CN108743621A - The bear gall powder and preparation method of ice crystal state - Google Patents
The bear gall powder and preparation method of ice crystal state Download PDFInfo
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Abstract
The invention discloses a kind of bear gall powder and preparation method of ice crystal state, which is the burnished gold or bright-yellow powder of hyaloid gloss, shows glassy yellow fluorescence, and hydroscopicity is less than 2%, and solubility is more than 10% in water, and the solubility in ethyl alcohol is more than 1.2g%.By making material ice crystalization then by freeze-drying in the preparation process of bear gall powder, bear gall powder obtained is presented excellent technique effect, excellent technique effect is especially for example presented in physics and chemistry properties the present invention.Particularly, the present invention is diluted with a small amount of water in advance when preparing bear gall powder, it fills and then carries out cryogenic refrigeration, contained active constituent in bear gall juice is set to be in a kind of ice crystal state, then it distils, thus gained freeze-drying bear gall powder can be referred to as ice crystal state bear gall powder in the present invention, or can be described as ice crystal bear gall powder.Especially the present invention can be referred to as the bear gall powder of the gloomy precious bear gall powder of a new generation without any auxiliary material and chemical addition agent.
Description
Technical field
The invention belongs to the technical fields of medical and health product, are related to a kind of bear gall powder being prepared by special process,
Further relate to the preparation method of this bear gall powder.The present invention in the preparation process of bear gall powder by making material ice crystalization then pass through
Freeze-drying, bear gall powder obtained are presented excellent technique effect, excellent skill are especially for example presented in physics and chemistry properties
Art effect.Particularly, the present invention is diluted with a small amount of water in advance when preparing bear gall powder, is then carried out cryogenic refrigeration afterwards, is made bear gall
Contained active constituent is in a kind of ice crystal state in juice, then distils, and thus gained freeze-drying bear gall powder is in the present invention
In can be referred to as ice crystal state bear gall powder, or can be described as ice crystal bear gall powder.Especially the present invention can be referred to as a new generation
The bear gall powder of gloomy treasured bear gall powder is free of any auxiliary material and chemical addition agent.
Background technology
More《Chinese Pharmacopoeia》The medicinal material of the bile with bear gall and/or its secretion is recorded or comprising its preparation.Example
Such as, version in 2005《Chinese Pharmacopoeia》It is ursidae animal black bear Selenarctos that medicinal material bear gall has been recorded in one annex 24
The drying gall-bladder of thibetanus Cuvier or brown bear Ursus arctos Linnaeus.Version in 2010《Chinese Pharmacopoeia》One
It is that ursidae animal black bear Selenarctos thibetanus Cuvier draw through operation on gallbladder that bear gall powder has been recorded in annex 27
Flow dry product obtained by bile；This edition pharmacopeia one has also recorded bear gall capsule, bear gall pills for curing heart disease/pellet, bear gall hemorrhoid spirit cream etc.
It is preparation made of raw material including bear gall powder.Version in 2015《Chinese Pharmacopoeia》One has been recorded bear gall capsule, the Xiongdan Jiuxin heart
Ball, bear gall hemorrhoid spirit cream, bear gall ZHILING SHUAN etc. are preparation made of raw material including bear gall powder.
Currently, substitute of the dry product of drain-out bear gall's bile as natural bear gall is used as medicine and examines listing, life
Entitled bear gall powder is a kind new medicine of health ministry approval.Bear gall powder is that ursidae animal black bear drains courage by operation on gallbladder
Dry product obtained by juice, cold in nature, bitter enter liver, courage, spleen, stomach, large intestine channel, have heat-clearing, soothing the liver, the work(of improving eyesight.Modern study
It was found that bear gall powder chemical composition is more complicated, main ursodesoxycholic acid containing mating type (UDCA), chenodeoxycholic acid (CDCA), courage
Sour (CA), deoxycholic aicd (DCA), Tauro ursodesoxy cholic acid (TUDCA), Taurochenodeoxycholic Acid (TCDCA) and cholesterol, courage
Pigment, amino acids, protein, peptide, aliphatic acid, trace element etc..Wherein ursodesoxycholic acid is important characteristic component.Mesh
It is preceding to be clinically mainly used in the diseases in the liver and gallbladder such as gall stone, fatty liver, cholecystitis, virus hepatitis, chronic hepatitis B, eyelid
Herpes zoster, the diseases such as hemorrhoid.
CN103520210A (201310523280.X, Sheng Yuantang) discloses a kind of bear gall powder purification process, including as follows
The step of sequence carries out：(1) polyvinylpyrrolidone (PVP) and sterile water distilled water are added in freshly extd bear gall juice,
Mixing is shaken, clarification is stood, obtains supernatant；(2) absolute ethyl alcohol of 2 times of volumes is added in gained supernatant in step (1),
Bear gall alcohol extract is made；(3) macro porous silica gel pillar is added in bear gall purification obtained by step (2), it is anhydrous using 2 times of volumes 75%
Ethyl alcohol, which divides 3 times, washs silicon gel column, collects cleaning solution；(4) with sterile distilled water to gained cleaning solution in step (3) into
Row dilution so that a concentration of the 16.5% of absolute ethyl alcohol；(5) by bear gall of the gained containing 16.5% absolute ethyl alcohol in step (4)
Juice supernatant is added in cellulose powder CF11 pillars, vortex oscillation mixing, progress bear gall juice separation, under the conditions of 5000rpm, from
After centrifugation, isometric sterile distilled water is added in heart 5min in cellulose powder CF11 pillars, under the conditions of 5000rpm,
Centrifuge 5min；(6) gained supernatant in collection step (5), is added the 3mol/L NaAc of 1/10 volume and isometric isopropyl
Alcohol, mixing, 20 DEG C precipitate, and after the completion of precipitation, under the conditions of 4 DEG C, 12000rpm centrifuges 30min, abandons supernatant, collects precipitation； (7)
75% absolute ethyl alcohol is added to wash the precipitation collected in step (6), after washing, under 4 DEG C of environment, 12000rpm
30min is centrifuged, supernatant is abandoned, collects precipitation；(8) it by gained precipitation in step (7), is dissolved in distilled water, stirs 1 to 3 hour,
Bear gall solution is made, it is 2 to 8 to adjust pH, is heated to 50 DEG C and keeps the temperature, addition compound protease, after enzymolysis, is gone out
Enzyme carries out ultrafiltration membrance filter, can be obtained bear gall powder finished product after the supernatant of acquisition is spray-dried.It is believed that the inventive technique institute
Bear gall powder is obtained, effective content is high, and pigment content is low, no fishy smell, and medical value is promoted.
CN105147729A (201510650516.5, pasture river) discloses a kind of preparation method of bear gall powder, and step includes：
(A), it filters：Fresh drained bear bile is taken, filters, obtains filtrate；(B), it sterilizes：High concentration ethanol, ethyl alcohol are added in filtrate
Ethanol content is 75%~85% in liquid after addition, is then stirred, and is stood, and mixing time is 20~40 minutes, is stood
Time is 24~72 hours；(C), it concentrates：It is concentrated under reduced pressure and removes ethyl alcohol, reduced pressure carries out at 35~45 DEG C, is concentrated under reduced pressure
After obtain sterilizing bear bile fluid；(D), it is freeze-dried：Sterilizing bear bile fluid is freeze-dried, and the method for the freeze-drying is：
Sterilizing bear bile fluid is cooled to 35~40 DEG C, 0.5~3.5h of constant temperature with the rate of temperature fall of 1~2 DEG C/min, it is evacuated to 1~
15Pa, then room temperature is warming up to the heating rate of 1~3 DEG C/min.It is believed that the characteristics of invention utilizes new fresh bear bile to be liquid,
It is miscible with bile using ethyl alcohol, using ethyl alcohol to virus, pathogenic bacteria killing effect, by control ethyl alcohol in liquid content and
Time does not destroy the active constituent in bear gall juice, kills various pathogenic bacteria and virus, ensure clinical application safety, effectively
Property, the defect of traditionally bear gall powder production is overcome, gained bear gall powder appearance is golden yellow, has transparent gloss, greatlys improve
Bear gall powder quality.
