CN101015611A - Extraction method of antibacterial and antidiarrhea active compound in rubus corchorifolius leaf, extractive and use thereof - Google Patents
Extraction method of antibacterial and antidiarrhea active compound in rubus corchorifolius leaf, extractive and use thereof Download PDFInfo
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- CN101015611A CN101015611A CN 200710034500 CN200710034500A CN101015611A CN 101015611 A CN101015611 A CN 101015611A CN 200710034500 CN200710034500 CN 200710034500 CN 200710034500 A CN200710034500 A CN 200710034500A CN 101015611 A CN101015611 A CN 101015611A
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Abstract
The invention discloses Rubus corchorifolius extract with antibacterial and antidiarrheal effects, and its method and application. The method comprises drying and crushing leaves of Rubus corchorifolius, extracting with ethanol, filtering, mixing the filtrates, concentrating, separating with a solvent having moderate polarity, concentrating, and drying. This extract with good antibacterial and antidiarrheal effects can be used to produce antibacterial drug, and antidiarrheal drug exhibiting inhibitory effects on intestinal peristalsis in vitro. As compared with the prior arts, the invention has the advantages of less toxic and adverse side effects and low cost.
Description
Technical field
The present invention relates to the extraction of plants ' medicinal component, specifically, provide a kind of effect of from compound in rubus corchorifolius leaf, extracting method, extract and the extract of antibacterial and diarrhea active component.
Background technology
Having antibacterial and Rubus corchorifolius (Rubus corchorifolius L.f) the diarrhea effect is a kind of machaka in the Rosaceae rubus, all there is distribution in the whole nation except that northeast, Gansu, Xinjiang, Tibet, all there is extensive distribution in mountain area, the western Hunan, the wild resource reserves are quite big, its fruit, root and stem can be used as medicine, and it is glutted to have a removing food stagnancy food, belly pain, traumatic injury, effects such as impetigo.Root has the effect of wind-damp dispelling, puts down in writing its fruit according to Compendium of Material Medica, and root and leaf are used as medicine the effect of invigorating blood circulation.
Look into new discovery, the research report of relevant rubus is more both at home and abroad, and it is less to the research of Rubus corchorifolius, it mainly concentrates on the development and use and the chemical constituent of resource, utilize its aggregate fruit to be used for food processing, utilize its tannin as industrial chemicals, the nutritional labeling of Rubus corchorifolius and value and stem and leaf Coumarins composition have been carried out preliminary study as ChenBing Hua etc.; The Study on extraction process of extracting tea polyphenols from compound in rubus corchorifolius leaf has been studied in security gift etc.; Easily wipe out with Chen Gongxi the comprehensive utilization of Rubus corchorifolius has been used as summary; Liu Jianben, Tang Mingzai inquires into the extraction and the character of Rubus corchorifolius pigment; Wu Xianjin has introduced the variation of several biochemical component content in the Rubus corchorifolius fruit growth; Bulletins such as Xu Yihua the tissue culture and the fast breeding of Rubus corchorifolius.
At present both at home and abroad the research of Rubus corchorifolius is mainly concentrated on the report of the aspects such as utilization, nutritive value, chemical constituent of resource, not seeing has antibacterial and the report diarrhea aspect, does not also see the report of relevant Rubus corchorifolius patent aspect.
Summary of the invention
The extract that the object of the present invention is to provide a kind of method of from natural plants, extracting antibacterial and antidiarrhea active, extracted according to this method and the purposes of this extract, the antibiotic and the Western medicine medicine preparation toxic and side effects that can overcome synthetic are big, the shortcoming that price is high.
For achieving the above object, embodiment of the present invention are: the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf may further comprise the steps:
(1) compound in rubus corchorifolius leaf of gathering is dried in the shade in indoor, pulverize;
(2), add to add 80% ethanol of 10 times of volumes, under the room temperature lixiviate centrifugal after 48 hours, get its supernatant, add 8 times of volume 80% ethanol again and repeat to extract 1 time;
(3), filter, merging filtrate concentrates;
(4), the solvent of the each middle polarity with 3 times of volumes of the extracting solution that will concentrate, extract as ethyl acetate, n-butyl alcohol or acetone, until extract liquid phase colourless till;
(5), with extract at 50 ℃, be rotated evaporation and concentration under the 0.09Mpa condition to the extractum shape, put that pre-cooling placed the freezer dryer lyophilization 48 hours after one day in-25 ℃ of ultra cold storage freezers.
