CN110090274A - A kind of Chinese medicine composition and preparation method and application for treating the swollen humidifier fever of chicken kidney - Google Patents
A kind of Chinese medicine composition and preparation method and application for treating the swollen humidifier fever of chicken kidney Download PDFInfo
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Abstract
The present invention provides a kind of Chinese medicine compositions for treating the swollen humidifier fever of chicken kidney, belong to field of veterinary.Its technical solution are as follows: Chinese medicine composition is made of the raw material of following parts by weight: 0.1-10 parts of smilax, 0.1-10 parts of rhizoma imperatae, 0.1-10 parts of sophora flower, 0.1-10 parts of motherwort, 0.1-10 parts of Pogostemon cablin, 0.1-10 parts of rhizoma alismatis, 0.1-10 parts of Rhizoma Atractylodis Macrocephalae.The invention has the benefit that there is clearing heat and promoting diuresis, and the turbid effect of invigorating the spleenization, the swollen syndrome of dampness-heat of chicken kidney caused by primary treatment is damp and hot and dietary protein level is excessively high.
Description
Technical field
The present invention relates to a kind of field of veterinary more particularly to a kind of Chinese medicine compositions for treating the swollen humidifier fever of chicken kidney.
Background technique
Chicken kidney disease is caused by a variety of diseases or virulence factor, including ephritis, kidney stone, gout, ureteral calculi,
Uremia etc., common trait are that kidney swelling, renal tubule and ureter uratic deposit occur, and it is dead to can lead to chicken group when serious
It dies.Recently as gradually increasing for pathogenic infection pressure various in environment, with kidney swell the disease for important clinical manifestation by
It is cumulative more, serious financial consequences are caused to poultry husbandry, have seriously affected the development of poultry husbandry.
Damp and hot is an important factor for leading to nephrosis state of an illness continuing advances and recurrent exerbation.Vibration sound is taught when China Academy of TCM
It awards and thinks, damp and hot stasis is the main pathogenesis of nephrosis, and nephrosis syndrome of dampness-heat is the most common card type.The chicken of different days can occur
Kidney trouble, diseased chicken performance is apathetic, feather is fluffy and disorderly, it is drowsiness to bow, draws white loose stool or in water sample shape, perianal by excrement
Just it pollutes.Chicken body is thin, and Chicks ' Growth is slow, and laying hen group's egg drop reduction, lopsided egg increases.Nephrotic bronchitis causes
It is more, the course of disease is longer, the death rate etc., hair patient finally terminated with death.Nephrosis caused by gumboro disease, the course of disease
Short, disease incidence is high, and the death rate is up to 30-50%.Different degrees of economic loss is caused to poultry husbandry.The swollen syndrome of dampness-heat of chicken kidney is existing
For one of the principal disease of chicken death in poultry husbandry.Once the swollen disease of kidney occurs, the death rate will step up, especially work as chicken group
Other diseases along with kidney swell disease occur when, the death rate will will increase l times or more.
Currently, according to clinical symptom and dissect lesion degree, clinical multiselect anti-microbial type medicine (such as fluorine parasiticin, amoxycillin
Penicillin, the Norfloxacin of quinolones, Ciprofloxacin, Ofloxacin etc.)；Vitamin C pulvis or aqueous solvent, cleum jecoris piscis concentratum water
Agent or cleum jecoris piscis concentratum pulvis, or with commodity nutritional additive speed mend -14 and diuretics such as kidney swell antidote, SHENZHONG JIEDULING etc..
But some drugs such as sulfamido, aminoglycoside, cephalosporins etc. by kidney excretion, there is potentially kidney in vivo
Toxic effect, if for a long time, large dosage of use be easy to cause kidney injury.Aggravate one's illness development instead.And most " swollen solutions of kidney
Poison " medicine not only has diuresis while having the side effect of dehydration.After the similar drug use, chicken group's excrement is thin, padding is moist, when
Between slightly long chicken group just start de- water and rock-soil coupling and dead, if not being discontinued, death cannot terminate, and situation can be more next
It is more serious.
Summary of the invention
The purpose of the present invention is to provide one kind to have clearing heat and promoting diuresis, and the turbid effect of invigorating the spleenization, primary treatment is damp and hot and raises
Expect the Chinese medicine composition of the swollen humidifier fever for the treatment of chicken kidney of the swollen syndrome of dampness-heat of chicken kidney caused by protein content is excessively high.
The present invention is realized by following measure:
A kind of Chinese medicine composition for treating the swollen humidifier fever of chicken kidney, which is characterized in that the Chinese medicine composition is by following weight
The raw material composition of part: 0.1-10 parts of smilax, 0.1-10 parts of rhizoma imperatae, 0.1-10 parts of sophora flower, 0.1-10 parts of motherwort, Pogostemon cablin
0.1-10 parts, 0.1-10 parts of rhizoma alismatis, 0.1-10 parts of Rhizoma Atractylodis Macrocephalae (every part of weight is 100g).
Specific feature of the invention is also:
The Chinese medicine composition is made of the raw material of following parts by weight: 3.66 parts of smilax, 3.66 parts of rhizoma imperatae, sophora flower
0.93 part, 0.93 part of motherwort, 0.28 part of Pogostemon cablin, 0.28 part of rhizoma alismatis, 0.26 part of Rhizoma Atractylodis Macrocephalae.
The Chinese medicine composition is made of the raw material of following parts by weight: 3.74 parts of smilax, 3.74 parts of rhizoma imperatae, and sophora flower
0.83 part, 0.83 part of motherwort, 0.30 part of Pogostemon cablin, 0.29 part of rhizoma alismatis, 0.27 part of Rhizoma Atractylodis Macrocephalae.
The Chinese medicine composition is made of the raw material of following parts by weight: 3.81 parts of smilax, 3.81 parts of rhizoma imperatae, and sophora flower
0.74 part, 0.74 part of motherwort, 0.32 part of Pogostemon cablin, 0.3 part of rhizoma alismatis, 0.28 part of Rhizoma Atractylodis Macrocephalae.
The Chinese medicine composition is manufactured as follows:
1. take smilax that 20%~90% alcohol reflux is added to extract twice, 15~120 minutes every time, what merging obtained twice
Extracting solution, and be filtered, finally recycle ethyl alcohol；
2. taking sophora flower, motherwort, rhizoma imperatae, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae extracting in water three times, 15~120 minutes every time, merge three times
Obtained extracting solution, is filtered；
3. by step 1. with step 2. in finally obtained extracting solution be combined and concentrated to relative density about 1.06 (60
DEG C), the extracting solution after concentration is subjected to spray drying, obtains spray powder；
4. taking Pogostemon cablin, Pogostemon cablin is crushed to 80~200 mesh, obtains Pogostemon cablin fine powder, 3. spray drying that step is obtained
Powder and Pogostemon cablin fine powder are mixed and added into conventional pharmaceutical adjuvants, are prepared into required dosage form.
The Chinese medicine composition is made into any one of tablet, pill, capsule, granule.
The effervescent the preparation method comprises the following steps:
1. taking smilax that 60% alcohol reflux is added to extract twice, 60 minutes every time, merges the extracting solution obtained twice, go forward side by side
Row filtering, finally recycles ethyl alcohol.