The method that CN106386659A (201610755739.2, day is helped) discloses bear gall powder factorial praluction, this method
Selection including black bear breeding raises, takes courage, feeding Chinese herbal medicine, cryogenic temperature freezing drying, specific as follows：(1) black bear breeding
Selection：Select healthy and strong, varietal characteristic is apparent, feeding power is strong, production performance is good, constitution is solid, limb hoof is healthy and strong, 3 years old or more
Black bear do culture bear；(2) it raises：Culture bear is fed using mixed feed, the mixed feed matching in mass ratio
Than for：50~60 parts of corn, 3~5 parts of fish meal, 10~15 parts of barley, 10~15 parts of the soybean fried, 3~5 parts of meat, silkworm chrysalis 3
~5 parts；Nursing starts to take courage when reaching 90 ㎏ or more to black bear weight；(3) courage is taken：Using the painless drainage of the self tubing of animal
Method adopts courage, and specific practice is, between the stomach wall and gall-bladder of black bear, is woven in stomach wall end using the group of black bear itself and manufactures annular
Sphincter, when sphincters contract, can close tube chamber, and when diastole makes tube chamber open, domination or hormone of the sphincter by autonomic nerve
It adjusts, using this characteristic, nutrient solution is fed to black bear when adopting courage, black bear sphincter relaxation, tube chamber is made to open, be disappeared with cotton ball soaked in alcohol
Stainless steel hollow probe after disinfection is probeed into tube chamber channel by the open tube chamber passway of poison, bile i.e. along hollow probe from
Dynamic flow to connects in the cup of bile, takes extraction probe after the completion of courage；(4) Chinese herbal medicine is fed：After the completion of taking courage, fed to black bear
The Chinese herbal medicine of syrup water is added in clothes, continuously feeds 10 days；The Chinese herbal medicine formula is：20~30 parts of Cortex Magnoliae Officinalis, 20~30 parts of green peel,
20~30 parts of Chinese cassia tree, 20~30 parts of spinach；20~30 parts of the fleece-flower root, 20~30 parts of Radix Glycyrrhizae, 20~30 parts of folium isatidis, Radix Isatidis 20
~30 parts；20~30 parts of corn protein powder, 20~30 parts of analysis for soybean powder, 20~30 parts of walnut dregs, 20~30 parts of peanut cypress；The fruit of glossy privet
40~50 parts, 40~50 parts of adlay, 5~10 parts of dried orange peel, 5~10 parts of ginger；Said herbal medicine is crushed and is added after mixing
Enter syrup water and feeds black bear；(5) cryogenic temperature freezing drying：By the bear gall juice of taking-up in advance -60 DEG C of temperature and it is following freeze, so
It is placed under vacuum state, the water sublimed contained obtains dry bear gall powder.It is believed that the inventive method was prepared
Bear gall powder quality is good, yield is high and is not injured to black bear body.
CN102114044A (201010617773.6, Gui Zhentang) discloses a kind of extracting method of bear gall juice, in bear
Wound is cut on gall-bladder, and forms fistula with musculature, is tightened；Fistula mouth acquisition bile is squeezed after recovery from illness.This method can be used for
It is discontinuous, at regular time and quantity and long-term acquisition, and bear itself will not be impacted using bile.The invention discloses a kind of excellent
Matter bear gall powder and preparation method thereof, the bear gall powder are in glassy yellow fluorescence under 365nm ultraviolet lamps, there is 3 colors at 198nm
Spectral peak；Preparation method include by bile stand, separation, crushed after being dried sieving to get.It is believed that outside bear gall powder prepared by the invention
Pure color is seen, Tauro ursodesoxy cholic acid content is high in bear gall powder, nonhygroscopic, is conducive to storage and transportation and processing.
CN103040869A (201310027917.6, Kang Ao) discloses a kind of artificial bear gall powder, and it is original that it, which is by fowl courage,
Material is added cow-bezoar sodium ursodexoxycholate and is prepared, and wherein cow-bezoar sodium ursodexoxycholate and the weight proportion of fowl courage is：Cow-bezoar bear
20-40 parts of deoxysodium cholate, 80-60 parts of fowl courage.The present invention also provides the preparation methods of the artificial bear gall powder.Invention is not only matched
Fang Kexue is unique, raw material is easy to get, is simple for process, is of low cost, ensures quality, ensure curative effect, save the wild animals, and inherent
Quality and appearance character are all almost close with natural bear gall, provide a simplicity, economy, safe and environment-friendly, and quality and appearance are all
It is the ideal substitute of natural bear gall with the extremely similar artificial bear gall powder of natural bear gall.
CN1311002A (00102073.0, Shi Lixia) discloses a kind of refined bear gall powder and preparation method thereof, belongs to pharmacy
The common bear gall powder in field easy moisture absorption caking, there is that tooth gluing sense, taste are extremely stench, extremely bitter, impurity is more, absorption is slow, and property is unstable easy
Corruption, effective component content is low, limits the application range of bear gall powder, and when oral application is commonly incorporated into flavoring agent, mitigates bad smell.
The invention is refined using ethanol extraction method, ethyl alcohol extraction activated carbon decolorizing method and ethyl acetate partition method purification bear gall powder
Rear bear gall pink colour it is shallow it is fine and smooth, without tooth gluing sense, without bad smell, bitter taste is light, be not easy corruption, be not easy moisture absorption caking, property is stablized, have
Effect component content is averagely increased to 2 times or more.Extend period of storage, expands application range, improve curative effect of medication.
CN106038601A (201610368003.X, great Yi) discloses a kind of high-content, high-purity, low fishy smell bear gall powder
Preparation method, specific method is to be sufficiently mixed bear gall powder, activated carbon and filter aid, then carries mixture with ethanol solution
It is feminine gender to take into extracting solution cholanic acid, collects ethanol extract, concentrates and recycle ethyl alcohol, collects concentrate, dry and obtain；Institute
It is water and the insoluble silicate mineral of alcohol to state filter aid.It is believed that the method for the invention is simple, more operability, controllability
Good, content of the bear gall powder obtained in terms of Tauro ursodesoxy cholic acid reaches as high as 45% or more, the rate of recovery nearly 100%, with weight
The rate of recovery is calculated up to 85% or more, this method is suitable for industrialization large-scale production, at low cost, can be used in preparing special system
High-quality high-content, high-purity, low fishy smell bear gall powder needed for agent enterprise.
However, this field is still expected to have new method to prepare the bear gall powder with advantageous property.
Invention content
The purpose of the present invention is to provide a kind of new methods to prepare the bear gall powder with advantageous property.The present invention is another
It is designed to provide a kind of bear gall powder with advantageous property.In addition, the present invention also provides the bear gall powders of the invention prepared
Using.
For this purpose, first aspect present invention provides a kind of bear gall powder, it is the burnished gold or foresythia of hyaloid gloss
Powder, shows glassy yellow fluorescence at 365nm, and for example≤1%, and its solubility in water is more than 10g/ to hydroscopicity≤2%
100ml, the solubility in 90% ethyl alcohol are more than 1.2g/100ml, and the pH value of 5% aqueous solution is in 6.0~7.5 ranges.
Bear gall powder according to a first aspect of the present invention, the solubility in water are 13.6~14.2g/100ml.
Bear gall powder according to a first aspect of the present invention, the solubility in 90% ethyl alcohol are 1.25~2g/100ml.
Bear gall powder according to a first aspect of the present invention, the pH value of 5% aqueous solution is in 6.0~7.0 ranges.
Bear gall powder according to a first aspect of the present invention is prepared by a method comprising the following steps to obtain：
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, is diluted with water, obtains bear bile fluid；
(2) it is filled with 20~30min of nitrogen into bear bile fluid obtained by step (1), is then filled with 10~20min of carbon dioxide；
(3) bear bile fluid handled through aforesaid operations is inclined in material disc, be immediately placed in advance be refrigerated to -45 DEG C it is below
In freeze drier, freeze 2~5 hours；Then -25~-20 DEG C are warming up to 0.25~0.35 DEG C of speed per minute, kept
1~1.5 hour；Then it is warming up to -5~0 DEG C with 0.25~0.35 DEG C of speed per minute, is kept for 2~3 hours；Then with every
The speed of 0.25~0.35 DEG C of minute is warming up to 10~15 DEG C, is kept for 4~5 hours；Then with 0.25~0.35 DEG C per minute
Speed is warming up to 30~35 DEG C, is kept for 2~3 hours, terminates freeze-drying program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
In bear gall powder according to a first aspect of the present invention, wherein step (1) plus the water of 0.5~1 times of amount dilutes.
When inflatable body filled in a manner of bubbling in bear gall powder according to a first aspect of the present invention, wherein step (2)
Gas.