In the step (3), described concentrate is to be rotated evaporation and concentration under 50 ℃, 0.09Mpa condition.
In the step (4), described medium polar solvent is an ethyl acetate.
Step (5) lyophilization gained mixture can further carry out chromatography, and method may further comprise the steps:
A, silica gel is dried by the fire activation in 6 hours in 105 ℃ baking oven;
B, wet method dress post, diameter=7cm, height=64cm, volume is: 2978.74cm
2, silica gel 900 grams;
C, take by weighing sample, use the acetic acid ethyl dissolution sample, add silica gel then and stir, in 50 ℃ of oven dry down, standby;
D, employing wet method dress post left standstill after installing 12 hours;
E, use a dry method on a sample, the sample that step c is handled well is packed in the chromatographic column;
F, add eluent, eluting step by step, chloroform and methanol that eluent is followed successively by 3 times of column volumes carry out gradient elution, and flow velocity 2.5ml/min collects eluent.
Among the step f, the 1st gradient is pure chloroform eluting, and each gradient is a chloroform thereafter: methanol=90: 1,80: 1,65: 1,50: 1,35: 1,20: 1, use the methanol solution eluting at last.
The present invention utilizes the natural plants plum leaf to be raw material, extracts its active substance, and this active substance has antibacterial and the diarrhea effect, and available its produced antibacterial and diarrhea medicine.The development and use compound in rubus corchorifolius leaf not only can further be excavated folks of china medicine treasure-house, make full use of the natural resources, open up new road for developing new natural drug, and the utilization of compound in rubus corchorifolius leaf can not destroy ecological environment, the aim and the meaning that meet sustainable development, tcm product broad market prospect development of new, nontoxic from compound in rubus corchorifolius leaf.
The specific embodiment
(1) extraction and the separation and purification of the antibacterial diarrhea composition of compound in rubus corchorifolius leaf
1, the extracting method of the antibacterial diarrhea composition of compound in rubus corchorifolius leaf, its concrete steps are:
(1) compound in rubus corchorifolius leaf of gathering is dried in the shade indoor, cross 20 mesh sieves and be polished into coarse powder;
(2) take by weighing 2500g compound in rubus corchorifolius leaf dry powder, add 80% ethanol of 10 times of volumes, under the room temperature lixiviate centrifugal after 48 hours, get its supernatant, add 8 times of volume 80% ethanol again and repeat to extract 1 time, centrifugal back merges centrifugal liquid, is the compound in rubus corchorifolius leaf crude extract;
(3) with crude extract at 50 ℃, be rotated evaporation and concentration under the 0.09Mpa condition, the about 500ml of concentrated solution.
2, compound in rubus corchorifolius leaf extract extraction separating method.The present invention has tested three kinds of different solvents respectively and has extracted respectively, for carrying out follow-up antibacterial and stripped intestinal test.
(1) petroleum ether extraction: the petroleum ether that concentrated solution adds 3 times of volumes at every turn extracts, repeatedly extract till petroleum ether layer is colourless, merge petroleum ether layer, with petroleum ether extraction liquid at 50 ℃, 0.09Mpa be rotated evaporation and concentration under the condition to the extractum shape, put that pre-cooling placed the freezer dryer lyophilization 48 hours after one day in-25 ℃ of ultra cold storage freezers, petroleum ether extract 25g;
(2) ethyl acetate extraction: concentrated solution adds the ethyl acetate extraction of about 3 times of volumes, repeatedly extract till ethyl acetate layer is colourless, the combined ethyl acetate layer, with acetic acid ethyl acetate extract at 50 ℃, 0.09Mpa be rotated evaporation and concentration under the condition to the extractum shape, put that pre-cooling placed the freezer dryer lyophilization 48 hours after one day in-25 ℃ of ultra cold storage freezers, acetic acid ethyl ester extract 32g;
(3) n-butanol extraction: concentrated solution adds the n-butanol extraction of about 3 times of volumes, repeatedly extract till n-butanol layer is colourless, merge n-butanol layer, with butanol extraction liquid at 50 ℃, 0.09Mpa be rotated evaporation and concentration under the condition to the extractum shape, put that pre-cooling placed the freezer dryer lyophilization 48 hours after one day in-25 ℃ of ultra cold storage freezers, n-butyl alcohol extract 56g.