2. taking sophora flower, motherwort, rhizoma imperatae, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae extracting in water twice, 90 minutes every time, merge gained twice
The extracting solution arrived, is filtered.
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, use be concentrated under reduced pressure mode
Total extract is concentrated into relative density about 1.06 (60 DEG C), then by the total extract after concentration by the way of spray drying
Spray drying is carried out, spray powder is obtained.
4. taking Pogostemon cablin, Pogostemon cablin is crushed to 100 mesh, obtains Pogostemon cablin fine powder, then appropriate NaHCO3It is added appropriate
In the PEG6000 of melting, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, citric acid, dextrin,
Sucrose adds alcohol granulation up to effervescent.
5. to step, 4. the middle effervescent prepared is detected.
The step 5. in detection method are as follows:
S1, preparation reference substance solution: taking appropriate astilbin reference substance, control substance of Rutin, accurately weighed, adds 60% methanol
Mixed solution of every 1mL containing 50 μ g of astilbin, 100 μ g of rutin is made, obtains reference substance solution；
S2, prepare medical fluid to be detected: take the appropriate step 4. in the effervescent for preparing and be ground into fine powder 1.0g,
It is accurately weighed, it pours into stuffed conical flask, 60% methanol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated 30 minutes,
It lets cool, then weighed weight, the weight of less loss is supplied with 60% methanol, is shaken up, filter, take subsequent filtrate, obtain medical fluid to be detected；
Each 10 μ l of medical fluid to be detected of S3, the respectively accurate reference substance solution for measuring step S1 preparation and step S2 preparation,
Inject liquid chromatograph, using high performance liquid chromatography in reference substance solution and medical fluid to be detected astilbin and rutin into
Row assay, compares
The step 4. in, the NaHCO3It is 1:0.8, the NaHCO with the PEG6000 mass ratio3The citron
Sour mass ratio is 1:1.25, and the dextrin and the sucrose solution mass ratio are 1:1.
The Chinese medicine composition is in preparation for treating the application in the drug that chicken kidney swells humidifier fever.
The invention has the benefit that clearing heat and promoting diuresis, the turbid effect of invigorating the spleenization, primary treatment is damp and hot and feed protein contains
The excessively high swollen syndrome of dampness-heat of caused chicken kidney is measured, by Chinese veterinarian's theory, the swollen disease of kidney belongs to humidifier fever, and damp and hot knot makes urinary tract not in lower coke
Benefit, the puckery pain of frequent micturition are very then closed and obstructed, the rules for the treatment of with clearing away heat and promoting diuresis it is treating stranguria based on.The traditional chinese medicine composition of the invention is with monarchs such as smilaxs
Medicine, is equipped with rhizoma imperatae, sophora flower, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae with cooling blood and hemostasis at the effect of taking the saturating network of its promoting menstruation, removing toxic substances dehumidifying, reducing fever and causing diuresis,
Motherwort is with activating microcirculation and removing stasis medicinal, and Pogostemon cablin is eliminated dampness with aromatics and middle preventing or arresting vomiting, delivers relieving summer-heat, activating spleen and strengthening stomach.
Detailed description of the invention
Fig. 1 is that (upper figure is astilbin for astilbin and the hybrid standard product of rutin in description of the invention experiment two
291nm detection, the following figure are rutin 257nm detection) map.
Fig. 2 is the map of smilax negative sample in description of the invention.
Fig. 3 is the map of sophora flower negative sample in description of the invention experiment two.
Fig. 4 is the canonical plotting of astilbin in description of the invention experiment two.
Fig. 5 is the standard curve of rutin in description of the invention experiment two.
Specific embodiment
In order to clarify the technical characteristics of the invention, being illustrated below by specific embodiment to this programme.
Embodiment 1:
Raw material composition: smilax 366g, rhizoma imperatae 366g, sophora flower 93g, motherwort 93g, Pogostemon cablin 28g, rhizoma alismatis 28g, white
Art 26g.
Preparation method:
1. taking smilax 366g that 8 times of 60% alcohol refluxs of amount is added to extract twice, 60 minutes every time, what merging obtained twice was mentioned
Liquid is taken, and is filtered, ethyl alcohol is finally recycled；
2. taking sophora flower 93g, motherwort 93g, rhizoma imperatae 366g, rhizoma alismatis 28g, Rhizoma Atractylodis Macrocephalae 26g that 8 times of amount water is added to extract twice, often
Secondary 60 minutes, merges obtained extracting solution twice, be filtered；
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, use be concentrated under reduced pressure mode
Total extract is concentrated into relative density about 1.06 (60 DEG C), then by the total extract after concentration by the way of spray drying
Spray drying is carried out, spray powder is obtained；
4. taking Pogostemon cablin 28g, Pogostemon cablin is crushed to 100 mesh, obtains Pogostemon cablin fine powder, then by 100gNaHCO3Add
Enter 80g melting PEG6000 in, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, 125g citron
Acid, dextrin, sucrose, supply 1000g, add alcohol granulation up to effervescent；
5. to step, 4. the middle effervescent prepared is detected.
Step 5. in detection method:
S1, preparation reference substance solution: taking appropriate astilbin reference substance, control substance of Rutin, accurately weighed, adds 60% methanol
Mixed solution of every 1mL containing 50 μ g of astilbin, 100 μ g of rutin is made, obtains reference substance solution；
S2, prepare medical fluid to be detected: take the appropriate step 4. in the effervescent for preparing and be ground into fine powder 1.0g,
It is accurately weighed, it pours into stuffed conical flask, 60% methanol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated 30 minutes,
It lets cool, then weighed weight, the weight of less loss is supplied with 60% methanol, is shaken up, filter, take subsequent filtrate, obtain medical fluid to be detected；
S3, the medical fluid to be detected each 10 that successively prepared by the accurate reference substance solution for measuring step S1 preparation and step S2 respectively
μ l, inject liquid chromatograph, using high performance liquid chromatography in reference substance solution and medical fluid to be detected astilbin and reed
Fourth carries out assay, compares.
As a result: the content of astilbin is 1.56mg in every gram of Chinese medicine of the present invention, and the content of rutin is 5.28mg.
The Chinese medicine of the swollen syndrome of dampness-heat for the treatment of chicken kidney of this test preparation is during storage 24 months, in appearance character, identification, inspection
Look into, content items Index for examination has no significant change, and meets every regulation of preclinical drug standard, quality is substantially steady
It is fixed.
Embodiment 2:
Raw material composition: smilax 374g, rhizoma imperatae 374g, sophora flower 83g, motherwort 83g, Pogostemon cablin 30g, rhizoma alismatis 29g, white
Art 27g.
