CN106588827B - For treating the extracting method and application of the spun gold crab apple extract of ulcerative colitis - Google Patents
For treating the extracting method and application of the spun gold crab apple extract of ulcerative colitis Download PDFInfo
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Abstract
The present invention provides a kind of active pharmaceutical ingredients for being used to treat ulcerative colitis extracted from spun gold Malus spectabilis, the ingredient can reinforce mucous membrane of colon shielding guaranteeing role, film lymph node bacterium transport ratio is reduced, colon is prevented to shorten, improves ulcerative colitis curative effect.
Description
Technical field
The present invention relates to natural drug extractive technique fields, more particularly to a kind of for treating the gold of ulcerative colitis
Silk crab apple extract.
Background technique
Ulcerative colitis belongs to a kind of nonspecific inflammatory enteropathy, and clinical manifestation is mainly mucus pus and blood stool, diarrhea, abdomen
Pain pain, tenesmus and different degrees of constitutional symptom etc., lesion primary limitation is distributed in colorectal mucosa and submucosa.It should
Sick protracted course of disease, clinic there is no the method for radical cure, induce and maintain clinical remission, prevention and treatment complication, improvement patients ' life quality to be
Clinical treatment target at present.Clinically for the disease mainly with immunobiologic agent, probiotics, immunosuppressor, sugared cortical hormone
The treatment methods such as element, make conditions of patients alleviation, improve patients ' life quality etc..
Replace phloroglucinol derivatives compound (PPAPs) containing natural polycyclic polyisocyanate pentenyl in hypericum, belongs to
Hypericin, the parent nucleus of this structure are phloroglucins, usually by benzoyl, isobutyryl or 2- Metliyl-butyyl and more
A isopentene group replaces.The diversity of structure makes the bioactivity for causing such compound to have multiplicity, including antibiotic property, anti-inflammatory
The nervous systems effects such as property, antiviral, antidepression.PPAP class compound has become natural product chemistry and correlation in recent years
One new research hotspot in field.
Rigid wait of being permitted of Kunming Inst. of Botany, Chinese Academy of Sciences extracts from spoon calyx Hypericum Chinense (Guttiferae Hypericum)
12 kinds of bicyclic polyisocyanate pentenyls replace phloroglucinol derivatives compound (BPPAs), and a variety of monocycle isophthalic three are extracted from Herba Hyperici Patuli
Phenolic compound, and it was found that these monocycle phloroglucinol derivatives compounds have antitumor activity.
The spun gold Malus spectabilis in Shandong Laoshan region is also a common kind in Guttiferae Hypericum, and the applicant is logical
Cross the study found that its also contain there are many bicyclic polyisocyanate pentenyl replace phloroglucinol derivatives compound (BPPAs).Due to this kindization
Closing object has effects that excellent antibacterial anti-inflammatory, and applicant is by extracting separation, between the bicyclic polyisocyanate pentenyls of two kinds of acquisition replace
Benzenetriol class compound (BPPAs), a stepping of going forward side by side action object pharmaceutical activity detection, one of bicyclic polyisocyanate pentenyl of discovery
Replace phloroglucinol derivatives compound that there is significant curative effect in terms for the treatment of ulcerative colitis, is worth clinical application.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of natural extraction drug extracted from spun gold Malus spectabilis at
Point, which can reinforce mucous membrane of colon shielding guaranteeing role, reduce film lymph node bacterium transport ratio, prevent colon from shortening, change
Kind ulcerative colitis curative effect.
Ulcerative colitis is treated in preparation in order to solve the above technical problems, the present invention provides a kind of active pharmaceutical ingredients
Drug in application, structural formula are as follows:
Wherein, the active pharmaceutical ingredient is extracted from spun gold Malus spectabilis.