3, Rubus corchorifolius active component column chromatographic isolation and purification
(1) activated silica gel: take by weighing the new silica gel 1.0Kg of 80～100 orders, put into baking oven and dried by the fire 6 hours down at 105 ℃;
(2) dress post: adopt wet method dress post, the silica gel that activation is good mixes with chloroform, stirs evenly with glass rod, topples in the post diameter=7cm, height=64cm, volume 2978.74cm while stirring
2, silica gel 900 gram, install post after, leave standstill after 12 hours and go up sample again.
(3) go up sample: ethyl acetate extraction layer sample 30g, use acetic acid ethyl dissolution, it is even to add silica gel the mixings splash bar that 60g activates, and places in the culture dish upper props after 50 ℃ of oven dry grindings.
(4) eluting: add eluent, step by step eluting.This experiment is carried out gradient elution with chloroform and methanol, and the 1st gradient is pure chloroform eluting, and each gradient is a chloroform thereafter: methanol=90: 1,80: 1,65: 1,50: 1,35: 1,20: 1, use the methanol solution eluting at last; Effluent volume is that 3 times of column volumes are 8936ml.
(5) merging of column chromatography sample
After column chromatography is finished, merge eluent, statistics altogether 110 bottles of eluents, per 10 bottles synthesize a sample, combination situation is as follows: 1-10,11-20,21-30,31-40,41-50,51-60,61-70,71-80,81-90,91-100,101-110.Wherein 2,3,4,6,7,9,10 groups respectively account for 2 gradients, and 1,5,8,11 respectively is the eluent merging in the gradient, gets the 50mL eluent for every bottle in every group of sample, merge to be concentrated to about 2mL, and it is standby to put into refrigerator cold-storage with the sealing of penicillin bottle.
(2), bacteriostatic experiment
1, extracting solution and extraction sample for the preparation of test agent: every kind of sample takes by weighing 0.1g and is dissolved in and pours in the 1ml sterilized water in the little penicillin bottle that prior sterilization installs filter paper, 65 ℃ of heating of water-bath about 15 minutes, impel sample fully to dissolve, then the penicillin bottle is put into baking oven, keep 45 ℃ (more than 12 hours), till the filter paper oven dry.Contrast is the gentamycin of 4ug/ml.
2, the active preparation that detects for test agent of column chromatography sample segmentation: take out cold preservation and concentrate good merging sample, each sample is got 1mL and is put into the penicillin bottle, put into 12 of the filter papers of the bacterium of having gone out in each bottle, other gets every kind of each 1mL of recovery liquid that merges phase, respectively put into 12 of filter papers, and with merge sample and unify reference numeral, prepare gentamycin (4ug/mL) contrast, with each sample and to put into 45 ℃ of dry for standby of baking oven in the same old way.
3, bacteriostatic experiment method: the strain of preservation activated 12 hours in plating medium after, these 3 kinds of antibacterials are made into 2.0 * 10 respectively in superclean bench
8The clump count of CFU/ml is put into 3 different test tubes, adds the 0.2ml bacteria suspension in each culture dish, smears with the glass bend pipe to make it to be evenly distributed, the filter paper that is soaked with sample is put into the culture dish of writing corresponding contrast numbering, each sample do three parallel, in incubator, cultivate 37 ℃ of temperature.
4, bacteriostatic experiment result:
(1) fungistatic effect of extracting solution and liquid-liquid extraction sample
By antibacterial result as can be known: stock solution (concentrating sample of 80% ethanol extract) and ethyl acetate extraction layer fungistatic effect are best, to staphylococcus aureus, shigella dysenteriae, escherichia coli all have very strong fungistatic effect, n-butyl alcohol extract is to staphylococcus aureus, the fungistatic effect of shigella dysenteriae, these three kinds of strains of escherichia coli is weak slightly than the fungistatic effect of stock solution (concentrating sample of 80% ethanol extract) and acetic acid ethyl ester extract, and petroleum ether extract does not have bacteriostasis.