Bear gall powder according to a first aspect of the present invention, wherein step are filled with 25~30min of nitrogen in (2).
Bear gall powder according to a first aspect of the present invention, wherein step are filled with 15~20min of carbon dioxide in (2).
Bear bile fluid is inclined in material disc in bear gall powder according to a first aspect of the present invention, wherein step (3), and liquid layer depth is small
In 5cm.
Bear bile fluid is inclined in material disc in bear gall powder according to a first aspect of the present invention, wherein step (3), and liquid layer depth is small
In 2.5cm.
Bear bile fluid is inclined in material disc in bear gall powder according to a first aspect of the present invention, wherein step (3), and liquid layer depth is
1.5~2.5cm.
In bear gall powder according to a first aspect of the present invention, wherein step (3), make material disc be immediately placed on be refrigerated in advance-
In 55~-45 DEG C of freeze drier.
In bear gall powder according to a first aspect of the present invention, wherein step (3), make material disc be immediately placed on be refrigerated in advance-
In 50~-45 DEG C of freeze drier.
In bear gall powder according to a first aspect of the present invention, wherein step (3), make material disc be immediately placed on be refrigerated in advance-
In 50~-45 DEG C of freeze drier, freeze 3~4 hours；Then -25~-20 DEG C are warming up to 0.3 DEG C of speed per minute,
It is kept for 1~1.5 hour；Then it is warming up to -5~0 DEG C with 0.3 DEG C of speed per minute, is kept for 2~3 hours；Then with per minute
0.3 DEG C of speed is warming up to 10~15 DEG C, is kept for 4~5 hours；Then 30~35 are warming up to 0.3 DEG C of speed per minute
DEG C, it is kept for 2~3 hours, terminates freeze-drying program.
It has been unexpectedly discovered that bear bile fluid is made to be filled with nitrogen and carbon dioxide successively in advance, it is not only able to significantly increase
Add the solubility of gained bear gall powder, and active constituent Tauro ursodesoxy cholic acid (C26H45NO6S) display in gained bear gall powder
Go out more excellent stability, this is the prior art can not predict at all.
In addition, the present invention is diluted with a small amount of water in advance when preparing bear gall powder, cryogenic refrigeration is carried out after being filled with two kinds of gases,
So that contained active constituent in bear gall juice is in a kind of ice crystal state, then distil, thus gained freeze-drying bear gall powder exists
It can be referred to as ice crystal state bear gall powder in the present invention.
Further, second aspect of the present invention provides the method for preparing bear gall powder, includes the following steps：
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, is diluted with water, obtains bear bile fluid；
(2) it is filled with 20~30min of nitrogen into bear bile fluid obtained by step (1), is then filled with 10~20min of carbon dioxide；
(3) bear bile fluid handled through aforesaid operations is inclined in material disc, be immediately placed in advance be refrigerated to -45 DEG C it is below
In freeze drier, freeze 2~5 hours；Then -25~-20 DEG C are warming up to 0.25~0.35 DEG C of speed per minute, kept
1~1.5 hour；Then it is warming up to -5~0 DEG C with 0.25~0.35 DEG C of speed per minute, is kept for 2~3 hours；Then with every
The speed of 0.25~0.35 DEG C of minute is warming up to 10~15 DEG C, is kept for 4~5 hours；Then with 0.25~0.35 DEG C per minute
Speed is warming up to 30~35 DEG C, is kept for 2~3 hours, terminates freeze-drying program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
In method according to a second aspect of the present invention, wherein step (1) plus the water of 0.5~1 times of amount dilutes.
When inflatable body it is inflated in a manner of bubbling in method according to a second aspect of the present invention, wherein step (2).
Method according to a second aspect of the present invention, wherein step are filled with 25~30min of nitrogen in (2).
Method according to a second aspect of the present invention, wherein step are filled with 15~20min of carbon dioxide in (2).
Bear bile fluid is inclined in material disc in method according to a second aspect of the present invention, wherein step (3), and liquid layer depth is less than
5cm。
Bear bile fluid is inclined in material disc in method according to a second aspect of the present invention, wherein step (3), and liquid layer depth is less than
2.5cm。
Bear bile fluid is inclined in material disc in method according to a second aspect of the present invention, wherein step (3), and liquid layer depth is
1.5~2.5cm.
In method according to a second aspect of the present invention, wherein step (3), so that material disc is immediately placed on and be refrigerated to -55 in advance
In~-45 DEG C of freeze drier.
In method according to a second aspect of the present invention, wherein step (3), so that material disc is immediately placed on and be refrigerated to -50 in advance
In~-45 DEG C of freeze drier.
In method according to a second aspect of the present invention, wherein step (3), so that material disc is immediately placed on and be refrigerated to -50 in advance
In~-45 DEG C of freeze drier, freeze 3~4 hours；Then -25~-20 DEG C are warming up to 0.3 DEG C of speed per minute, protected
It holds 1~1.5 hour；Then it is warming up to -5~0 DEG C with 0.3 DEG C of speed per minute, is kept for 2~3 hours；Then with per minute
0.3 DEG C of speed is warming up to 10~15 DEG C, is kept for 4~5 hours；Then 30~35 are warming up to 0.3 DEG C of speed per minute
DEG C, it is kept for 2~3 hours, terminates freeze-drying program.
Method according to a second aspect of the present invention, obtained by bear gall powder be hyaloid gloss burnished gold or cadmium yellow
Color powder, shows glassy yellow fluorescence at 365nm, and for example≤1%, and its solubility in water is more than hydroscopicity≤2%
10g/100ml, the solubility in 90% ethyl alcohol are more than 1.2g/100ml, and the pH value of 5% aqueous solution is in 6.0~7.5 ranges
It is interior.
Method according to a second aspect of the present invention, obtained by bear gall powder solubility in water be 13.6~14.2g/
100ml.In another embodiment, the moisture of bear gall powder of the present invention is less than 3%.
Method according to a second aspect of the present invention, obtained by solubility of the bear gall powder in 90% ethyl alcohol be 1.25~
2g/100ml。
Method according to a second aspect of the present invention, obtained by bear gall powder its 5% aqueous solution pH value 6.0~7.0
In range.
In the above-mentioned preparation method of the invention the step of, although the specific steps of its description are in certain details or language
Step different from description and described in the preparation example of following detailed description part, however, people in the art
Member can summarize approach described above step completely according to the detailed disclosure of full text of the present invention.
Any embodiment of the either side of the present invention, can be combined with other embodiments, as long as they are not
It will appear contradiction.In addition, in any embodiment of either side of the present invention, any technical characteristic can be adapted for other realities
The technical characteristic in scheme is applied, as long as they are not in contradiction.The invention will be further described below.
All documents recited in the present invention, their full content are incorporated herein by reference, and if these are literary
When offering expressed meaning and the inconsistent present invention, it is subject to the statement of the present invention.In addition, the various terms that use of the present invention and
Phrase has that well known to a person skilled in the art general senses, nonetheless, the present invention remain desirable at this to these terms and
Phrase is described in more detail and explains, the term and phrase referred to is if any inconsistent with common art-recognized meanings, with institute's table of the present invention
Subject to the meaning stated.
Bear gall is ursidae animal black bear (Selenarctos thibetanus Cuvier) or brown bear (Ursus arctos
Linnaeus drying gall-bladder).Substitute of the dry product of drain-out bear gall as natural bear gall is used as medicine and examines listing,
It is named as bear gall powder, is a kind new medicine of health ministry approval.Bear gall powder is ursidae animal black bear (Selenarctos
Thibetanus Cuvier) by dry product obtained by operation on gallbladder bile drainage, cold in nature, bitter enters liver, courage, spleen, stomach, big
Intestines pass through, and have heat-clearing, soothing the liver, the work(of improving eyesight.Modern study finds that bear gall powder chemical composition is more complicated, mainly contains mating type
Ursodesoxycholic acid (UDCA), chenodeoxycholic acid (CDCA), cholic acid (CA), deoxycholic aicd (DCA), Tauro ursodesoxy cholic acid
(TUDCA), Taurochenodeoxycholic Acid (TCDCA) and cholesterol, bilins, amino acids, protein, peptide, aliphatic acid, micro-
Secondary element etc..Wherein ursodesoxycholic acid is important characteristic component.Clinically it is mainly used in gall stone, fatty liver, courage at present
The diseases in the liver and gallbladder such as capsulitis, virus hepatitis, chronic hepatitis B, eyelid herpes zoster, the diseases such as hemorrhoid.