The present invention also provides the extracting methods of the active pharmaceutical ingredient of above-mentioned treatment ulcerative colitis comprising,
The first step takes the root and leaf portion point of spun gold Malus spectabilis, pulverizes, mix；
Second step, the mixture 15kg for taking the first step to obtain are impregnated 4 times using methanol, are impregnated 24 hours, are made every time every time
It is 10L with quantity of methyl alcohol, 4 soak filterings merge, remove solvent using Rotary Evaporators, and the concentration for obtaining 3.3kg produces
Object, enriched product are liquid；
Third step, by enriched product at 4 parts, every part with etc. the silica gel of quality mix, further revolve on a rotary evaporator
Turning to evaporate being partly dissolved for remnants, obtain solid-state object to be filtered, is ground into powder, upper silicagel column carries out coarse filtration using chloroform,
And it obtains bicyclic polyisocyanate pentenyl and replaces phloroglucinol derivatives compound (BPPAs) 319.8g
4th step, the product that third step obtains use liquid chromatogram post separation, and eluent uses methanol percent by volume
80% methanol aqueous solution isolates 4 kinds of different crude products, respectively the first crude product 41.1g, the second crude product 56.3g, the
Three crude product 35.7g, the 4th crude product 39.2g；
5th step uses silica gel column purification to the second crude product, and the eluent of use is respectively ether/ethyl acetate volume
Mixed solution than 1: 2, the mixed solution and pure ethyl acetate of ether/ethyl acetate volume ratio 1: 1 isolate 6 kinds of thick productions
Object, respectively the first crude product 8.1g, the second crude product 5.5g, third crude product 16.3g, the 4th crude product 7.2g, the 5th are thick
Product 6.6g, the 6th crude product 3.1g；
6th step is purified the third crude product that the 5th step obtains using sephadex column Sephadex-LH20, elution
Liquid is eluted using chloroform/methanol volume ratio 1: 1 as eluent, and four kinds of crude products, respectively the first crude product are obtained
3.5g, the second crude product 2.9g, third crude product 2.7g, the 4th crude product 1.8g；
7th step, the first crude product obtained for the 6th step further uses silicagel column to purify, used to wash
De- liquid is petrol ether/ethyl acetate volume ratio 100: 1, petrol ether/ethyl acetate volume ratio 50: 1, petroleum ether/acetic acid second respectively
Ester volume ratio 10: 1, petrol ether/ethyl acetate volume ratio 2: 1, petrol ether/ethyl acetate volume ratio 1: 1, pure ethyl acetate, point
Two kinds of products are separated out, the first product quality is 217mg, and the second product quality 151mg, first product is exactly that the treatment is burst
The active pharmaceutical ingredient of ulcer colitis.
The present invention also provides a kind of for treating the endo-medicine of ulcerative colitis comprising chemical combination shown in formula 1
Object as active pharmaceutical ingredient and pharmaceutically acceptable carrier and excipient,
Mass percent of the active pharmaceutical ingredient in entire drug is 10%~20%, preferably 10%~15%.
The endo-medicine can be prepared into various regular dosage forms using customary preparation methods.
Wherein the endo-medicine is prepared into tablet, capsule, pill and oral solution.
The present invention also provides a kind of for treating the tablet of ulcerative colitis comprising 1 compound represented of formula, crystallite
Cellulose, starch, magnesium stearate,
Wherein, the mass percent of each material composition is 1 compound represented 10%~20% of formula, microcrystalline cellulose 40%
~80%, starch 30%~50%, magnesium stearate 1%~3%, each material composition quality sum are 100%.
The present invention also provides the preparation methods of above-mentioned tablet, specially weigh each raw material by weight, mix, fill
Divide and stir evenly 20 minutes, particle is uniformly made, tabletting obtains tablet.
Beneficial effects of the present invention:
The present invention extracts natural extraction drug ingedient from spun gold Malus spectabilis, which, which can reinforce mucous membrane of colon shielding, protects
Barrier effect, reduces film lymph node bacterium transport ratio, and colon is prevented to shorten, and improves ulcerative colitis curative effect.
Specific embodiment
The present invention provides a kind of for treating the active pharmaceutical ingredient of ulcerative colitis, is mentioned from spun gold Malus spectabilis
It takes out.