(2) fungistatic effect of column chromatography segmentation sample
By bacteriostatic experiment as can be known: what fungistatic effect was best in 11 merging mutually is 21-30 number and 31-40 number, next is 61-70 number and 71-80 number, and wherein the 21-30 number inhibition zone size to staphylococcus aureus, escherichia coli, dysentery bacterium is respectively 1.93cm, 1.60cm, 1.97cm; Its maximum inhibition zone is than the also big 0.24cm of the celebrating maximum inhibition zone of big contrast; 31-40 number the inhibition zone size to staphylococcus aureus, escherichia coli, dysentery bacterium is respectively 1.67cm, 1.33cm, 1.53cm; Its maximum inhibition zone is than the little 0.03cm of the celebrating minimum inhibition zone of big contrast; 61-70 number, the fungistatic effect of 71-80 are better, 1-10 number no bacteriostasis; There is not tangible fungistatic effect 11-20 number; Then only staphylococcus aureus is had slight fungistatic effect 81-90 number, the inhibition zone size is 0.87cm; The fungistatic effect of 41-50 number, 51-60 number, 91-100 number, 101-110 number a little less than; 1-10 number no bacteriostasis; There is not tangible fungistatic effect 11-20 number; Then only staphylococcus aureus is had slight fungistatic effect 81-90 number, the lysate of its sample is not to all there is fungistatic effect in the same old way.
Three, the stripped intestinal experimental technique of compound in rubus corchorifolius leaf extraction separation thing, its concrete steps are:
1, the preparation of sample
Accurately each 0.1g of weighing sample is dissolved in the 1ml tyrode's solution, promptly is made into the solution of pastille 0.1g/ml.In addition,, and get 1ml mixed liquor product in contrast so these two kinds of samples uses contain the tyrode's solution of ethanol 23% because of petroleum ether and ethyl acetate are insoluble in water.
2, the preparation of stripped intestinal segment
With rabbit fasting 24h, with mallet fiercely attack rabbit hindbrain oblongata portion make it the stupor, cut the abdominal cavity rapidly open, be the about 8cm of starting point clip duodenum apart from stomach pylorus 5cm, put into 38 ℃ tyrode's solution, be cut into the intestinal segment that is about 2～3cm.Stripped intestinal segment is placed in 38 ℃ the tyrode's solution of ventilation, abundant flush away content, and then it is standby to move in 37～38 ℃ the fresh tyrode's solution ventilation.
3, process and step
Tonotransducer is connected with the input port third channel of Pclab bio signal acquisition processing system, with the calibration of 5g counterweight.Get an intestinal segment, in two sections ligation of intestinal segment, an end is done a short-term ring and is fixed on L pipe below with silk thread, and other end binding links to each other with muscle tone transducer lever.Under (38 ± 0.5) ℃ condition, constantly in tyrode's solution, ventilate, with bio signal acquisition processing system record intestinal segment shrinkage curve.The autorhythmicity of observing intestine in vitro under normal circumstances shrinks, and traces 5min, adds the sample that 100 μ l have prepared then, lays the application of sample labelling simultaneously, with shrink tension (g), contraction frequency (inferior/min) be index, write down 5min.With 38 ℃ of tyrode's solution flushings 3 times, treat to carry out application of sample next time again after intestinal segment recovers normally.Same intestinal segment can use repeatedly continuously.
4, date processing
Handle with SAS statistical analysis software (v6.12), adopt the pairing experimental design, experimental data is with average ± standard error (X ± Es) expression, The data t check between group.10 waveforms are respectively selected in the test of intestine in vitro motion effects before and after application of sample, calculate tension increment and frequency respectively, tension increment=maximum tension-minimum tension, i.e. peak value, tension increment rate of change=(application of sample forward pull-application of sample backward pull) * 100/ application of sample forward pull increment.
