CN1840539A - Salangane saponin and preparation method and use thereof - Google Patents
Salangane saponin and preparation method and use thereof Download PDFInfo
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- CN1840539A CN1840539A CN 200510042579 CN200510042579A CN1840539A CN 1840539 A CN1840539 A CN 1840539A CN 200510042579 CN200510042579 CN 200510042579 CN 200510042579 A CN200510042579 A CN 200510042579A CN 1840539 A CN1840539 A CN 1840539A
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The disclosed preparation method for Swallow saponins comprises: cutting up fresh material, adding proper solvent to leach and concentrating raffinate; taking column chromatography, eluting with eluent then anotehr eluent; collecting to vacuum condense and dry to obtain the product with hemolysis index more than 5000H.I./g and lots of other curative function.
Description
Technical field:
The present invention relates to Living marine resources development and use and natural active matter screening applied technical field, be to prepare a kind of Salangane saponin and preparation method thereof specifically with Echinodermata, Stelleroidea, Spinulosa, Asterinidae animal petrel, and Salangane saponin eliminate the phlegm, antibechic, new purposes aspect relievining asthma.
Background technology:
Petrel (Asterina pectinifera) is China common zoobenthos in yellow marine site, the Bohai Sea, mainly be distributed in nearshore waters, cigarette prestige fishing ground, middle part, the Bohai Sea and surrounding waters, Chang Mount island, in classification, belong to Echinodermata, Stelleroidea, Spinulosa, Asterinidae can be used as medicine in traditional traditional Chinese medical science, LI Shi-Zhen in Jie portion of listing in Compendium of Material Medica, comparatively detailed description is arranged.Traditional Chinese medical theory is thought, but the petrel suppressing the hyperactive liver and easing the stomach, relieving gastric hyperacidity to alleviate stomachache, among the people in China, once be widely used in diseases such as treatment stomach ulcer, thyromegaly, diarrhoea, otitis media, epilepsy.Modern study shows, petrel contains multiple biologically active substances such as starfish saponin, sterol, amino acid, polypeptide, polysaccharide, lipid, wherein starfish saponin is its distinctive animality steroidal saponin, has multiple physiology and pharmacologically actives such as anticancer, antibiotic, anti-inflammatory and lasting step-down.As one of sociales of marine site, the yellow Bohai Sea of China echinoderms, petrel Shandong coastal waters particularly Jiaodong Peninsula a large amount of distributions are arranged, aboundresources, with low cost, be a kind of good oceanic resources with huge value of exploiting and utilizing, but, because the edible improper food poisoning that causes, reason such as be detrimental to health, this potential source biomolecule resource of petrel fails to be developed fully always, moreover, as the harmful organism that jeopardizes mariculture, petrel is because of being in the top of zoobenthos food chain, happiness food scallop, mollusks such as oyster are to normal sea farming and still a kind of threat of production.Therefore, up to now, a large amount of petrel resources is not only brought into play its due edible and pharmaceutical use, and the mankind's life and production has been produced harm to a certain degree.For fully developing the edible and pharmaceutical use of petrel, patent application people once adopted classical solvent method that Salangane saponin is extracted to have carried out preliminary study before this, classical Salangane saponin extracting method is a solvent method, be petrel is ground into Powdered, with methyl alcohol or extraction using alcohol, extracting solution suction filtration final vacuum is concentrated, pH value is transferred in concentrated solution benzene degreasing after the degreasing, dialyse with dialysis tubing, use water saturated n-butanol extraction again, the butanol extraction liquid vacuum concentration is used acetone precipitation, and is centrifugal, collecting precipitation, vacuum-drying gets Salangane saponin.This method complex process, extracting cycle is long, and solvent consumption is big, the low and saponin(e quality instability of productive rate.