Bear gall powder liver protection pharmacologically, cholagogic, litholytic effect.Have research by Female guinea pigs experiments have shown that bear gall
Powder can reduce cholesterol concentration, improve bile acid concentration, alleviate fatty degeneration of liver caused by high caloric diet high in fat, it was demonstrated that bear
Courage powder, which has, treats and prevents adipohepatic effect.In addition, TUDCA may influence the intestines liver cycle of bile acid, increase total courage
The content of UDCA in juice acid pond, reduces the content to the virose bile acid of liver cell, and prolonged application does not have apparent toxin for liver pair
Effect.There is research to induce N-nitrosodimethylamine (DMN) inhibiting effect of rat liver fibrosis by inquiring into bear gall powder.As a result it demonstrate,proves
Bright, bear gall powder has the function of that DMN is preferably inhibited to induce rat liver fibrosis.Its mechanism of action may be thin with inhibition Ku Pufu
Born of the same parents (Kupffer cell, KC), reduce the secretion of cell factor, inhibit hepatic stellate cells (hepatic satellite cell,
HSC activation) and conversion, synthesis and the secretion for reducing collagenous fibres are related.Have research by the external dissolve stone of bear gall powder, in vivo
The each group of data comparison of anti-stone experiment, it is found that bear gall powder has dissolve stone work to bile pigment calculus, cholesterol stone and mixed type calculus
With.Analysis of experimental results shows that bear gall powder can reduce bile cholesterol content, increases total bile acid content, can be obviously improved
Bile of forming calculus ingredient.Have research by rabbit experimental studies have found that, bear gall powder significantly reduce rabbit bait cholesterol courage
The incidence of calculus reduces the content of free cholesterol in bile, increases the content of total bile acid, it was demonstrated that bear gall powder has prevention
The effect that bait gall stone is formed.Chenodeoxycholic acid, ursodesoxycholic acid can make the reduction of bile cholesterol content, this mainly leads to
Cross inhibit cholesterol small intestine absorption, inhibit the activity of methyl glutaryl coenzyme A reductase to reducing cholesterol biosynthesis and
It realizes.
The antitumaous effect of bear gall powder pharmacologically.Have research by with bear gall to K562, SP20 tumour cell and mouse
S180 ascites carcinoma inhibiting tumor assays find that 1mg/ml concentration bear bile fluid is to human leukemia cell line K562 cells；20 μ g/ml are to mouse
Myeloma cell SP20 have an obvious inhibiting effect, cell disruption is dead.The results show that bear gall powder, which has, inhibits tumour cell life
Effect that is long, extending life cycle, improve immune function.There is research by being ground to transplanted tumor cell H22 models in Mice Body
Study carefully, finds each dosage group of bear gall powder to the tumour inhibiting rate of Murine Hepatoma22 36.00% or more；Each dosage group is to H22 hepatoma mice
Weight, thymus index, spleen index and liver index all have no significant effect.The results show that bear gall powder to rat liver cancer H22 have it is bright
Aobvious inhibiting effect.
The effect of the inhibition thrombosis of bear gall powder pharmacologically.There is research by being formed to rat suppository and to blood platelet
It is demonstrated experimentally that after injection refined bear gall powder, can inhibition thrombosis, hence it is evident that inhibit the exception of hemorheological property, while to blood
Platelet aggregation also has certain inhibiting effect.There is apparent inhibition to make for the activation of blood platelet when refined bear gall powder is to cerebral infarction
With.Studies have found that bear bile powder for injection can obviously inhibit the formation of rat inside and outside thrombus, blood viscosity is made to reduce, pressed down
Platelet aggregation processed improves thrombotic ischemic tissue of brain lesion degree, reduces malonaldehyde level in damage brain tissue, protects super oxygen
Compound dismutase activity has protection and therapeutic effect to cerebral ischemia.
The protective effect to cell hypoxia damage of bear gall powder pharmacologically.There is research to be caused using sodium dithionite
ECV304 cells obviously damage.The results show that anoxic can obviously induce damage, Tauro ursodesoxy cholic acid caused by ECV304 cells
The cellular damage is can obviously reduce with Taurochenodeoxycholic Acid, there is significant anti-ECV304 cell hypoxias damage.Bear gall
Powder makes damaging cells number substantially reduce, and LDH leakages rate, cell mortality are remarkably decreased, and cell survival rate significantly improves.Its brain
Protective effects are related to the protective effect of vascular endothelial cell anoxia-induced apoptosis with it.
Bear gall powder anti-inflammatory, antibacterial pharmacologically and antivirus action.There is research by making mouse, rat wound, finds
Bear gall pearl acne cream obviously accelerates mouse soft-tissue trauma healing, substantially reduced to mouse ear edge swelling, makes diagonal
Rat toes swelling caused by pitching dish is substantially reduced, it was demonstrated that bear gall pearl acne cream has preferable anti-inflammatory effect.There is research to send out
Existing, bear gall powder has apparent bacteriostasis to staphylococcus aureus and Escherichia coli.Studies have found that 6 kinds of diseases of bear gall powder pair
Poison has inhibiting effect, wherein effect is significantly inhibited to sick 4 types (CoxB4) of coxsackie B race and parainfluenza virus I types (HVJ),
Effect is significantly inhibited to mouse influenza pneumonia, causes dead mouse to have significant protective effect influenza.
The anti-allergic effects of bear gall powder pharmacologically.There is research to pass through IgE induced rats passive cutaneous anaphylaxis (PCA)
Experiment finds that refined bear gall powder can obviously inhibit P of Rats CA, can obviously inhibit release, the cell of mast cell degranulation histamine
Interior calcium intake and tumor necrosis factor-alpha, interleukin-6 and NF- κ B ρ 65, protein expression.Refined bear gall powder anti-I type is abnormal
One of important mechanisms of reaction are by inhibiting the expression of NF- kB proteins, to prevent the inflammatory cytokines such as TNF-α, IL-6
It generates.
The antifatigue effect of bear gall powder pharmacologically.Studies have found that when compound bear gall preparation may be swum by extending
Between and the pole-climbing time improve exercise tolerance, so that liver glycogen content is improved, blood urea nitrogen and Serum lactic acid content made to reduce, keep blood newborn
Acidohydrogenase vigor improves, and to provide more energy for body, has delayed the generation of fatigue, and then improve to exercise load
Adaptability；Compound bear gall preparation can be substantially reduced a shrinkage amplitude for rabbits' isolated duodenum smooth muscle, be to pass through
The contraction for inhibiting muscle excessive releases the spasm of smooth muscle to achieve the purpose that delay fatigue generates.
Bear gall powder antibechic pharmacologically, eliminating the phlegm, antipyretic, analgesic activity.There is research studies have shown that bear gall fritillary capsule energy
Enough substantially reduce concentrated ammonia liquor stimulation induced mice, cavy cough number；Promote mouse tracheae excretion phenol red and increases rat row
The effect of amount of expectoration；The experiment of rat fever caused by yeast powder also indicates that it with refrigeration function.The results show that bear gall fritillaria cough-relieving glue
Capsule has significant antibechic, eliminating the phlegm and faint refrigeration function.Studies have found that bear gall powder can significantly reduce 2,4- dinitros
Rat fever caused by phenol has certain refrigeration function, has apparent analgesic activity to pain caused by hot plate and acetic acid.
Bear gall powder has clinically been applied to disease in the liver and gallbladder.There is research to use bear gall Capsule in Treating Chronic Hepatitis B
(CHB) 33, same period inpatient 20 is used in combination to compare, observes two groups of patient's jaundice recession situations.As a result, plus with bear gall glue
Capsule treatment can promote jaundice prompt resolution, liver function to be improved, and have no adverse effects to blood picture and renal function.There is research to report
Road Ursofalk treats chronic hepatitis B, and obstinate type jaundice has obvious curative effects.There is research by 265 cholecystitis and cholelithiasis
Patient is randomly divided into black precious bear gall capsule for treating group and lidan paishi tablets control group.Wherein treatment group 214, control group 51,
Treatment group takes orally black precious bear gall capsule, and control group takes orally lidan paishi tablets.As a result, treatment group's healing 34, effective 82, effectively
79, invalid 19, total effective rate is up to 91.12%.Cholecystolithiasis effective percentage is treated up to 88.34% by treatment group, treats cholecystitis
Effective percentage is 96.35%.Clinical observation confirms that black treasured bear gall capsule for treating cholecystitis, gall stone are significant in efficacy.