5, stripped intestinal experimental result
The intestinal experiment shows by exsomatizing: compound in rubus corchorifolius leaf extract, acetic acid ethyl ester extract all have inhibitory action to the motion of the stripped duodenum of rabbit, jejunum, ileum, colon, the inhibition effect of n-butyl alcohol extract is weak slightly than compound in rubus corchorifolius leaf extract, acetic acid ethyl ester extract, and petroleum ether extract unrestraint effect; The intestinal effect that suppress to exsomatize in the column chromatography for separation sample is best is to merge phase 31-40 number, merge mutually for 71-80 number and 81-90 number merging mutually.Show that Rubus corchorifolius may pass through to suppress the motion of intestinal tube, thereby play anti-diarrhea effect.
Claims (7)
1, the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf is characterized in that, may further comprise the steps:
(1) compound in rubus corchorifolius leaf of gathering is dried in the shade in indoor, pulverize;
(2) add 80% ethanol of 10 times of volumes, under the room temperature lixiviate centrifugal after 48 hours, get its supernatant, add 8 times of volume 80% ethanol again and repeat to extract 1 time;
(3), filter, merging filtrate concentrates;
(4), the solvent of the each middle polarity with 3 times of volumes of the extracting solution that will concentrate, extract as ethyl acetate, n-butyl alcohol or acetone, until extract liquid phase colourless till;
(5), with extract at 50 ℃, be rotated evaporation and concentration under the 0.09Mpa condition to the extractum shape, put-the 25C ultra cold storage freezer in pre-cooling after 1 day, placed the freezer dryer lyophilization 48 hours.
2, the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf according to claim 1 is characterized in that, in the step (3), described concentrating is to be rotated evaporation and concentration under 50 ℃, 0.09Mpa condition.
3, the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf according to claim 1 is characterized in that in the step (4), the solvent of middle polarity is an ethyl acetate.
4, the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf according to claim 1 is characterized in that step (5) lyophilization gained mixture can further carry out chromatography, and method may further comprise the steps:
A, silica gel is dried by the fire activation in 6 hours in 105 ℃ baking oven;
B, wet method dress post, diameter=7cm, height=64cm, volume is: 2978.74cm
2, silica gel 900 grams;
C, sample treatment: take by weighing sample, use the acetic acid ethyl dissolution sample, add silica gel then and stir, in 50 ℃ of oven dry down, standby;
D, employing wet method dress post left standstill after installing 12 hours;
E, use a dry method on a sample, the sample that step c is handled well is packed in the chromatographic column;
F, add eluent, eluting step by step, chloroform and methanol that eluent is followed successively by 3 times of column volumes carry out gradient elution, and flow velocity 2.5ml/min collects eluent.
5, the extracting method of the antibacterial and diarrhea composition of compound in rubus corchorifolius leaf according to claim 4 is characterized in that among the step f, the 1st gradient is pure chloroform eluting, thereafter each gradient is a chloroform: methanol=90: 1,80: 1,65: 1,50: 1,35: 1,20: 1, use the methanol solution eluting at last.
6, a kind of extract of the method for claim 1 preparation.
7, a kind of extract of the method for claim 1 preparation is used to produce the medicine and the diarrhea medicine of antibacterial, the anti-enterokinesia effect of exsomatizing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103766798A (en) * | 2014-01-22 | 2014-05-07 | 浙江师范大学 | Vanilla plant extract and preparation method thereof as well as application in food preservation |
| CN103922935A (en) * | 2014-03-31 | 2014-07-16 | 曹庸 | Method for separating P-hydroxyl ethyl cinnamate from raspberry leaves and application of P-hydroxyl ethyl cinnamate |
-
2007
- 2007-03-07 CN CN 200710034500 patent/CN101015611A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103766798A (en) * | 2014-01-22 | 2014-05-07 | 浙江师范大学 | Vanilla plant extract and preparation method thereof as well as application in food preservation |
| CN103766798B (en) * | 2014-01-22 | 2016-01-20 | 浙江师范大学 | Flowering raspberry plant extracts and preparation method thereof with it for food fresh keeping |
| CN103922935A (en) * | 2014-03-31 | 2014-07-16 | 曹庸 | Method for separating P-hydroxyl ethyl cinnamate from raspberry leaves and application of P-hydroxyl ethyl cinnamate |
| CN103922935B (en) * | 2014-03-31 | 2015-08-05 | 曹庸 | A kind of method being separated p-Coumaric Acid ethyl ester from compound in rubus corchorifolius leaf |
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