The extracting method of the drug of the treatment ulcerative colitis specifically includes,
The first step takes the root and leaf portion point of spun gold Malus spectabilis, pulverizes, mix；
Second step, the mixture 15kg for taking the first step to obtain are impregnated 4 times using methanol, are impregnated 24 hours, are made every time every time
It is 10L with quantity of methyl alcohol, 4 soak filterings merge, remove solvent using Rotary Evaporators, and the concentration for obtaining 3.3kg produces
Object, enriched product are liquid；
Third step, by enriched product at 4 parts, every part with etc. the silica gel of quality mix, further revolve on a rotary evaporator
Turn to evaporate being partly dissolved for remnants, obtains solid-state object to be filtered, be ground into powder, upper silicagel column is carried out slightly using chloroform
Filtering, and obtain bicyclic polyisocyanate pentenyl and replace phloroglucinol derivatives compound (BPPAs) 319.8g
4th step, the product that third step obtains use liquid chromatogram post separation, and eluent uses methanol percent by volume
80% methanol aqueous solution isolates 4 kinds of different crude products, respectively the first crude product 41.1g, the second crude product 56.3g, the
Three crude product 35.7g, the 4th crude product 39.2g；
5th step uses silica gel column purification to the second crude product, and the eluent of use is respectively ether/ethyl acetate volume
Mixed solution than 1: 2, the mixed solution and pure ethyl acetate of ether/ethyl acetate volume ratio 1: 1 isolate 6 kinds of thick productions
Object, respectively the first crude product 8.1g, the second crude product 5.5g, third crude product 16.3g, the 4th crude product 7.2g, the 5th are thick
Product 6.6g, the 6th crude product 3.1g；
6th step is purified the third crude product that the 5th step obtains using sephadex column Sephadex-LH20, elution
Liquid is eluted using chloroform/methanol volume ratio 1: 1 as eluent, and four kinds of crude products, respectively the first crude product are obtained
3.5g, the second crude product 2.9g, third crude product 2.7g, the 4th crude product 1.8g；
7th step, the first crude product obtained for the 6th step further uses silicagel column to purify, used to wash
De- liquid is petrol ether/ethyl acetate volume ratio 100: 1, petrol ether/ethyl acetate volume ratio 50: 1, petroleum ether/acetic acid second respectively
Ester volume ratio 10: 1, petrol ether/ethyl acetate volume ratio 2: 1, petrol ether/ethyl acetate volume ratio 1: 1, pure ethyl acetate, point
Separate out two kinds of products, the first product quality is 217mg, the second product quality 151mg, first product be exactly treat it is exedens
The active pharmaceutical ingredient of colitis.
The present invention also provides application of 1 compound represented of formula in the drug of preparation treatment ulcerative colitis.
The present invention also provides the endo-medicines for treating ulcerative colitis comprising 1 compound represented conduct of formula
Active pharmaceutical ingredient and pharmaceutically acceptable carrier and excipient.
Mass percent of the active pharmaceutical ingredient in entire drug is 10%~20%, preferably 10%~15%.
The endo-medicine can be prepared into various regular dosage forms using customary preparation methods, be preferably prepared to tablet, glue
Wafer, pill, oral solution, are most preferably prepared into tablet.
The present invention also provides a kind of for treating the tablet of ulcerative colitis comprising 1 compound represented of formula, crystallite
Cellulose, starch, magnesium stearate, the mass percent of each material composition are 1 compound represented 10%~20% of formula, and crystallite is fine
Plain 40%~80%, starch 30%~50%, magnesium stearate 1%~3% are tieed up, each material composition quality sum is 100%.
The present invention also provides the preparation methods of above-mentioned tablet, specially weigh each raw material by weight, mix, fill
Divide and stir evenly 20 minutes, particle is uniformly made, tabletting obtains tablet.
The present invention will be described in detail below with reference to the drawings of preferred embodiments, whereby to the present invention how applied technology method
Technical problem is solved, and the realization process for reaching technical effect can fully understand and implement.