Bear gall powder has clinically been applied to ophthalmology disease.There is research to 92 acute bacterial conjunctivitis patients using single
Blind random grouping, parallel control method, observe curative effect and adverse reaction.Compound bear guts gutta combines compound neomycin sulphate drop
Ocular fluid 46 is treatment group, and Compound Neomycin Sulfate Eye Drops 46 are control group.As a result, effective 38 for the treatment of group, improvement 6
Example, obvious effective rate 82.6%, total effective rate 95.7%；Effective 29 of control group improves 8, and obvious effective rate 63.0% always has
Efficiency is 80.4%.As a result, compound bear guts gutta joint Compound Neomycin Sulfate Eye Drops are used for acute bacterial conjunctivitis,
It is curative for effect.There is research to 36 patients, takes bear gall powder 1g, addition normal saline solution is appropriate, is applied to eyelid bleb office outside
Portion.After 1~2 day, local pain disappears general coating, red and swollen substantially reduced, and scar is not stayed in bleb drying incrustation after decrustation.Knot
Fruit proves that bear gall treated powder eyelid Herpes Zoster is definite.
Bear gall powder has clinically been applied to angiocardiopathy.Bear gall pills for curing heart disease is mainly used in coronary heart diseases and angina pectoris etc.
The treatment of angiocardiopathy.There is research that the patient of 558 angiocardiopathies is randomly divided into treatment group and control group, treatment group
419, take orally bear gall pills for curing heart disease treatment；Control group 139, with suxiao jiuxin pills oral medication.Pass through electrocardiogram clinical observation
Treatment group 419, effective 138, effective 194, total effective rate be 79.24% control group 139, effective 47, effective 56
Example, total effective rate 74.10%.The results show that bear gall pills for curing heart disease is significant in efficacy to angiocardiopathy.
Bear gall powder has clinically been applied to respiratory disease.There is research by 84 Bronchopneumonia patients (age 2
Month~10 years old) it is divided into treatment group and control group, treatment group 42, using tanreqin injection (radix scutellariae, bear gall powder, cornu caprae hircus, gold
Honeysuckle flower and Fructus Forsythiae) added with antibiotic combination therapy；Control group 42, antibiotics alone treatment.Two groups of courses for the treatment of are 7~10 days.Knot
Fruit, treatment group's total effective rate 95.2%, control group total effective rate 71.4%.The results show that tanreqin injection treats bronchus
Pneumonia is significant in efficacy.Have research by 76 Patients With Respiratory Tract Infections (6 months ages~3 years old 52,3~7 years old 13,7~14 years old
11) it is randomly divided into treatment group and control group, treatment group 38 is added using by 0.25~4mL/kg/d of tanreqin injection
Intravenous infusion in 5% Glucose Liquid 100mL；5% Glucose Liquid is added using by Shuanhuanglian injection 1mL/kg/d in control group 38
Intravenous infusion in 100mL, two groups are treated 7 days.As a result, treatment group's total effective rate 94.74%, control group total effective rate 65.79%.Knot
Fruit proves that tanreqin injection treatment infantile respiratory tract infection is safe and effective, is worth extensive use.
Bear gall powder has clinically been applied to hemorrhoid.There is curative effect of the research for observation compound bear gall hemorrhoid frost, by selected disease
Example is randomly divided into treatment group and control group, treatment group 97, internal piles 45, external piles 24, mixed hemorrhoid 28；Control group 68,
Internal piles 38, external piles 12, mixed hemorrhoid 18.Treatment group's externally used compound bear gall hemorrhoid frost, control group is with 1：5000KMnO4 takes advantage of
Hip bath after heat is first smoked.As a result, the total effective rate for the treatment of group's internal piles, external piles, mixed hemorrhoid is respectively 97.78%, 95.83%,
96.43%；Control group internal piles, external piles, mixed hemorrhoid total effective rate be respectively 84.21%, 66.67%, 61.11%, display is multiple
The curative effect of square bear gall hemorrhoid frost is notable.
Bear gall powder provided by the invention is presented excellent performance and excellent physicochemical property is for example presented.In this explanation of the invention
It is confirmed in book.
Specific implementation mode
The present invention can be further described by the following examples, however, the scope of the present invention and unlimited
In following embodiments.One of skill in the art, can be with it is understood that under the premise of without departing substantially from the spirit and scope of the present invention
Various change and modification are carried out to the present invention.The present invention carries out the material and test method that are arrived used in experiment general
And/or specific description.Although to realize the present invention many materials and operating method used in purpose be it is known in the art that
But the present invention is still described in detail as far as possible herein.
The assay method of hydroscopicity and moisture：Test sample 2g is taken, is laid in drying to the flat weighing bottle of constant weight, it is thick
Degree is no more than 5mm, accurately weighed；It is 5 hours dry at 100~105 DEG C to open bottle cap, bottle cap is covered, it is cold in dislocation drier
But 30 minutes, accurately weighed weight；It is dried 1 hour in above-mentioned temperature again, it is cooling, it weighs, until the difference weighed twice in succession is not
Until 5mg.According to the weight of less loss, the percentage containing moisture in test sample is calculated, the hydroscopicity and water of sample are calculated
Divide content.
Embodiment 1：Prepare bear gall powder
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, adds the water dilution of 0.75 times of amount, obtains bear bile fluid；
(2) in a manner of bubbling, it is filled with nitrogen 27min into bear bile fluid obtained by step (1), is then filled with carbon dioxide
18min；
(3) bear bile fluid handled through aforesaid operations is inclined into material disc (1.5~2.5cm of liquid layer depth), be immediately placed on
It is refrigerated in -50 DEG C of freeze drier, freezes 3.4 hours in advance；Then -22 DEG C are warming up to 0.3 DEG C of speed per minute,
It is kept for 1 hour；Then -3 DEG C are warming up to 0.3 DEG C of speed per minute, are kept for 2.5 hours；Then with 0.3 DEG C per minute
Speed is warming up to 12 DEG C, is kept for 4.5 hours；Then 32 DEG C are warming up to 0.3 DEG C of speed per minute, are kept for 2.5 hours, terminated
It is freeze-dried program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
Bear gall powder obtained by the present embodiment is the burnished gold or bright-yellow powder of hyaloid gloss, shows bright orange at 365nm
Color fluorescence,
Hydroscopicity≤2% (0.31%),
Solubility in water (13.92g/100ml) within the scope of 13.6~14.2g/100ml,
Solubility in 90% ethyl alcohol within the scope of 1.25~2g/100ml (1.83g/100ml),
The pH value of 5% aqueous solution (pH value 6.63) in 6.0~7.0 ranges,
Moisture is less than 3% (0.63%).
Embodiment 2：Prepare bear gall powder
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, adds the water dilution of 0.5 times of amount, obtains bear bile fluid；
(2) in a manner of bubbling, it is filled with nitrogen 30min into bear bile fluid obtained by step (1), is then filled with carbon dioxide
15min；
(3) bear bile fluid handled through aforesaid operations is inclined into material disc (1.5~2.5cm of liquid layer depth), be immediately placed on
It is refrigerated in -55 DEG C of freeze drier, freezes 3 hours in advance；Then -25 DEG C are warming up to 0.3 DEG C of speed per minute, protected
It holds 1.5 hours；Then -2 DEG C are warming up to 0.25 DEG C of speed per minute, are kept for 2 hours；Then with 0.25 DEG C per minute
Speed is warming up to 10 DEG C, is kept for 5 hours；Then 30 DEG C are warming up to 0.25 DEG C of speed per minute, are kept for 3 hours, terminated cold
Freeze drying program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
Bear gall powder obtained by the present embodiment is the burnished gold or bright-yellow powder of hyaloid gloss, shows bright orange at 365nm
Color fluorescence,
Hydroscopicity≤2% (0.53%),
Solubility in water (14.12g/100ml) within the scope of 13.6~14.2g/100ml,
Solubility in 90% ethyl alcohol within the scope of 1.25~2g/100ml (1.32g/100ml),
The pH value of 5% aqueous solution (pH value 6.23) in 6.0~7.0 ranges,
Moisture is less than 3% (0.51%).