Preparation preparation method: 1. taking smilax 374g that 8 times of 60% alcohol refluxs of amount is added to extract twice, 60 minutes every time, merges two
Secondary obtained extracting solution, and be filtered, finally recycle ethyl alcohol；
2. taking sophora flower 83g, motherwort 83g, rhizoma imperatae 374g, rhizoma alismatis 29g, Rhizoma Atractylodis Macrocephalae 27g that 8 times of amount water is added to extract twice, often
Secondary 60 minutes, merges obtained extracting solution twice, be filtered；
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, use be concentrated under reduced pressure mode
Total extract is concentrated into relative density about 1.06 (60 DEG C), then by the total extract after concentration by the way of spray drying
Spray drying is carried out, spray powder is obtained；
4. taking Pogostemon cablin 30g, Pogostemon cablin powder is crushed to 100 mesh, obtains Pogostemon cablin fine powder, then by 100gNaHCO3
Be added 80g melting PEG6000 in, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, 125g Chinese holly
Rafter acid, dextrin, sucrose, supply 1000g, add alcohol granulation up to effervescent；
5. to step, 4. the middle effervescent prepared is detected.
Step 5. in detection method:
S1, preparation reference substance solution: taking appropriate astilbin reference substance, control substance of Rutin, accurately weighed, adds 60% methanol
Mixed solution of every 1mL containing 50 μ g of astilbin, 100 μ g of rutin is made, obtains reference substance solution；
S2, prepare medical fluid to be detected: take the appropriate step 4. in the effervescent for preparing and be ground into fine powder 1.0g,
It is accurately weighed, it pours into stuffed conical flask, 60% methanol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated 30 minutes,
It lets cool, then weighed weight, the weight of less loss is supplied with 60% methanol, is shaken up, filter, take subsequent filtrate, obtain medical fluid to be detected；
S3, the medical fluid to be detected each 10 that successively prepared by the accurate reference substance solution for measuring step S1 preparation and step S2 respectively
μ l, inject liquid chromatograph, using high performance liquid chromatography in reference substance solution and medical fluid to be detected astilbin and reed
Fourth carries out assay, compares.
As a result: the content of astilbin is 1.63mg in every gram of Chinese medicine of the present invention, and the content of rutin is 5.48mg.
Embodiment 3:
Raw material composition: smilax 381g, rhizoma imperatae 381g, sophora flower 74g, motherwort 74g, Pogostemon cablin 32g, rhizoma alismatis 30g, white
Art 28g.
Prepare preparation method:
1. taking smilax 381g that 8 times of 60% alcohol refluxs of amount is added to extract twice, 60 minutes every time, what merging obtained twice was mentioned
Liquid is taken, and is filtered, ethyl alcohol is finally recycled；
2. taking sophora flower 74g, motherwort 74g, rhizoma imperatae 381g, rhizoma alismatis 30g, Rhizoma Atractylodis Macrocephalae 28g that 8 times of amount water is added to extract twice, often
Secondary 60 minutes, merges obtained extracting solution twice, be filtered；
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, use be concentrated under reduced pressure mode
Total extract is concentrated into relative density about 1.06 (60 DEG C), then by the total extract after concentration by the way of spray drying
Spray drying is carried out, spray powder is obtained；
4. taking Pogostemon cablin, Pogostemon cablin powder 32g is crushed to 100 mesh, Pogostemon cablin fine powder is obtained, then by 100gNaHCO3
Be added 80g melting PEG6000 in, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, 125g Chinese holly
Rafter acid, dextrin, sucrose, supply 1000g, add alcohol granulation up to effervescent；
5. to step, 4. the middle effervescent prepared is detected.
Step 5. in detection method:
S1, preparation reference substance solution: taking appropriate astilbin reference substance, control substance of Rutin, accurately weighed, adds 60% methanol
Mixed solution of every 1mL containing 50 μ g of astilbin, 100 μ g of rutin is made, obtains reference substance solution；
S2, prepare medical fluid to be detected: take the appropriate step 4. in the effervescent for preparing and be ground into fine powder 1.0g,
It is accurately weighed, it pours into stuffed conical flask, 60% methanol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated 30 minutes,
It lets cool, then weighed weight, the weight of less loss is supplied with 60% methanol, is shaken up, filter, take subsequent filtrate, obtain medical fluid to be detected；
S3, the medical fluid to be detected each 10 that successively prepared by the accurate reference substance solution for measuring step S1 preparation and step S2 respectively
μ l, inject liquid chromatograph, using high performance liquid chromatography in reference substance solution and medical fluid to be detected astilbin and reed
Fourth carries out assay, compares.
As a result: the content of astilbin is 1.72mg in every gram of Chinese medicine of the present invention, and the content of rutin is 5.47mg.
The inventor of drug of the present invention has carried out a series of realities in terms of the selection of bulk pharmaceutical chemicals, preparation method and applications
Test research, it is determined that the bulk pharmaceutical chemicals and preparation method of preparation drug of the present invention, making it compared with prior art has apparent dash forward
Curative effect advantage out.
Test one, drug effect clinical test
Step 1: the foundation of injury of kidney modeling method
1, material
Experimental animal: 1 age in days Sanhuang broiler.
Forage standard: the powder that basal diet is prepared referring to NPC, China Broiler forage standard in 1998.
2, test method
It takes normal raising to 11 age in days healthy chick 100,5 groups is randomly divided into after weighing, is fed to raise by every kilogram respectively
Expect that spice adds 0.0,1.0,2.0,3.0 and 4.0 gram of Compound New Nomin of meat-chicken complete feedstuff, observes chick after administration daily
Spirit, appetite, drinking-water, defecation, movement etc., when successive administration was to 7 days, 4 groups of chickens of all administrations show as spirit it is depressed,
Feed intake decline, draws water sample loose stools, has part chicken lime sample occur just.So far, stop test, weigh respectively, count each group
Average weight increasing a day, average daily feed intake, feed-weight ratio, and the histopathologic change and title of the dissect observation heart, liver,spleen,kidney, the organs such as lung
Amount statistics organ index (organ wet weight/living body weight × 100).
3, test result
3.1, clinical symptoms
After successive administration 7 days, 4 groups for adding 1 ‰~4 ‰ Compound New Nomin by spice all occur in various degree
Spirit is depressed, feed intake declines and water sample is had loose bowels, wherein the chicken symptom of 3 ‰, 4 ‰ dosage groups of addition is the most obvious, most of chicken
Only there is thin, the white lime sample loose stool of drawing.
3.2, growth performance and organ index
Table 1 gives the growth performance and organ index of Compound New Nomin 7d each group chickenN=20
Note: colleague data Superscript letters neighbor significant difference (P < 0.05).
The Average weight increasing a day for adding 3 ‰, 4 ‰ SMZ group chickens in feed it can be seen from 1 data of table is substantially less than negative right
According to group, and feed-weight ratio is then significantly higher than negative control group；The medication group Kidney coefficients of all addition SMZ are all larger than negative control
Group, but add 3 ‰, 4 ‰ SMZ groups and be then noticeably greater than 1 ‰, 2 ‰ SMZ groups of negative control group and addition.Show to add in feed
3 ‰, 4 ‰ SMZ, which are used in conjunction, just to be caused the swollen property damage of kidney for 7 days and influences the growth indexes such as weight gain.
3.3, dissect lesion
Compared with negative control group chicken, 1 ‰, 2 ‰ SMZ group chicken kidney slightly swelling are added, are in pale asphyxia；Add 3 ‰,
4 ‰ SMZ group chicken kidney obvious tumefactions, it is pale, it is partially in piebald kidney sample.