The extraction of 1 spun gold Malus spectabilis of embodiment
The root and leaf portion point for taking spun gold Malus spectabilis, are pulverized, are mixed, the mixture 15kg of acquisition is taken to be impregnated using methanol
It 4 times, impregnates 24 hours every time, the use of quantity of methyl alcohol is every time 10L, 4 soak filterings are merged, removed using Rotary Evaporators
Remove solvent, obtain the enriched product of 3.3kg, enriched product is liquid, by enriched product at 4 parts, every part with etc. quality silica gel
Mixing, further rotation evaporates being partly dissolved for remnants on a rotary evaporator, obtains solid-state object to be filtered, is ground into powder,
Upper silicagel column carries out carry out coarse filtration using chloroform, and obtains bicyclic polyisocyanate pentenyl and replace phloroglucinol derivatives compound
(BPPAs) product of acquisition is used liquid chromatogram post separation by 319.8g, and eluent uses the first of methanol percent by volume 80%
Alcohol solution, isolates 4 kinds of different crude products, respectively the first crude product 41.1g, the second crude product 56.3g, third crude product
35.7g, the 4th crude product 39.2g use silica gel column purification to the second crude product, and the eluent of use is respectively ether/acetic acid
The mixed solution of ethyl ester volume ratio 1: 2, the mixed solution and pure ethyl acetate of ether/ethyl acetate volume ratio 1: 1, isolates
6 kinds of crude products, respectively the first crude product 8.1g, the second crude product 5.5g, third crude product 16.3g, the 4th crude product 7.2g,
5th crude product 6.6g, the 6th crude product 3.1g use sephadex column Sephadex- to the third crude product obtained herein
LH20 purifying, eluent are eluted using chloroform/methanol volume ratio 1: 1 as eluent, obtain four kinds of crude products, respectively
First crude product 3.5g, the second crude product 2.9g, third crude product 2.7g, the 4th crude product 1.8g, for obtain herein
One crude product further uses silicagel column to be purified, and used eluent is petrol ether/ethyl acetate volume ratio 100 respectively
: 1, petrol ether/ethyl acetate volume ratio 50: 1, petrol ether/ethyl acetate volume ratio 10: 1, petrol ether/ethyl acetate volume ratio 2
: 1, petrol ether/ethyl acetate volume ratio 1: 1, pure ethyl acetate isolates two kinds of products, and the first product is object shown in formula 1
Matter, quality 217mg, the second product are substance shown in formula 2, and quality 151mg, first product is exactly to treat exedens knot
The active pharmaceutical ingredient of enteritis.
First product shown in formula 1 uses CDCl3Nmr analysis is carried out as solvent.
1H NMR(CDCl3, 600MHz): δ 5.72 (1H, d)；5.64 (1H, m)；5.08 (1H, brs)；4.92 (1H, t)；
4.71 (1H, t)；4.49 (1H, s)；2.94 (1H, m)；2.64 (1H, m)；2.59 (1H, sept)；2.51 (1H, dd)；2.25
(1H, m)；2.19 (1H, m)；2.16 (1H, m)；2.05 (1H, m)；1.82 (1H, m)；1.75 (3H, s)；1.65 (12H, s)；
1.58 (2H, overlap)；1.54 (1H, m)；1.54 (3H, s)；1.38 (3H, s)；1.37 (3H, s)；1.13 (3H, s)；1.10
(3H, d)；0.97 (3H, d)；0.91 (2H, t).
Second product shown in formula 2 uses CDCl3Nmr analysis is carried out as solvent.
1H NMR(CDCl3, 600MHz): δ 5.72 (1H, d)；5.61 (1H, m)；5.07 (1H, brs)；4.92 (1H, t)；
4.71 (1H, t)；4.47 (1H, s)；2.97 (1H, dd)；2.62 (1H, dd)；2.51 (1H, dd)；2.42 (1H, m)；2.30 (2H,
m)；2.15 (1H, m)；2.07 (1H, overlap)；1.83 (1H, m)；1.75 (3H, s)；1.70 (2H, m)；1.64 (12H, s)；
1.60 (2H, overlap)；1.60 (3H, s)；1.57 (1H, m)；1.37 (3H, s)；1.37 (3H, s)；1.31 (3H, s)；1.13
(3H, s)；0.95 (3H, d)；0.97 (3H, d).
Pharmacodynamic experiment
Experimental animal: 100 male mices, between weight 20g~24g, by Qingdao City experimental animal and zoopery
The heart provides.
Experimental drug: trinitrobenzene sulfonic acid (TNBS), Sigma company provide.
Grouping and model: 100 mouse are randomly divided into normal group, model group, 1 group for the treatment of, treatment 2 groups and control group, often
Group 20.
Modeling method, except for the normal group, after remaining 4 groups of fasting 24 hours, the silicone tube of diameter 2mm is inserted in etherization
Enter at mouse Colon to anus 8cm, configuring the ethanol solution of trinitrobenzene sulfonic acid, (it is 30% that 20mgTNBS, which is dissolved in determining alcohol,
In ethanol solution), using the ethanol solution bowel lavage of the 0.5ml trinitrobenzene sulfonic acid, after bowel lavage, animal is made to lie low, retained
It is 20 minutes, naturally awake, free diet.Except for the normal group, in 4 groups of modeling 3 days, there is diarrhea, mucus purulence blood in all animals
After an action of the bowels, modeling success.