Embodiment 3：Prepare bear gall powder
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, adds the water dilution of 1 times of amount, obtains bear bile fluid；
(2) in a manner of bubbling, it is filled with nitrogen 25min into bear bile fluid obtained by step (1), is then filled with carbon dioxide
20min；
(3) bear bile fluid handled through aforesaid operations is inclined into material disc (1.5~2.5cm of liquid layer depth), be immediately placed on
It is refrigerated in -45 DEG C of freeze drier, freezes 4 hours in advance；Then -20 DEG C are warming up to 0.35 DEG C of speed per minute,
It is kept for 1.25 hours；Then -3 DEG C are warming up to 0.35 DEG C of speed per minute, are kept for 3 hours；Then with 0.35 DEG C per minute
Speed be warming up to 15 DEG C, kept for 4 hours；Then 35 DEG C are warming up to 0.35 DEG C of speed per minute, are kept for 2 hours, terminated
It is freeze-dried program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
Bear gall powder obtained by the present embodiment is the burnished gold or bright-yellow powder of hyaloid gloss, shows bright orange at 365nm
Color fluorescence,
Hydroscopicity≤2% (0.45%),
Solubility in water (13.68g/100ml) within the scope of 13.6~14.2g/100ml,
Solubility in 90% ethyl alcohol within the scope of 1.25~2g/100ml (1.33g/100ml),
The pH value of 5% aqueous solution (pH value 6.44) in 6.0~7.0 ranges,
Moisture is less than 3% (0.57%).
Embodiment 4：Prepare bear gall powder
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, adds the water dilution of 0.6 times of amount, obtains bear bile fluid；
(2) in a manner of bubbling, it is filled with nitrogen 30min into bear bile fluid obtained by step (1), is then filled with carbon dioxide
10min；
(3) bear bile fluid handled through aforesaid operations is inclined into material disc (1.5~2.5cm of liquid layer depth), be immediately placed on
It is refrigerated in -52 DEG C of freeze drier, freezes 2 hours in advance；Then -23 DEG C are warming up to 0.25 DEG C of speed per minute,
It is kept for 1.5 hours；Then it is warming up to 0 DEG C with 0.3 DEG C of speed per minute, is kept for 2.2 hours；Then with 0.25 DEG C per minute
Speed be warming up to 13 DEG C, kept for 4.3 hours；Then 32 DEG C are warming up to 0.27 DEG C of speed per minute, are kept for 2.3 hours,
Terminate freeze-drying program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
Bear gall powder obtained by the present embodiment is the burnished gold or bright-yellow powder of hyaloid gloss, shows bright orange at 365nm
Color fluorescence,
Hydroscopicity≤2% (0.54%),
Solubility in water (13.66g/100ml) within the scope of 13.6~14.2g/100ml,
Solubility in 90% ethyl alcohol within the scope of 1.25~2g/100ml (1.94g/100ml),
The pH value of 5% aqueous solution (pH value 6.37) in 6.0~7.0 ranges,
Moisture is less than 3% (0.46%).
Embodiment 5：Prepare bear gall powder
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, adds the water dilution of 0.8 times of amount, obtains bear bile fluid；
(2) in a manner of bubbling, it is filled with nitrogen 20min into bear bile fluid obtained by step (1), is then filled with carbon dioxide
20min；
(3) bear bile fluid handled through aforesaid operations is inclined into material disc (1.5~2.5cm of liquid layer depth), be immediately placed on
It is refrigerated in -48 DEG C of freeze drier, freezes 5 hours in advance；Then -24 DEG C are warming up to 0.3 DEG C of speed per minute, protected
It holds 1 hour；Then -5 DEG C are warming up to 0.35 DEG C of speed per minute, are kept for 2.8 hours；Then with 0.35 DEG C of speed per minute
Degree is warming up to 12 DEG C, is kept for 4.8 hours；Then 34 DEG C are warming up to 0.34 DEG C of speed per minute, are kept for 2.7 hours, terminated
It is freeze-dried program；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
Bear gall powder obtained by the present embodiment is the burnished gold or bright-yellow powder of hyaloid gloss, shows bright orange at 365nm
Color fluorescence,
Hydroscopicity≤2% (0.48%),
Solubility in water (13.85g/100ml) within the scope of 13.6~14.2g/100ml,
Solubility in 90% ethyl alcohol within the scope of 1.25~2g/100ml (1.76g/100ml),
The pH value of 5% aqueous solution (pH value 6.57) in 6.0~7.0 ranges,
Moisture is less than 3% (0.82%).
The method for respectively referring to embodiment 1- embodiments 5, different be only be not diluted with water in step (1), but directly
Bear gall juice stoste is subjected to subsequent operation, thus obtained five batches of samples are presented dark yellow or brown color, have no hyaloid gloss,
Remaining parameter includes solubility in solubility, ethyl alcohol in hydroscopicity, water, 5 gained of pH value, moisture and embodiment 1- embodiments
Bear gall powder is essentially identical.This shows to dodge in freeze-drying plus a small amount of water contributes to improvement product appearance, obtains being in hyaloid gloss
Powder, may infer that bear gall powder of the present invention due to being added to water form ice crystal, bear gall powder of the present invention after advance deep freeze
Also referred to as ice crystal bear gall powder or ice crystal state bear gall powder.
Embodiment 11：Prepare bear gall powder
The method for respectively referring to embodiment 1- embodiments 5, different is only not inflated with nitrogen in step (2), obtains five batches of bears
Courage powder.
Bear gall powder obtained by the present embodiment is light yellowish brown powder, and glassy yellow fluorescence is shown at 365nm,
Hydroscopicity≤2% (0.83~1.32%),
Solubility in water within the scope of 8.6~9.4g/100ml,
Solubility in 90% ethyl alcohol within the scope of 0.82~0.94g/100ml,
The pH value of 5% aqueous solution in 6.2~6.8 ranges,
Moisture is less than 3% (0.82~1.04%).
Embodiment 12：Prepare bear gall powder
The method for respectively referring to embodiment 1- embodiments 5, different is only not filling CO 2 in step (2), obtains five
Criticize bear gall powder.
Bear gall powder obtained by the present embodiment is light yellowish brown powder, and glassy yellow fluorescence is shown at 365nm,
Hydroscopicity≤2% (0.81~1.34%),
Solubility in water within the scope of 8.9~9.7g/100ml,
Solubility in 90% ethyl alcohol within the scope of 0.85~0.91g/100ml,
The pH value of 5% aqueous solution in 6.2~6.6 ranges,
Moisture is less than 3% (0.88~1.01%).
Embodiment 13：Prepare bear gall powder
The method for respectively referring to embodiment 1- embodiments 5, different is only that inflated with nitrogen does not also fill titanium dioxide in step (2)
Carbon but directly carry out next step, obtain five batches of bear gall powders.
Bear gall powder obtained by the present embodiment is light yellowish brown powder, and glassy yellow fluorescence is shown at 365nm,
Hydroscopicity≤2% (0.93~1.23%),
Solubility in water within the scope of 9.4~9.9g/100ml,
Solubility in 90% ethyl alcohol within the scope of 0.92~0.98g/100ml,
The pH value of 5% aqueous solution in 6.24~6.7 ranges,
Moisture is less than 3% (0.82~1.07%).
In addition, obtained from commercially available approach five batches of bear gall powders (Chinese medicines quasi-word Z19991061, Z20000030,
Z20000026, Z20000055, Z20000031), their related physicochemical property parameter is measured, it is as a result as follows：Hydroscopicity≤
2% (in 0.57~1.73% range), solubility in water is within the scope of 8.3~10.1g/100ml, in 90% second
Solubility in alcohol is within the scope of 0.84~1.17g/100ml, and the pH value of 5% aqueous solution is in 6.0~7.0 ranges, moisture
Content is less than 3% (in 0.51~1.66% range).
Bear gall powder is prepared using the method recorded in CN102114044B its [0180] to [0183], measures their correlation
Physicochemical property parameter is as a result as follows：Hydroscopicity 1.42%, solubility 9.7g/100ml in water are molten in 90% ethyl alcohol
Solution degree 0.82g/100ml, the pH value 6.4 of 5% aqueous solution, moisture 1.47%；This batch of bear gall powder is known as in the present invention
044#。
Bear gall powder is prepared using the method recorded in CN105147729A its [0022] to [0024], measures their correlation
Physicochemical property parameter is as a result as follows：Hydroscopicity 1.17%, solubility 8.9g/100ml in water are molten in 90% ethyl alcohol
Solution degree 0.68g/100ml, the pH value 6.7 of 5% aqueous solution, moisture 1.26%；This batch of bear gall powder is known as in the present invention
729#。
The method recorded in specification " alcohol extraction procedure one " using CN1311002A prepares bear gall powder, measures them
Related physicochemical property parameter, it is as a result as follows：Hydroscopicity 1.86%, solubility 10.2g/100ml in water, in 90% ethyl alcohol
In solubility 0.91g/100ml, the pH value 6.6 of 5% aqueous solution, moisture 1.37%；This batch of bear gall powder is in the present invention
Referred to as 002#.