3.4, renal tissue sections observation
Negative control group glomerulus structure is normal, and glomerulus blister cavities is obvious, and capsula glomeruli parietal layer and renal tubular cell structure are clear
Chu, cell boundary is more visible, adds 3 ‰, the 4 ‰ most of glomerulus swelling of SMZ group chicken kidney, and glomerulus blister cavities expands, portion
Divide Malpighian corpuscle, renal tubule swelling rupture, diminution, atrophy shape, visible lymphocytic infiltration in some Malpighian corpuscles is presented.And it adds
1 ‰, 2 ‰ SMZ group chicken renal lesions are not then fairly obvious.
Step 2: the experiment clinical test for the treatment of chicken injury of kidney
1, material
1.1, reagent: the traditional chinese medicine composition of the invention effervescent.
1.2, control drug: grey indigo plant oral solution.
1.3, experimental animal: 1 age in days Sanhuang broiler.
1.4, forage standard: the powder that basal diet is prepared referring to NPC-1998 China Broiler forage standard.
2, test method
2.1, chicken injury of kidney modeling
1 age in days Sanhuang broiler 600 is purchased, normal raising separated 90 at random and be only used as (every group 30 of negative control group to 18 days
Only, 3 repetitions) individually raising with no treatment；Remaining is 510 multiple only with the addition of every kilogram of feed spice is pressed in basal diet
Square radonil (SMZ) 3.0g (this additive capacity is establishing experimental result and determine referring to injury of kidney modeling method), it is continuous to raise
The injury of kidney modeling method fed carries out artificial modeling.As a result when the feed of 3 ‰ SMZ of continuous feeding addition was to 7 days, entire chicken group goes out
Existing spirit is depressed, drinks loss of appetite, and feed intake is decreased obviously, and draws white lime water sample loose stool.When ending the 7th day 24:00, entirely
Chicken group dead 13, take dead chicken and extremely depressed 17 dissects of chicken of spirit it has been observed that kidney obvious tumefaction, majority is in pale
Color piebald shape；Collecting part obvious tumefaction kidney makees frozen section observation display, most of glomerulus swelling, and glomerulus blister cavities expands
Greatly, part renal tubular cell is disorganized, small tracheal rupture.Accordingly, experimental result is established in conjunction with injury of kidney modeling method, it is believed that
The injury of kidney modeling success of 510 chickens of this batch.After the dead and spiritual extremely depressed chicken of rejecting, 450 are selected manually
Moldability injury of kidney illness chicken is tested for successive treatment.
2.2, therapeutic test
Successful 450 chickens of above-mentioned mould are randomly divided into 5 processing groups (including II, III, IV, V, VI group) by weight, often
30 (setting 3 repetitions) of group.II group is positive drug control group, the grey mixed drink 2.0ml/L of indigo plant oral solution；III, IV, V it is followed successively by reality
Apply the basic, normal, high dosage of effervescent (dosage successively are as follows: 0.5g/L, 1.0g/L, 2.0g/L) group of one raw material proportioning of example
(1.0g/L is to be mixed with drug 1.0g in every liter of water), the mixed drink administration of whole day；VI group is positive controls, and drug therapy is not handled.
Second day (i.e. 26 ages in days) after modeling success start to be administered, and continuous use 5 days.In addition, I group be negative control group, 90
Chicken without any processing.Experimental period, which is observed from 26 ages in days to 35 ages in days, to be stopped, and totally 10 days.
2.3 test indexs and efficacy determination
Entire experimental period, is observed and recorded mental status, feed intake and excrement situation to each group chicken integral status day by day.
The experimental observation phase terminates, and weighs respectively, counts Average weight increasing a day, the average daily feed intake, feed-weight ratio of each group, and the dissect observation heart, liver,
The histopathologic change and weighing statistics renal index (kidney weight in wet base/living body weight × 100) of the organs such as spleen, lung, especially kidney.And
By following standard determination curative effect:
Cure: chicken spirit, appetite, excrement restore normal；Dissect is observed the internal organs such as the heart, liver, spleen, lung, kidney and is seen without naked eyes
Examine lesion, and renal index≤1.10.
Effective: chicken spirit, appetite, excrement return to normal；Dissect observes the internal organs such as the heart, liver, spleen, lung, kidney without bright
It is aobvious to visually observe lesion, and 1.10 renal index≤1.20 <.
Effective: chicken spirit, appetite return to normal, but still excrement of having loose bowels；Dissect observe the heart, liver, spleen, lung, without bright
It is aobvious to visually observe lesion, but kidney still has mild swelling, and 1.20 renal index≤1.30 <.
Invalid: chicken spirit is depressed, loss of appetite, draws white lime sample or serious water sample loose stool；It is bright that dissect observes kidney
Aobvious swelling, or be in piebald kidney sample, and renal index > 1.30.
3. clinical trial results
3.1, each group clinicing symptom observation result
When 26 age in days, II~VI group of experimental chicken performance feed intake is reduced, spirit is depressed, draws water sample or lime sample loose stool.Through
It crosses after therapeutic test on the 5th (when 30 age in days), " effervescent " middle and high dosage group and the spiritual shape of positive drug control group chicken group
State, which has, to be obviously improved, and water sample loose stool significantly reduces, and white lime sample loose stool disappears；The low dose group chicken group state of mind is also
Improve, water sample loose stool phenomenon is still serious, and a small number of chickens still draw white lime sample loose stool.When to 35 age in days, middle high dose group
Restore completely with the positive drug control group state of mind, excrement is also normal；The low dose group state of mind is restored substantially, but still
So there is part chicken to draw water sample loose stool.VI group i.e. positive controls chicken group to the observation period terminates still to have about 50% chicken spirit heavy
Strongly fragrant, loss of appetite, about 70% draws white lime sample or water sample loose stool.I group i.e. negative control group chicken group the observation period spirit, appetite and
Excrement is completely normal.Out of 26 ages in days to 35 ages in days the entire observation period, I~VI group of experimental chicken group is dead without occurring.
3.2, growth performance and renal index observe result
The growth performance and renal index of 2 each group chicken of tableN=30
Note: colleague data Superscript letters neighbor significant difference (P < 0.05).
3.3, treatment observation result
Terminate to the experimental observation phase, every chicken of each group determines whether to have loose bowels by observation perianal feather；And it slaughters and cuts open
Inspection observation visceral organ tissue's lesion.As the result is shown: I group of all chicken perianal feather is clean, without phenomenon of having loose bowels；In dissect
Dirty equal nothing visually observes lesion.II, IV, the V group i.e. middle and high dosage group of positive drug control group and effervescent only has about
10~15% chicken perianal feathers are moist, have loose bowels shape in slight water sample；It is dirty without naked eyes that dissect observes the heart, liver, spleen, intrapulmonary
Observe lesion, only about 10% chicken kidney mild swelling.III group i.e. effervescent low dose group has about 50% chicken anus
Surrounding feather is moist, wherein about 20% chicken feather filth is unclear；Dissect observes about 20% chicken kidney mild swelling, 20% chicken
Kidney moderate swelling.VI group i.e. positive controls only have about 25~30% chicken perianal feather dry cleansings, i.e., there are about
70% chicken still has phenomenon of having loose bowels；Dissect observes about 40% chicken kidney obvious tumefaction, about 30% chicken kidney mild swelling.