Medication
Compound 2 shown in compound 1 shown in formula 1 and formula 2 is dissolved in distilled water respectively and is configured to aqueous solution, every 1ml
The quality of the compound 1 and compound 2 that dissolve in solution is 35mg, and 4 DEG C are stored in spare in refrigerator, 1ml/d bowel lavage, control group
Salicylazosulfapyridine is given, specification 250mg/ piece grinds, is configured to suspension with distilled water, is administered according to 0.3g/kg, 1ml/d
Bowel lavage, model group give the chloride injection bowel lavage of isometric 0.9%, and equal 10 days are 1 course for the treatment of.
Observation index
General status, colon lengths and the mass change of animal during observation modeling
On 11st, cervical dislocation put to death each group mouse, and dissociate colon, took out entire colon, with sterile 0.9% is pre-chilled
Sodium chloride injection is clean by colonic irrigation, observes and records the substantially change of each group's mouse Colon, measures entire colon
Length.
Referring to disease activity index (DAI) standards of grading, the daily weight for observing mouse, fecal character and (connection of occulting blood
Aniline process measurement) situation, and record scoring.
1 DAI standards of grading of table
| It scores | Weight declines (%) | Stool | Stool blood |
| 0 | < 1 | Amount less, firmly, it is dry, not glutinous, do not dissipate | Without color |
| 1 | 1~5 | Amount less, firmly, it is wet, glutinous | Color reaction is dotted |
| 2 | 6~10 | It measures more, soft, very glutinous | Continue blue |
| 3 | 11~15 | It measures more, soft, scattered | Dark color is defecated+occults blood blue |
| 4 | > 15 | Loose stools | Bloody stool+dark blue reaction |
Note: DAI=(weight declines score+stool score+hematochezia score)/3
Each group mouse lymphonodi mesenterici bacterial translocation rate
Clip universal mesentery lymph node, is homogenized respectively after weighing quality, and tissue is homogenized each 0.1ml and is trained in plain agar
It supports after being cultivated for 24 hours in 37 DEG C of incubators on base using painting bacterium method, according to diluting colonies count multiples bacterium colony number, (every g tissue contains
Bacterium amount), it is indicated with Colony Forming Unit (CFU), every part of sample does double culture.Calculating bacterium transport ratio, bacterium transport ratio=
Positive bacterial culture number of elements/total the number of elements of culture.
Statistical method
Calculating analysis is carried out using 16.0 statistics software of SPSS, measurement data uses mean ± standard deviation Table
Show, mean compares using one-way analysis of variance between multiple groups, and P < 0.05 is that difference is statistically significant.
As a result
Each group mouse general status compares
During experiment, normal to organize mouse hair color gloss, stool and urine is normal, and spirit is gamboled, and 2 groups of model group and treatment are from modeling
3d starts apathetic depressed, and fur is loosely matt, and loss of appetite is had loose bowels, bloody stool, and form is thin, weight loss, feed
It reduces, motion frequency reduces.Control group, 1 group for the treatment of are identical as model group symptom before the treatment, after treatment, control group bloody stool number
Amount is reduced, and stool is formed, but effect is unobvious, and 1 group of stool for the treatment of forms completely, and bloody stool quantity is almost without weight
Mitigate it is unobvious, general status better than model group, control group, treatment 2 groups.
Each group DAI scoring is compared, and the results are shown in Table 2.
± Δ is compared in 2 each group DAI of table scoring
| Group | n | DAI scoring |
| Treat 1 group | 20 | 1.09±0.13*Δ |
| Treat 2 groups | 20 | 3.61±0.25 |
| Model group | 20 | 3.92±0.28 |
| Normal group | 20 | 0.41±0.10 |
| Control group | 20 | 1.57±0.30* |
Compared with model group,*P < 0.01；Compared with the control group,ΔP < 0.05.