From result above as it can be seen that bear gall powder made from method of the embodiment of the present invention 1 to embodiment 5 shows notable higher
Solubility.
Test example 1：The quality testing of bear gall powder
1, character：Embodiment 1 to 5 each sample of embodiment is the burnished gold or bright-yellow powder of hyaloid gloss；Bitter,
Micro- raw meat.
11 embodiment of embodiment, 13 each sample and five batches of commercially available bear gall powders, 044#, 729#, 002# are light yellowish brown powder
End；Bitter, micro- raw meat.
2, differentiate (1)：It takes this product content appropriate (being equivalent to bear gall powder 0.06g), ethyl alcohol 5ml is added to make dissolving, filter, filter
Liquid is evaporated, and residue adds 10% sodium hydroxide solution 5ml, is set in water-bath heating hydrolysis 8 hours (or 120 DEG C hydrolyze 2 hours), is put
It is cold, salt acid for adjusting pH value is added dropwise to 2~3, with ethyl acetate shaking extraction 2 times, each 10ml, combined ethyl acetate liquid steams
Dry, residue adds ethyl alcohol 5ml to make dissolving, stands, takes supernatant as test solution.Separately ursodesoxycholic acid reference substance, goose is taken to go
Oxycholic acid reference substance and cholic acid reference substance add ethyl alcohol that the 1ml respectively mixed solutions containing 0.5mg are made, as a contrast product solution.According to thin
Layer chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015) is tested, and is drawn each 4ul of above two solution, is put respectively in same
On one silica gel g thin-layer plate, with isooctane-isoamyl ether-n-butanol-glacial acetic acid-water (10:5:3:5:1) upper solution (is faced with matching
System) it is solvent, it is unfolded, takes out, dry, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C, sets for spray
It is inspected under ultraviolet lamp (365nm).It is general to require, in test sample chromatography, on position corresponding with reference substance chromatography, show identical
The fluorescence spot of color.As a result：Embodiment 1 is commercially available to 5 each sample of embodiment, 11 embodiment of embodiment, 13 each sample and five batches
Bear gall powder, 044#, 729#, 002# show the fluorescence spot of same color on position corresponding with reference substance chromatography.
3, differentiate (2)：Test sample is taken, according to the method test under this test example (assay) item.It is general to require, test sample
In chromatography, chromatographic peak identical with reference substance main peak retention time should be presented.As a result：Embodiment 1 is to 5 each sample of embodiment, reality
It applies 11 embodiment of example, 13 each sample and five crowdes of commercially available bear gall powders, 044#, 729#, 002# is presented and retained with reference substance main peak
Time identical chromatographic peak.
4, Check pig galls are examined：Hyodesoxycholic acid reference substance is taken, adds ethyl alcohol 1ml the is made solution containing 0.5mg, product are molten as a contrast
Liquid.It is tested according to thin-layered chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015), draws the test solution differentiated under (1) item
With each 4ul of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with isooctane-isoamyl ether-n-butanol-ice vinegar
Acid-water (10:5:3:5:1) upper solution (facing with preparation) is solvent, is unfolded, takes out, dry, sprays with 10% sulfuric acid ethyl alcohol
Solution, it is clear to be heated to spot development at 105 DEG C, sets and is inspected under ultraviolet lamp (365nm).It is general to require, in test sample chromatography,
On position corresponding with reference substance chromatography, the fluorescence spot of same color should must not be shown.As a result：Embodiment 1 is each to embodiment 5
The not aobvious same color of sample, 11 embodiment of embodiment, 13 each sample and five crowdes of commercially available bear gall powders, 044#, 729#, 002#
Fluorescence spot.
5, assay
It is measured according to high performance liquid chromatography (four general rules 0512 of Chinese Pharmacopoeia version in 2015).
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With methanol-di(2-ethylhexyl)phosphate
Hydrogen sodium solution (0.03mol/L) (68：32) (being 4.4 with phosphorus acid for adjusting pH value) is mobile phase；Detection wavelength is 210nm；Column temperature
It is 40 DEG C.Number of theoretical plate is calculated by Tauro ursodesoxy cholic acid peak should be not less than 2500.
The preparation of reference substance solution：Take taurine sodium deoxycholate reference substance appropriate, it is accurately weighed, add methanol to be made often
Solution of the 1ml containing 1mg is to get (being equivalent to Tauro ursodesoxy cholic acid 0.9578mg).
The preparation of test solution：This product content under content uniformity item, finely ground, mixing is taken to take and (be equivalent to bear in right amount
Courage powder 0.12g), it is accurately weighed, it sets in 50ml measuring bottles, adds methanol appropriate, 10 points of supersound process (power 300W, frequency 50kHz)
Clock is let cool, and with methanol dilution to scale, is shaken up, filtration, take subsequent filtrate to get.
Measuring method：It is accurate respectively to draw reference substance solution and each 5~10ul of test solution, liquid chromatograph is injected, is surveyed
It is fixed to get.
General to require, the Tauro ursodesoxy cholic acid (C26H45NO6S) in bear gall powder must not be less than 30%.
As a result：Tauro ursodesoxy cholic acid (C26H45NO6S) content in embodiment 1 to 5 each sample of embodiment 34~
Tauro ursodesoxy cholic acid (C26H45NO6S) content in 38% range, such as in embodiment 1 is 37.6%；Embodiment 11 is implemented
Tauro ursodesoxy cholic acid in 13 each sample of example and five batches of commercially available bear gall powders, 044#, 729#, 002# each sample
(C26H45NO6S) for content in 23~33% ranges, some contents are more than 30%, somewhat smaller than 30%, such as embodiment 11
Tauro ursodesoxy cholic acid (C26H45NO6S) content in the bear gall powder with reference to obtained by 1 method of embodiment is 27.5%.
The above result shows that present invention gained bear gall powder has the typical activity substance Tauro ursodesoxy cholic acid of high level.
Test example 2：The stability of bear gall powder
It is protected from light and is sealed 6 months under the conditions of so that bear gall powder sample is placed in 40 DEG C of constant humidity, 0 is measured according to the method for test example 1
Tauro ursodesoxy cholic acid content when the moon and June in sample, criticizes sample to Mr. Yu, its sample after this high-temperature treatment is calculated according to following formula
Tauro ursodesoxy cholic acid remnants rates in product：
Remaining rate %=[0 month Tauro ursodesoxy cholic acid content of Tauro ursodesoxy cholic acid content ÷ in June] × 100%
As a result：Tauro ursodesoxy cholic acid remnants rates in embodiment 1 to 5 each sample of embodiment are in 97~100% ranges
It is interior, such as 1 sample Tauro ursodesoxy cholic acid remnants rates of embodiment are 99.6%；Ox in 11 embodiment of embodiment, 13 each sample
Sulphur ursodesoxycholic acid remnants rates are in 88~92% ranges, such as the bear gall powder sample with reference to obtained by 1 method of embodiment of embodiment 11
Product Tauro ursodesoxy cholic acid remnants rates are 90.2%；Ox sulphur bear in five batches of commercially available bear gall powders, 044#, 729#, 002# each sample
Deoxycholic aicd remnants rates are in 87~93% ranges, such as 729# bear gall powder sample Tauro ursodesoxy cholic acid remnants rates are
89.6%.These are the result shows that present invention gained bear gall powder has excellent chemical stability.
Above disclosed is only presently preferred embodiments of the present invention, cannot limit the right of the present invention with this certainly
Range, therefore according to equivalent variations made by scope of the present invention patent, be still within the scope of the present invention.
Claims (10)
1. a kind of bear gall powder is the burnished gold or bright-yellow powder of hyaloid gloss, glassy yellow fluorescence is shown at 365nm,
For example≤1%, and its solubility in water is more than 10g/100ml to hydroscopicity≤2%, and the solubility in 90% ethyl alcohol is big
In 1.2g/100ml, the pH value of 5% aqueous solution is in 6.0~7.5 ranges.
2. bear gall powder according to claim 1,：
Solubility in water is 13.6~14.2g/100ml；
Solubility in 90% ethyl alcohol is 1.25~2g/100ml；And/or
The pH value of 5% aqueous solution is in 6.0~7.0 ranges.