Detailed data and efficacy result are shown in Table 3.
3 observation of curative effect result of table
Note: colleague data Superscript letters neighbor significant difference (P < 0.05).
4, conclusion
Effervescent is used in conjunction 5 days by the mixed drink administration of 1.0g/L, 2.0g/L whole day, can be effectively caused by therapeutic agent
Injury of kidney, total effective rate is higher than the grey blue oral solution of control drug, and up to 96.7%, therefore, this effervescent treats kidney damage
The recommended dose of the clinical effect trial of wound is: effervescent 1.0g/L, is used in conjunction 5 days, and effect is better than the grey indigo plant of control drug
Oral solution.
Test two, the traditional chinese medicine composition of the invention Study on Preparation
1, instrument and reagent
(HITACHI pumps L-2130, detector L-2400 to high performance liquid chromatograph；1200 quarternary low pressure gradient of Agilent
Pump, VWD detector), air dry oven, digital display air dry oven GZX-9146MBE, vacuum oven DZF-6050 type are sprayed
Dry SY-6000, granule WK-60 type, control substance of Rutin (100080-201409, content 92.6%, Chinese food drug
Examine and determine research institute)；Astilbin reference substance (lot number 111798-201504, purity 93.9%, Chinese food drug assay research
Institute)；For agents useful for same in addition to methanol, acetonitrile are chromatographically pure, remaining reagent is that analysis is pure；Wahaha Pure Water.
2, method
2.1 Different Extraction Methods compare
Following 3 kinds of extracting methods are devised, using the rate of transform of astilbin and rutin as inspection target.
The extraction process of use is as follows:
Technique 1: smilax, rhizoma imperatae, motherwort, sophora flower, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae Six-element medicinal material offer medicine in prescription ratio, add 10
Amount water decocts 2 times, each 1h again, and merging filtrate is concentrated into every milliliter of about 0.25g containing medicinal material；
Technique 2: 10 times of smilax 60% alcohol refluxs of amount extract 2 times, sophora flower, rhizoma imperatae, motherwort, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae 10
Amount water decocts 2 times, each 1h again, and merging filtrate is concentrated into every milliliter of about 0.25g containing medicinal material.
Technique 3: sophora flower and 10 times of smilax 60% alcohol refluxs of amount extract 2 times, rhizoma imperatae, motherwort, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae 10
Amount water decocts 2 times, each 1h again, and merging filtrate is concentrated into every milliliter of about 0.25g containing medicinal material.
Content assaying method according to veterinary drug allusion quotation rhizoma smilacis glabrae medicinal material method, it may be assumed that
High effective liquid chromatography for measuring: C18 chromatographic column；Mobile phase: methanol/1% acetic acid (31:69)；Detection wavelength:
291nm (astilbin), 257nm (rutin).
Concentrate will be extracted to shake up, precision measures 1ml into 50mL volumetric flask, adds 60% methanol constant volume, high-efficient liquid phase color
Spectrometry measurement, sample volume 10uL record the peak area of astilbin and rutin；
It is according to the content that the content assaying method of pharmacopeia smilax and sophora flower measures to obtain astilbin in smilax
1.11%；The content of rutin is 6.92% in sophora flower.
The rate of transform for calculating extraction by different technology astilbin and rutin, is shown in Table 4.
4 extraction process of table compares
As can be seen from Table 4, in order to guarantee the rate of transform of effective component in smilax and sophora flower, smilax selects alcohol extracting
Technique, sophora flower, rhizoma imperatae, motherwort, rhizoma alismatis and Rhizoma Atractylodis Macrocephalae select extraction process by water.
Smilax alcohol extraction process:
Rhizoma smilacis glabrae medicinal material is taken, crushed 10 meshes, is uniformly mixed, weighs 50g (guaranteeing that sampling is uniform as far as possible) respectively, according to
The condition of orthogonal array extracts, and extracting solution filtering, filtrate merges concentration and recovery ethyl alcohol, is finally settled to 100mL.Contain
Quantity measuring method according to veterinary drug allusion quotation rhizoma smilacis glabrae medicinal material method, it may be assumed that
High effective liquid chromatography for measuring: C18 chromatographic column；Mobile phase: methanol/1% acetic acid (31:69)；Detection wavelength:
291nm.Concentrate will be extracted to shake up, precision measures 1ml into 50mL volumetric flask, adds 60% methanol constant volume, filters, and measures, meter
The concentration and the rate of transform for calculating concentrate effective component astilbin, as a result see the table below 5.
The factor level table that 5 smilax of table extracts
6 orthogonal design of table and intuitive analytical table (in conjunction with 5 numerical value of table)
7 analysis of variance table p=0.05 of table
Result can be seen that four factors to the extraction rate impact size order of astilbin from table 6 and 7 are as follows: extract
Number > concentration of alcohol > extraction time > liquid-solid ratio.
It can be seen that concentration of alcohol and extraction time from 7 analysis of variance table of table to have a significant impact to recovery rate tool.
As can be seen from Table 5, the highest level of extraction time is 3 times, and 60% and 70% ethyl alcohol extraction effect difference is not
Greatly, the highest level of extraction time is 90min, and the highest level of liquid-solid ratio is 12.
In conjunction with table 5, table 6 and table 7, considers from extraction efficiency and cost angle, select smilax extraction process are as follows: 60% ethyl alcohol
It extracts, liquid-solid ratio 8, extraction time 60min, extraction time is 2 times.
Sophora flower, motherwort, rhizoma imperatae, rhizoma alismatis and Rhizoma Atractylodis Macrocephalae water extraction process:
The major parameter for influencing water decocting process includes amount of water, extraction time, extraction time etc., using L9(34) orthogonal
Optimized extraction techniques parameter is tested, is to investigate to refer to rutin content using liquid-solid ratio, extraction time, extraction time as investigation factor
Mark, sets orthogonal test below.
About amount of water, in general: rhizome medication is generally with 8 times of medicinal material amount, leaf flower and the general medication of herb medication
12 times of material amount, rhizoma imperatae, Rhizoma Atractylodis Macrocephalae, rhizoma alismatis belong to root class, and sophora flower, mother wort are in the latter.Extraction time: it generally at least extracts
60min-120min, extraction time are 1-3 times.
Take sophora flower 9.3g, rhizoma imperatae 36.6g, motherwort 9.3g, rhizoma alismatis 2.8g, Rhizoma Atractylodis Macrocephalae 2.6g according to following orthogonal arrages through mentioning
It takes, be concentrated into 250ml, measure the content of rutin.
Content assaying method are as follows:
High effective liquid chromatography for measuring: C18 chromatographic column；Mobile phase: methanol/1% acetic acid (35:65)；Detection wavelength:
257nm.Said extracted concentrate is shaken up, precision measures 1ml into 50mL volumetric flask, adds 50% methanol constant volume, filters, and surveys
It is fixed, the concentration of concentrate rutin is calculated, the rate of transform of rutin is calculated, quantitative drying measurement yield of extract is taken, is shifted according to rutin
Rate and yield of extract account for 50% weight calculation, referring to table 9.