By 2 result of table it is found that 1 group for the treatment of and the control group disease activity index of the compound 1 for using the present invention to extract
Scoring is compared with 2 groups of model group and treatment, and difference is statistically significant, P < 0.01, and compared with the control group, difference has for 1 group for the treatment of
Statistical significance, P < 0.05, it is seen that the compound 1 that the present invention extracts is significantly improved ulcerative colitis tool.
Each group mouse Colon length and mass change compare, and the results are shown in Table 3.
3 each group mouse Colon length of table and mass change compare
Compared with model group,*P < 0.01；Compared with the control group,ΔP < 0.05.
The colon lengths of each group mouse after can be seen that trinitrobenzene sulfonic acid (TNBS) bowel lavage by the result of table 3 are equal
There is different degrees of shortening, and after treatment, 2 groups of 1 group for the treatment of, control group colon lengths and model group, treatment significant differences,
P < 0.01, and treating 1 group and control group more also has more significant difference, P < 0.05, each group difference is not in colon quality
Significantly, and from length in terms of mass ratio, 1 group for the treatment of, control group and model group treat 2 groups of significant differences, P < 0.01.It can be seen that
The compound 1 that the present invention extracts can prevent colon from shortening.
Each group mouse lymphonodi mesenterici bacterium transport ratio, the results are shown in Table 4.
4 each group mouse lymphonodi mesenterici bacterium transport ratio of table compares
| Group | N | Bacterium transport ratio (%) |
| Treat 1 group | 20 | 3*Δ |
| Treat 2 groups | 20 | 69 |
| Model group | 20 | 77 |
| Normal group | 20 | 0 |
| Control group | 20 | 43* |
Compared with model group,*P < 0.01；Compared with the control group,ΔP < 0.05.
As can be known from the results of Table 4, the lymphonodi mesenterici bacterium transport ratio of model group is significantly higher than normal group and treatment 1
Group, treats 2 groups of lymphonodi mesenterici bacterium transport ratios and model group difference is little, and difference is not shown between 1 group and normal group for the treatment of
It writes, illustrates that drug provided by the invention can reinforce mucous membrane of colon shielding guaranteeing role.
All above-mentioned this intellectual properties of primarily implementation, there is no this new products of implementation of setting limitation other forms
And/or new method.Those skilled in the art will utilize this important information, above content modification, to realize similar execution feelings
Condition.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (9)
1. a kind of extracting method for the active pharmaceutical ingredient for treating ulcerative colitis, it is characterised in that: the pharmaceutical activity at
It point is extracted from spun gold Malus spectabilis,
The structural formula of the active pharmaceutical ingredient is
The extracting method of the active pharmaceutical ingredient includes:
The first step takes the root and leaf portion point of spun gold Malus spectabilis, pulverizes, mix；
Second step, the mixture 15kg for taking the first step to obtain are impregnated 4 times using methanol, are impregnated 24 hours every time, are used first every time
Alcohol amount is 10L, and 4 soak filterings merge, remove solvent using Rotary Evaporators, obtain the enriched product of 3.3kg, dense
Contracting product is liquid；
Third step, by enriched product at 4 parts, every part with etc. the silica gel of quality mix, further rotation is steamed on a rotary evaporator
Falling remaining partial solvent, obtains solid-state object to be filtered, be ground into powder, upper silicagel column carries out carry out coarse filtration using chloroform,
And it obtains bicyclic polyisocyanate pentenyl and replaces phloroglucinol derivatives compound 319.8g
4th step, the product that third step obtains use liquid chromatogram post separation, and eluent is using methanol percent by volume 80%
Methanol aqueous solution, isolates 4 kinds of different crude products, and the first crude product 41.1g, the second crude product 56.3g, third slightly produce respectively
Object 35.7g, the 4th crude product 39.2g；
5th step uses silica gel column purification to the second crude product, and the eluent of use is respectively ether/ethyl acetate volume ratio 1:
2 mixed solution, ether/ethyl acetate volume ratio 1:1 mixed solution and pure ethyl acetate, isolates 6 kinds of crude products, point
Not Wei the first crude product 8.1g, the second crude product 5.5g, third crude product 16.3g, the 4th crude product 7.2g, the 5th crude product
6.6g, the 6th crude product 3.1g；
6th step purifies the third crude product that the 5th step obtains using sephadex column Sephadex-LH20, and eluent is adopted
It uses chloroform/methanol volume ratio 1:1 to be eluted as eluent, obtains four kinds of crude products, respectively the first crude product 3.5g, the
Two crude product 2.9g, third crude product 2.7g, the 4th crude product 1.8g；
7th step, the first crude product obtained for the 6th step further use silicagel column to purify, used eluent
It is petrol ether/ethyl acetate volume ratio 100:1, petrol ether/ethyl acetate volume ratio 50:1, petrol ether/ethyl acetate body respectively
Product than 10:1, petrol ether/ethyl acetate volume ratio 2:1, petrol ether/ethyl acetate volume ratio 1:1, isolate by pure ethyl acetate
Two kinds of products, the first product quality are 217mg, and the second product quality 151mg, first product is exactly that the treatment is exedens
The active pharmaceutical ingredient of colitis.