3. bear gall powder according to claim 1 is prepared by a method comprising the following steps to obtain：
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, is diluted with water, obtains bear bile fluid；
(2) it is filled with 20~30min of nitrogen into bear bile fluid obtained by step (1), is then filled with 10~20min of carbon dioxide；
(3) bear bile fluid handled through aforesaid operations is inclined in material disc, is immediately placed on and is refrigerated to -45 DEG C of freezings below in advance
In drying machine, freeze 2~5 hours；Then -25~-20 DEG C are warming up to 0.25~0.35 DEG C of speed per minute, keep 1~
1.5 hour；Then it is warming up to -5~0 DEG C with 0.25~0.35 DEG C of speed per minute, is kept for 2~3 hours；Then with per minute
0.25~0.35 DEG C of speed is warming up to 10~15 DEG C, is kept for 4~5 hours；Then with 0.25~0.35 DEG C of speed per minute
30~35 DEG C are warming up to, is kept for 2~3 hours, freeze-drying program is terminated；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
4. bear gall powder according to claim 3, wherein：In step (1) plus the water of 0.5~1 times of amount dilutes；Inflation in step (2)
It is to be inflated in a manner of bubbling when body；Step is filled with 25~30min of nitrogen in (2)；And/or it is filled with dioxy in step (2)
Change 15~20min of carbon.
5. bear gall powder according to claim 3, wherein：Bear bile fluid is inclined in material disc in step (3), and liquid layer depth is less than 5cm；
Liquid layer depth is less than 2.5cm；Liquid layer depth is 1.5~2.5cm；In step (3), make material disc be immediately placed on be refrigerated in advance-
In 55~-45 DEG C of freeze drier；And/or in step (3), so that material disc is immediately placed on and be refrigerated to -50~-45 DEG C in advance
Freeze drier in.
6. in bear gall powder according to claim 3, wherein step (3), making material disc be immediately placed on and being refrigerated to -50~-45 in advance
DEG C freeze drier in, freeze 3~4 hours；Then -25~-20 DEG C are warming up to 0.3 DEG C of speed per minute, keep 1~
1.5 hour；Then it is warming up to -5~0 DEG C with 0.3 DEG C of speed per minute, is kept for 2~3 hours；Then with 0.3 DEG C per minute
Speed is warming up to 10~15 DEG C, is kept for 4~5 hours；Then 30~35 DEG C are warming up to 0.3 DEG C of speed per minute, keep 2~
3 hours, terminate freeze-drying program.
7. the method for preparing bear gall powder, includes the following steps：
(1) the bear gall juice by the acquisition of no Tube Drain method filters, and obtains filtrate, is diluted with water, obtains bear bile fluid；
(2) it is filled with 20~30min of nitrogen into bear bile fluid obtained by step (1), is then filled with 10~20min of carbon dioxide；
(3) bear bile fluid handled through aforesaid operations is inclined in material disc, is immediately placed on and is refrigerated to -45 DEG C of freezings below in advance
In drying machine, freeze 2~5 hours；Then -25~-20 DEG C are warming up to 0.25~0.35 DEG C of speed per minute, keep 1~
1.5 hour；Then it is warming up to -5~0 DEG C with 0.25~0.35 DEG C of speed per minute, is kept for 2~3 hours；Then with per minute
0.25~0.35 DEG C of speed is warming up to 10~15 DEG C, is kept for 4~5 hours；Then with 0.25~0.35 DEG C of speed per minute
30~35 DEG C are warming up to, is kept for 2~3 hours, freeze-drying program is terminated；
(4) by the dried lump in material disc be ground into can by the fine powder that 50 mesh sieve to get.
8. method according to claim 7, wherein：In step (1) plus the water of 0.5~1 times of amount dilutes；Inflatable body in step (2)
When be to be inflated in a manner of bubbling；Step is filled with 25~30min of nitrogen in (2)；Be filled in step (2) carbon dioxide 15~
20min；Bear bile fluid is inclined in material disc in step (3), and liquid layer depth is less than 5cm, and liquid layer depth is less than 2.5cm, liquid layer depth
For 1.5~2.5cm.
9. method according to claim 7, wherein：
In step (3), so that material disc is immediately placed on and be refrigerated in -55~-45 DEG C of freeze drier in advance；
In step (3), so that material disc is immediately placed on and be refrigerated in -50~-45 DEG C of freeze drier in advance；
In step (3), so that material disc is immediately placed on and be refrigerated in -50~-45 DEG C of freeze drier in advance, freezing 3~4 is small
When；Then -25~-20 DEG C are warming up to 0.3 DEG C of speed per minute, are kept for 1~1.5 hour；Then with 0.3 DEG C per minute
Speed is warming up to -5~0 DEG C, is kept for 2~3 hours；Then 10~15 DEG C are warming up to 0.3 DEG C of speed per minute, keep 4~5
Hour；Then 30~35 DEG C are warming up to 0.3 DEG C of speed per minute, are kept for 2~3 hours, terminate freeze-drying program.
10. method according to claim 7, obtained by bear gall powder be hyaloid gloss burnished gold or cadmium yellow toner
End, shows glassy yellow fluorescence at 365nm, and for example≤1%, and its solubility in water is more than 10g/ to hydroscopicity≤2%
100ml, the solubility in 90% ethyl alcohol are more than 1.2g/100ml, and the pH value of 5% aqueous solution is in 6.0~7.5 ranges；Its
The solubility of obtained bear gall powder in water is 13.6~14.2g/100ml；Bear gall powder obtained by it is in 90% ethyl alcohol
Solubility be 1.25~2g/100ml；The pH value of bear gall powder its 5% aqueous solution obtained by and/or is in 6.0~7.0 models
In enclosing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108578433A (en) * | 2018-07-14 | 2018-09-28 | 齐光伟 | For preventing or treating gall stone cholecystitis and improve the bear gall powder of gallbladder function |
| CN108578434A (en) * | 2018-07-14 | 2018-09-28 | 齐光伟 | Prevent or treat method and the bear gall powder used of eye conjunctivitis and eyelid herpes zoster |
| CN108635375A (en) * | 2018-07-14 | 2018-10-12 | 齐光伟 | Prevent or treats hepatopathy and liver fibrosis and improve the bear gall powder and purposes of liver function |
| CN108653332A (en) * | 2018-07-14 | 2018-10-16 | 齐光伟 | Inhibition thrombosis and platelet aggregation and the bear gall powder and purposes for preventing cerebral ischemia |
| CN108743622A (en) * | 2018-07-14 | 2018-11-06 | 齐光伟 | Immunity of organisms and muscle power are improved using bear gall powder and alleviate the method for organism fatigue |
| CN108785328A (en) * | 2018-07-14 | 2018-11-13 | 齐光伟 | Prevent or treat method and the bear gall powder used of entity tumor and hematological system tumor |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108578433A (en) * | 2018-07-14 | 2018-09-28 | 齐光伟 | For preventing or treating gall stone cholecystitis and improve the bear gall powder of gallbladder function |
| CN108578434A (en) * | 2018-07-14 | 2018-09-28 | 齐光伟 | Prevent or treat method and the bear gall powder used of eye conjunctivitis and eyelid herpes zoster |
| CN108635375A (en) * | 2018-07-14 | 2018-10-12 | 齐光伟 | Prevent or treats hepatopathy and liver fibrosis and improve the bear gall powder and purposes of liver function |
| CN108653332A (en) * | 2018-07-14 | 2018-10-16 | 齐光伟 | Inhibition thrombosis and platelet aggregation and the bear gall powder and purposes for preventing cerebral ischemia |
| CN108743622A (en) * | 2018-07-14 | 2018-11-06 | 齐光伟 | Immunity of organisms and muscle power are improved using bear gall powder and alleviate the method for organism fatigue |
| CN108785328A (en) * | 2018-07-14 | 2018-11-13 | 齐光伟 | Prevent or treat method and the bear gall powder used of entity tumor and hematological system tumor |
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Effective date of registration: 20190319 Address after: 264200 Zhengqi Road Xishou, Weihai Port-Lingang Economic and Technological Development Zone, Shandong Province Applicant after: Weihai Senbao Industrial Co., Ltd. Applicant after: Qi Guangwei Address before: 116000 Red Star International 29 Floor, 17 Huida Street, Ganjingzi District, Dalian City, Liaoning Province Applicant before: Qi Guangwei |
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Application publication date: 20181106 |