paste.
7. the propolis powder that preparation method as any one of claim 1 to 6 is obtained.
8. a kind of bee glue preparation is it is characterised in that include propolis powder as claimed in claim 7.
9. bee glue preparation according to claim 8 is it is characterised in that the dosage form of described bee glue preparation is tablet, hard capsule Agent, soft capsule, oral liquid.
10. as described in claim 8 or 9, bee glue preparation has in enhancing immunity and/or the medicine of anti-oxidation efficacy in preparation Application.
CN201610967859.9A 2016-11-03 2016-11-03 A kind of deep processing preparation of propolis compound and method of quality control Active CN106420834B (en)

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CN109260234A (en) * 2018-09-28 2019-01-25 广东青云山药业有限公司 A kind of green bee glue powder of Brazil and preparation method thereof
CN110959830A (en) * 2019-12-18 2020-04-07 宁波杰顺生物科技有限公司 Bee product and preparation method thereof

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