8 factor level table of table
9 sophora flower of table, rhizoma imperatae, motherwort, rhizoma alismatis and the intuitive analytical table of Rhizoma Atractylodis Macrocephalae extraction process by water (in conjunction with 8 numerical value of table)
10 sophora flower of table, rhizoma imperatae, motherwort, rhizoma alismatis and Rhizoma Atractylodis Macrocephalae extraction process by water analysis of variance table
A=0.05
When using rutin content as evaluation index, each factor is followed successively by C > A > B to the influence degree of extraction effect, that is, extracts
Number > liquid-solid ratio > extraction time, analysis of variance table show that extraction time has significant difference, can see in intuitive analytical table
Out, extract 2 times and extract 3 difference it is little, from save the cost, improve efficiency from the point of view of, determine optimum extraction process are as follows:
A1B1C2, that is, liquid-solid ratio 8, extraction time 60min, extraction time 2 times.
The investigation of 2.4 extracting solutions concentrate drying mode
It is concentrated under reduced pressure and effective component astilbin is concentrated for normal pressure and the rate of transform of rutin is not much different.Concentration is concentrated under reduced pressure
High-efficient, temperature is low and constant, therefore selects reduced pressure mode.
Drying process has investigated forced air drying respectively, has been dried under reduced pressure and is spray-dried three kinds of drying modes.Extracting solution is dense
It is reduced to relative density 1.06 (60 DEG C), takes out 20ml and keep sample to be measured, remaining sample is divided into 4 parts, carries out forced air drying respectively
(2 parts) are dried under reduced pressure and are spray-dried, and record dry time-consuming, dry cream moisture content are measured using dry weight-loss method, before drying
Concentrate be reference, calculate loss of effective components situation.
Forced air drying (1): use GZX-9146MBE digital display air dry oven, 80 DEG C of temperature, time about 6h；Forced air drying
(2): use GZX-9146MBE digital display air dry oven, 95 DEG C of temperature, time 12h；It is dried under reduced pressure: true using DZF-6050 type
Empty drying box, adds phosphorus pentoxide to absorb water by 50 DEG C, time about 4h；Spray drying: dry using SY-6000 laboratory spray
Machine, 170 DEG C of inlet air temperature.
11 drying process investigation table of table
As can be seen from Table 11, drying mode is the committed step for influencing active constituent content, forced air drying and decompression
Dry two kinds of drying modes take a long time, and loss of effective components is higher, in practice it has proved that: temperature is higher, and the time is longer, effectively at
Divide loss bigger.Spray drying makes to extract concentrate after being atomized, then with hot air, moisture rapid vaporization obtains drying
Product, test confirm that effective component is retained to the greatest extent.
The preparation of 2.5 preparations
Effervescent formulation is often to be prepared into tablet or granule using suitable bronsted lowry acids and bases bronsted lowry as a kind of dosage form made of disintegrating agent.
Preparation is set due to great amount of carbon dioxide gas can be generated after entering water to be easier to dissolve, this product is prepared into effervescent can be to avoid
Because stirring unevenness causes this product dissolution to be not thorough when farm largely uses.
The selection of acid-base pair: the pairing of gas-producing disintegrant soda acid can be selected: citric acid and NaHCO3；Tartaric acid and NaHCO3；
Citric acid and Na2CO3；Tartaric acid and Na2CO3；Citric acid, tartaric acid and NaHCO3；Citric acid, tartaric acid and Na2CO3 etc. are more
A series；Wherein, citric acid is strong organic acid, and good in taste, and NaHCO3 and Na2CO3 comparison generate used in same gas
Quality it is few, therefore alkali select NaHCO3.Document report effect when the ratio of citric acid and NaHCO3 are 1-1.5:1 is preferable.
The selection and dosage of PEG6000: due in effervescent acid source and alkali source met during preparation and storage
Water can generate carbon dioxide, the poor taste of alkali thus by alkali source therein with PEG6000 melt include, through preliminary experiment determine
The ratio range of PEG6000 and NaHCO3 is 0.8-1.2.
Wetting agent selects: directly selecting ethyl alcohol as wetting agent, generates carbon dioxide to prevent soda acid from meeting water.
Filler and corrigent: selection dextrin and sucrose.
Formulation and technology: NaHCO3 being melted with PEG6000 and is included, and is mixed, cooling, is crushed, and after sieving, is added to spray drying
Extract powder in, add suitable citric acid, dextrin and appropriate sucrose, add ethyl alcohol as wetting agent pelletize, be drying to obtain.
Optimization of orthogonal test formulation and technology, 12 orthogonal experiment factor level table of table are as follows.With particle recovery rate, effervesce time
For inspection target.Particle recovery rate it is higher scoring it is higher, with recovery rate it is highest be 100 points, the effervesce time refers to 10g particle
The time being totally dispersed into 200ml water, time more short commentary point is higher, and the time, most short person remembered 100 points.Particle recovery rate and effervesce
Time weighting accounts for 50%, i.e. comprehensive score=(particle recovery rate score+effervesce time score)/2 respectively.With comprehensive score into
The intuitive analysis of row and variance analysis, obtain intuitive analytical table and analysis of variance table.
12 orthogonal experiment factor level table of table
13 experimental design of table and intuitive analytical table (in conjunction with 12 numerical value of table)
14 analysis of variance table of table
By intuitive analytical table 13 it can be seen that 3 factors to this product particle recovery rate and effervesce time influence sequence be A >
The ratio of C > B, i.e. PEG6000 and NaHCO3 influence maximum, the followed by ratio of dextrin and sucrose, are finally soda acid ratio.
The optimum level of the ratio of PEG6000 and NaHCO3 is 0.8, and the optimum level of soda acid ratio is 1.25, dextrin sucrose ratio
Optimum level is 1.
PEG6000/NaHCO3 has a significant impact to result tool it can be seen from analysis of variance table 14.To sum up, this is obtained
The NaHCO3 that the best effervescence granular preparation process of product is 100g is added in the PEG6000 of 80g melting, stirs evenly, lets cool,
Flour sieving, add the citric acid of extract powder, 125g, dextrin: sucrose (1:1) supplies 1000g, adds alcohol granulation to obtain the final product.
Test three, the traditional chinese medicine composition of the invention assay
1, instrument and reagent
1260 high performance liquid chromatograph of Agilent (G1311C quaternary pump, G1329B automatic sampling instrument, G1316A column temperature
Case, G4212B diode array detector, Agilent chem workstation)；1200 high performance liquid chromatograph of Agilent (is equipped with
G1322A degasser, G1311A quaternary pump, G1329A automatic sampling instrument, G1315D diode array detector, Agilentization
Learn work station).
(lot number 110713111798-201504, Nat'l Pharmaceutical & Biological Products Control Institute, C21H22O11 contain astilbin
Amount is 93.9% meter)；(lot number 100080-201409, Nat'l Pharmaceutical & Biological Products Control Institute, C27H30O16 content are rutin
92.6%)；Acetonitrile, methanol are chromatographically pure.