As everyone knows, natural saponin(e has physiology and pharmacologically active widely, is the important raw and processed materials of medicine industry production and research and development.Up to now, though people have found a large amount of saponin(es in plant,, only find that echinodermss such as starfish, sea cucumber contain saponin(e in animal kingdom.The Stelleroidea Animal resources are very abundant, and natural reserves are very big, and are of a great variety, the kind of having reported in the world surpasses 1,000 kind, in China kind more than 100 is arranged also, the starfish that has medicinal exploitation to be worth accounts for larger proportion, but the starfish kind of development and use and research report seldom.Studies show that, the starfish saponin complex structure, separation and refining very difficult, starfish saponin is formed and active the existence between different genera than big-difference, different waters, Various Seasonal, the intravital saponin of different genera starfish distributes, there are specificity in chemical structure and biological activity, aspect biological activity, starfish saponin has anticancer, antithrombotic, antiulcer agent, antiviral, anti-ageing, multiple effects such as establishing-Yang and lasting step-down, for solving cancer, the treatment problem of the major disease of a series of long-term puzzlement human healths such as cardiovascular and cerebrovascular diseases provides a new approach, and its potential development prospect is wide.Comparatively speaking, the research of petrel and Salangane saponin is relative less, petrel (Asterina pectinifera) is as China common Stelleroidea echinoderms in yellow marine site, the Bohai Sea, Shandong coastal waters particularly Jiaodong Peninsula a large amount of distributions are arranged, aboundresources, be the important source of starfish saponin, but developed fully always.The application and development of Salangane saponin can be turned waste into wealth, and gives full play to biological activity and unique curative effect of Salangane saponin, improves the human life quality, benefits the people, benefits society.
Epidemiological study shows that the respiratory system disease sickness rate accounts for 16% of total population morbidity, accounts for the 3rd of urban population general mortality rate.Symptoms such as how many with phlegm respiratory system disease is, cough, asthma.Phlegm is the tracheal secretion of human body, this secretory product can be regulated the temperature and humidity that human body sucks air under the normal circumstances, and swallow and get rid of along with breathing by unconscious, but can be by expectoration, any coughing talked the phlegm action and meaned that all there are abnormal conditions in respiratory system, if the tracheae inner product has the phlegm of the expectoration treated, just may cause infection by tracheae, simultaneously, the phlegm heavy-gravity very normally that remains expectoration, therefore, expectoration usually makes the patient agonize, for the ease of expectoration, avoid infection, alleviate the patient suffering, use expectorant clinically usually; Asthma is the common disease of long-term hazards human health, and according to World Health Organization's statistics, at present, asthmatic patient accounts for 3.4% of the world's 6,000,000,000 populations; China has 2,500 ten thousand asthmatic patients at least, and wherein about 1,000 ten thousand is children.Asthma have the characteristics difficult, that expense is high of curing, asthmatic patient per capita year medical expense up to 2000 yuan, the treatment rate with 10% and 1,500 ten thousand person-times of calculating, national asthmatic patient year medical expense can reach 3,000,000,000 yuans.At present, if there is certain limitation in chemical synthetic drugs such as treating asthma drug main tracheae diastole agent, corticosteroid hormone in curative effect and secure context, doctor, trouble both sides press for clear and definite, safe and reliable, the stay-in-grade novel suppressing panting calming medicine of curative effect.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and provide a kind of Salangane saponin and preparation method thereof and eliminate the phlegm, antibechic, application aspect relievining asthma.Mainly solved the Salangane saponin complicated process of preparation, saponin(e quality instability and Salangane saponin eliminate the phlegm, antibechic, functional evaluation aspect relievining asthma and the problem of petrel resources development and utilization.
In order to achieve the above object, the present invention is achieved in that Salangane saponin, and its special character is that it is to be made by following method, with the petrel be raw material through pulverizing, add an amount of solvent lixiviate, with the extracting solution concentrating under reduced pressure, get concentrated solution, the concentrated solution that above-mentioned steps is obtained carries out column chromatography, remove impurity with the elutriant wash-out after, again with another elutriant wash-out, collect this elutriant, concentrating under reduced pressure gets Salangane saponin after the drying, the haemolytic index of Salangane saponin is greater than 5000H.I./g.
The present invention also provides the preparation method of Salangane saponin, it is to be made by following method, is raw material with the petrel through pulverizing, and adds an amount of solvent lixiviate, with the extracting solution concentrating under reduced pressure, concentrated solution, the concentrated solution that above-mentioned steps is obtained carries out column chromatography, remove impurity with the elutriant wash-out after, again with another elutriant wash-out, collect this elutriant, concentrating under reduced pressure gets Salangane saponin after the drying.
A kind of preferred version of the preparation method of Salangane saponin of the present invention is that described pulverizing is that fresh petrel is adopted any one mode in direct rubbing, freezing and pulverizing, the crushed after being dried.