2. the drug that the active pharmaceutical ingredient extracted using extracting method described in claim 1 treats ulcerative colitis in preparation
In application.
3. a kind of for treating the endo-medicine of ulcerative colitis, it is characterised in that: including 1 compound represented of formula as medicine
Object active constituent and pharmaceutically acceptable carrier and excipient,
4. endo-medicine as claimed in claim 3, it is characterised in that: quality hundred of the active pharmaceutical ingredient in entire drug
Divide than being 10%~20%.
5. endo-medicine as described in claim 3 or 4, it is characterised in that: the endo-medicine can use customary preparation methods
It is prepared into various regular dosage forms.
6. the endo-medicine as described in claim 4 or 5, it is characterised in that: the endo-medicine is prepared into tablet, capsule, ball
Agent or oral solution.
7. a kind of for treating the tablet of ulcerative colitis, it is characterised in that: including 1 compound represented of formula, microcrystalline cellulose
Element, starch, magnesium stearate,
8. tablet as claimed in claim 7, it is characterised in that: the mass percent of each material composition is 1 compound represented of formula
10%~20%, microcrystalline cellulose 40%~80%, starch 30%~50%, magnesium stearate 1%~3%, each material composition matter
The sum of amount is 100%.
9. the preparation method of the tablet of claim 7 or 8, it is characterised in that: be specially to weigh each raw material by weight, be blended in
Together, it stirs 20 minutes, particle is uniformly made, tabletting obtains tablet.
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| CN201611241273.0A CN106588827B (en) | 2016-12-29 | 2016-12-29 | For treating the extracting method and application of the spun gold crab apple extract of ulcerative colitis |
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| CN201611241273.0A CN106588827B (en) | 2016-12-29 | 2016-12-29 | For treating the extracting method and application of the spun gold crab apple extract of ulcerative colitis |
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| CN106588827A CN106588827A (en) | 2017-04-26 |
| CN106588827B true CN106588827B (en) | 2019-03-08 |
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| CN110025629B (en) * | 2019-05-23 | 2021-03-26 | 河南大学 | Application of filamental flowering crab polysaccharide in preparing immunity enhancing medicine |
Citations (2)
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|---|---|---|---|---|
| US20020031560A1 (en) * | 1995-09-29 | 2002-03-14 | Dr. Willmar Schwabe Gmbh & Co. | Stable extract of hypercium perforatum L., processes for its preparation and pharmaceutical compositions |
| CN104744422A (en) * | 2014-11-21 | 2015-07-01 | 华中科技大学 | Compound with antitumor and anti-HIV (human immunodeficiency virus) activities in hypericum sampsonii hance as well as separation preparation and application of compound |
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2016
- 2016-12-29 CN CN201611241273.0A patent/CN106588827B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020031560A1 (en) * | 1995-09-29 | 2002-03-14 | Dr. Willmar Schwabe Gmbh & Co. | Stable extract of hypercium perforatum L., processes for its preparation and pharmaceutical compositions |
| CN104744422A (en) * | 2014-11-21 | 2015-07-01 | 华中科技大学 | Compound with antitumor and anti-HIV (human immunodeficiency virus) activities in hypericum sampsonii hance as well as separation preparation and application of compound |
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| Title |
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| Cytotoxic polycyclic polyprenylated acylphloroglucinols from Hypericum attenuatum;Zhong-bo Zhou et al;《Fitoterapia》;20140303;第95卷;第1-7页 * |
| 金丝桃的化学成分;王静等;《中国中药杂志》;20020228;第27卷(第2期);第120-122页 * |
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