2, content assaying method
2.1, the preparation of Chinese medicine of the present invention: Chinese medicine of the present invention is prepared by following prescription and preparation process.
2.1.1, prescription: smilax 366g, rhizoma imperatae 366g, sophora flower 93g, motherwort 93g, Pogostemon cablin 28g, rhizoma alismatis 28g,
Rhizoma Atractylodis Macrocephalae 26g；
2.1.2, preparation process:
1. taking smilax 366g that 8 times of 60% alcohol refluxs of amount is added to extract twice, 60 minutes every time, what merging obtained twice was mentioned
Liquid is taken, and is filtered, ethyl alcohol is finally recycled；
2. taking sophora flower 93g, motherwort 93g, rhizoma imperatae 366g, rhizoma alismatis 28g, Rhizoma Atractylodis Macrocephalae 26g that 8 times of amount water is added to extract twice, often
Secondary 60 minutes, merges obtained extracting solution twice, be filtered；
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, use be concentrated under reduced pressure mode
Total extract is concentrated into relative density about 1.06 (60 DEG C), then by the total extract after concentration by the way of spray drying
Spray drying is carried out, spray powder is obtained；
4. taking Pogostemon cablin, Pogostemon cablin is crushed to 100 mesh, obtains Pogostemon cablin fine powder, then by 100gNaHCO3It is added
80g melting PEG6000 in, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, 125g citron
Acid, dextrin, sucrose add alcohol granulation up to effervescent.
2.2, the assay of astilbin and rutin
2.2.1, chromatographic condition
Chromatographic column: using octadecylsilane chemically bonded silica as filler, mobile phase: -0.1% acetum of methanol (36:
It 64) is mobile phase, flow velocity: 1ml/min, Detection wavelength are 257nm and 291nm, and theoretical cam curve should be not less than 4000；
2.2.2, solution preparation
The preparation of reference substance solution: taking astilbin and appropriate control substance of Rutin, accurately weighed, and 60% methanol is added to be made often
Milliliter 50 μ g and 100 μ g solution to get.
The preparation of test solution: taking the powder 1.0g that this product is finely ground, accurately weighed, sets in stuffed conical flask, precision plus
Enter 60% methanol 50ml, close plug, weighed weight is ultrasonically treated 30 minutes, lets cool, then weighed weight, supplied and subtracted with 60% methanol
The weight of mistake, shakes up, filtration, take subsequent filtrate to get.
The preparation of smilax negative sample solution: the medicinal material for removing remaining prescription outside smilax is prepared according to preparation process
At the negative sample of scarce smilax, it is made in the same way of the negative sample solution of scarce smilax.
The preparation of sophora flower negative sample solution: the medicinal material for removing remaining prescription outside smilax is prepared into according to preparation process
The negative sample for lacking smilax, is made in the same way of the negative sample solution of scarce smilax.
2.2.3, detection method
It is accurate respectively to measure above-mentioned reference substance, each 10 μ L of negative sample solution, high performance liquid chromatograph is injected, is examined
It surveys, as a result as shown in Fig. 1.
Under the chromatographic condition, in the map referring to 3 sophora flower negative sample of attached drawing, the rutin peak in the map with test sample
It is noiseless on position；In map referring to 2 smilax negative sample of attached drawing, in the map of test sample on astilbin peak position
It is noiseless.The present invention uses the same chromatographic condition, different Detection wavelengths, and single injected sampling can detect two principal components simultaneously,
And it does not interfere with each other, the detection efficiency greatly improved.
2.2.4, the drafting of standard curve
Accurately weighed astilbin and control substance of Rutin are set in 100ml measuring bottle, are settled to quarter after the dissolution of 60% methanol is added
Degree mixes, obtains the reference substance solution containing astilbin 106.16 μ g/ml and the 295.49 μ g/ml containing rutin.It is above-mentioned right that precision measures
It is appropriate according to product solution, with 60% methanol dilution, obtain containing 5.31 μ g/ml of astilbin, 10.62 μ g/ml, 16.99 μ g/ml,
The control series product solution of 21.23 μ g/ml, 42.47 μ g/ml, 106.16 μ g/ml；Containing 10.77 μ g/ml of rutin, 21.55 μ g/
The control series product solution of ml, 34.48 μ g/ml, 43.09 μ g/ml, 86.19 μ g/ml, 215.47 μ g/ml.
Above-mentioned control series product solution is taken, is analyzed by the chromatographic condition of foundation, records chromatogram and peak area, as a result
Referring to attached Figure 4 and 5, using astilbin peak area as ordinate, the concentration (μ g/ml) of astilbin is abscissa, is carried out linear
It returns, obtains the standard curve (n=6) of astilbin.Regression equation: y=22.863x-12.097, R2=0.9999.As a result:
The content of astilbin linear relationship within the scope of 5.31 μ of μ g/ml~106.16 g/ml is good.It is vertical sit with rutin peak area
Mark, the concentration (μ g/ml) of rutin are abscissa, carry out linear regression, obtain the standard curve (n=6) of rutin, regression equation: y
=20.713x-11.719, R2=1.As a result: the content of rutin is linearly closed within the scope of 10.77 μ of μ g/ml~215.47 g/ml
System is good.
2.2.5, precision
Precision draws same 10 μ L of test solution, repeats sample introduction 6 times, records chromatogram, calculates the peak face of astilbin
Product average value is 997.803, relative standard deviation 0.25%, and calculating rutin peak area value average value is 2370.825, relatively
Standard deviation is 0.16%, shows that traditional Chinese medicine test method precision of the present invention is good.
2.2.6, repeated
Prepare 6 parts of test solutions in parallel by sample solution preparation method；By above-mentioned chromatographic condition, sample introduction is analyzed respectively,
Chromatogram is recorded to calculate by standard curve respectively with the calculated by peak area content of astilbin and rutin.As a result: Chinese medicine of the present invention
The RSD of astilbin and rutin content is respectively 0.27% and 0.51% (n=6).Show that traditional Chinese medicine test method of the present invention repeats
Property is good.
2.2.7, stability
Take same sample lots to prepare test solution by sample solution preparation method, by above-mentioned chromatographic condition respectively at
0,2,4,6,8,10, sample introduction is analyzed for 12h different time, records chromatogram, peak area value is recorded, to investigate the in a few days stable of sample
Property.As a result, the content of rutin and astilbin is basicly stable in 12h, by rutin and astilbin calculated by peak area, RSD is
0.68% and 0.71%.Show that sample solution is stablized in 12 hours.
2.2.8, sample recovery rate test
Precision weighs the same lot number Chinese medicine 0.5g of the present invention of known content, and totally 6 parts, 10mL concentration, which is added, is respectively
The reference substance solution of the astilbin and rutin of 106.16 μ g/ml and 295.49 μ g/ml, adds 60% methanol constant volume to 50ml, close
Plug, weighed weight are ultrasonically treated 30 minutes, let cool, then weighed weight, the weight of less loss is supplied with 60% methanol, is shaken up, and filter
Cross, take subsequent filtrate to get.According to high effective liquid chromatography for measuring, using octadecylsilane chemically bonded silica as filler, methanol -1%
Acetum (36:64) is mobile phase, and Detection wavelength 257nm records chromatogram.
By external standard method with astilbin and the rutin calculated by peak area rate of recovery.As a result: the average recovery rate of astilbin is
100.39%, RSD are 0.64% (n=6)；The average recovery rate of rutin is 101.97%, RSD 0.51%.Show the present invention
Chinese medicine sample recovery rate is good.
3, conclusion
Using high performance liquid chromatography to the astilbin and rutin progress assay in Chinese medicine of the present invention, other ingredients
Noiseless to measurement result, for methodological study the result shows that linear relationship is good, precision, the rate of recovery and repeatability are preferable,
It can be used for the quality control of this product.
Technical characteristic of the present invention without description can realize that details are not described herein by or using the prior art, certainly,
The above description is not a limitation of the present invention, and the present invention is also not limited to the example above, the ordinary skill of the art
The variations, modifications, additions or substitutions that personnel are made within the essential scope of the present invention also should belong to protection model of the invention
It encloses.
Claims (8)
1. a kind of Chinese medicine composition for treating the swollen humidifier fever of chicken kidney, which is characterized in that the Chinese medicine composition is by following parts by weight
Raw material composition: 0.1-10 parts of smilax, 0.1-10 parts of rhizoma imperatae, 0.1-10 parts of sophora flower, 0.1-10 parts of motherwort, Pogostemon cablin
0.1-10 parts, 0.1-10 parts of rhizoma alismatis, 0.1-10 parts of Rhizoma Atractylodis Macrocephalae.
The Chinese medicine composition of humidifier fever 2. treatment chicken kidney according to claim 1 swells, which is characterized in that the Chinese traditional medicine composition
Object is made of the raw material of following parts by weight: 3.66 parts of smilax, 3.66 parts of rhizoma imperatae, 0.93 part of sophora flower, 0.93 part of motherwort, wide
0.28 part of wrinkled giant hyssop, 0.28 part of rhizoma alismatis, 0.26 part of Rhizoma Atractylodis Macrocephalae.
The Chinese medicine composition of humidifier fever 3. treatment chicken kidney according to claim 2 swells, which is characterized in that the Chinese traditional medicine composition
Object is manufactured as follows:
1. taking smilax that 20%~90% alcohol reflux is added to extract twice, 15~120 minutes every time, merge the extraction obtained twice
Liquid, and be filtered, finally recycle ethyl alcohol；
2. taking sophora flower, motherwort, rhizoma imperatae, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae extracting in water three times, 15~120 minutes every time, merge institute three times
Obtained extracting solution, is filtered；
3. by step 1. with step 2. in finally obtained extracting solution be combined and concentrated to about 1.06(60 DEG C of relative density), will be dense
Extracting solution after contracting carries out spray drying, obtains spray powder；
4. taking Pogostemon cablin, Pogostemon cablin is crushed to 80~200 mesh, obtains Pogostemon cablin fine powder, 3. spray powder that step is obtained with
Pogostemon cablin fine powder is mixed and added into conventional pharmaceutical adjuvants, is prepared into required dosage form；
5. to step, 4. the middle medicament prepared is detected.
The Chinese medicine composition of humidifier fever 4. treatment chicken kidney according to claim 3 swells, which is characterized in that the Chinese traditional medicine composition
Object is made into any one of tablet, pill, capsule, granule.
The Chinese medicine composition of humidifier fever 5. treatment chicken kidney according to claim 4 swells, which is characterized in that the effervescence granular
Agent the preparation method comprises the following steps:
1. taking smilax that 60% alcohol reflux is added to extract twice, 60 minutes every time, merge the extracting solution obtained twice, and carried out
Filter, finally recycles ethyl alcohol；
2. taking sophora flower, motherwort, rhizoma imperatae, rhizoma alismatis, Rhizoma Atractylodis Macrocephalae extracting in water twice, 60 minutes every time, merge obtained twice
Extracting solution is filtered；
3. by step 1. with step 2. in finally obtained extracting solution merge to obtain total extract, using be concentrated under reduced pressure mode will be total
Extracting solution is concentrated into about 1.06(60 DEG C of relative density), then the total extract after concentration is carried out by the way of spray drying
Spray drying obtains spray powder；
4. taking Pogostemon cablin, Pogostemon cablin is crushed to 100 mesh, obtains Pogostemon cablin fine powder, then appropriate NaHCO3What addition melted in right amount
In PEG6000, stir evenly, let cool, flour sieving, then be added step 3. in spray powder, citric acid, dextrin, sucrose, then
Alcohol granulation is added up to effervescent；
5. to step, 4. the middle effervescent prepared is detected.
6. it is according to claim 5 treatment chicken kidney swell humidifier fever Chinese medicine composition, which is characterized in that the step 5. in
Detection method are as follows:
S1, preparation reference substance solution: taking appropriate astilbin reference substance, control substance of Rutin, accurately weighed, and 60% methanol is added to be made
Mixed solution of every 1mL containing 50 μ g of astilbin, 100 μ g of rutin, obtains reference substance solution；
S2, prepare medical fluid to be detected: take the appropriate step 4. in the effervescent for preparing and be ground into fine powder 1.0g, it is accurate
It is weighed, it pours into stuffed conical flask, 60% methanol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated 30 minutes, lets cool,
Weighed weight again is supplied the weight of less loss with 60% methanol, is shaken up, and filtration takes subsequent filtrate, obtains medical fluid to be detected；
Each 10 μ l of medical fluid to be detected of S3, the respectively accurate reference substance solution for measuring step S1 preparation and step S2 preparation, injection
Liquid chromatograph, using high performance liquid chromatography in reference substance solution and medical fluid to be detected astilbin and rutin contain
It is fixed to measure, and compares.
The Chinese medicine composition of humidifier fever 7. treatment chicken kidney according to claim 5 swells, which is characterized in that
The step 4. in, the NaHCO3It is 1:0.8, the NaHCO with the PEG6000 mass ratio3The citric acid matter
Amount ratio is 1:1.25, and the dextrin and the sucrose solution mass ratio are 1:1.
The Chinese medicine composition of humidifier fever 8. treatment chicken kidney according to claim 1 swells, which is characterized in that the Chinese traditional medicine composition
Object is in preparation for treating the application in the drug that chicken kidney swells humidifier fever.
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| CN1095279A (en) * | 1993-05-17 | 1994-11-23 | 吉林省敦化市制药厂 | A kind of medicine for the treatment of nephropathy |
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Address after: Room 108, Business Service Center, No. 1318 Wangsha Road, Chengyang District, Qingdao City, Shandong Province Applicant after: QINGDAO VLAND BIOTECH Inc. Applicant after: QINGDAO ANIMAL PROTECTION NATIONAL ENGINEERING TECHNOLOGY RESEARCH CENTER CO.,LTD. Address before: 266000 No. 3 Chunhai Road, Chengyang District, Qingdao City, Shandong Province Applicant before: QINGDAO VLAND BIOTECH Inc. Applicant before: QINGDAO ANIMAL PROTECTION NATIONAL ENGINEERING TECHNOLOGY RESEARCH CENTER CO.,LTD. |
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Application publication date: 20190806 |