The preparation method's of Salangane saponin of the present invention another kind of preferred version is, described solvent is any one in the aqueous methanol of aqueous ethanol, different concns of water, ethanol, methyl alcohol, different concns.
The preparation method's of Salangane saponin of the present invention another kind of preferred version is, any one in the aqueous methanol of the described aqueous ethanol that is extracted as the distilled water that adds 3-20 times of petrel powder weight, ethanol, methyl alcohol, different concns, different concns carries out room temperature and extracted 12-144 hour; Extract in the aqueous methanol of the aqueous ethanol also can be the distilled water that adds 3-20 times of petrel powder weight, ethanol, methyl alcohol, different concns, different concns any one and heat and extracted 1-10 hour, Heating temperature is 50-80 ℃.
A kind of preferred version of the preparation method of Salangane saponin of the present invention is, described column chromatography is a macroporous resin column chromatography, and applied sample amount is the 1%-100% of macroporous resin weight, and applied sample amount refers to the weight of the concentrated solution of enrichment step.
The preparation method's of Salangane saponin of the present invention another kind of preferred version is, described column chromatography is a silica gel column chromatography, and applied sample amount is the 1%-30% of silica gel weight, and applied sample amount refers to the weight of the concentrated solution of enrichment step.
A kind of preferred version of the preparation method of Salangane saponin of the present invention is, adopt the wash-out of macroporous resin column chromatography, be that first distilled water with 2-10 times of macroporous resin adsorption volume carries out wash-out, the control elution speed be 1-3 times of macroporous resin adsorption volume/hour, use 20%, 50%, 80% ethanol wash-out successively again, elution requirement is identical with usefulness distilled water wash-out, and collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, vacuum-drying or lyophilize get Salangane saponin.
A kind of preferred version of the preparation method of Salangane saponin of the present invention is, adopt the wash-out of silica gel column chromatography, be to carry out gradient elution with ethyl acetate, ethanol respectively, elution volume is 3-10 times of silicagel column adsorption volume, elution speed be 1-3 times of silica gel adsorption volume/hour, collect above-mentioned ethanol eluate, concentrating under reduced pressure, vacuum-drying or lyophilize get Salangane saponin.
The invention provides Salangane saponin have in preparation eliminate the phlegm, antibechic, the functional food of antiasthmatic effect and the application aspect the medicine.
The hemolytic activity of the Salangane saponin that the present invention makes is: haemolytic index is greater than 5000H.I./g.
(hemolytic index H.I.) is meant the inverse that can make the consoluet minimum saponin(e concentration of red corpuscle in the blood under certain condition to haemolytic index.The mensuration of haemolytic index, on the one hand, the saponin(e solution that usually needs to prepare a series of different concns experimentizes, and " complete hemolysis " or " beginning haemolysis " this index and so-called " concentration of the rarest saponin(e solution " then are difficult to get rid of fully the interference of operator's subjective factor.The present invention adopts the spectrophotometric determination absorption curve, and the method for observing maximum light absorption value judges whether to reach complete hemolysis.This method measure haemolytic index have easy, fast, advantage accurately.Its calculation formula is as follows:
V---the total amount of liquid (mL) in vitro;
P---the concentration of saponin(e solution (is represented with percentage ratio, %);
S---the minimum volume (mL) that makes the red corpuscle in the test tube dissolve required saponin(e solution fully.
Be pairing saponin(e liquor capacity when wavelength 540nm place light absorption value reaches maximum and substantially no longer changes in this experiment.
The mensuration of Salangane saponin hemolytic activity:
The biological activity of Salangane saponin is with every gram sample haemolytic index (H.I./g) expression, and the concrete measuring method of haemolytic index is as follows:
(1) takes by weighing sodium-chlor 9g, be settled to 1000mL, be made into 0.9% physiological saline with dissolved in distilled water and dilution;
(2) extract rat artery blood, the anti-freezing of adding citric acid sodium, use then centrifugal behind the physiological saline mixing (2500rpm, 5min), repeated washing 2-3 time gets final product to the supernatant liquor redfree;
(3) remove supernatant liquor after, according to sedimentary erythrocytic volume, be made into 2% red cell suspension with physiological saline;
(4) accurately take by weighing sample to be checked after the 0.1g drying,, promptly be made into the sample solution of 0.1% (1mg/mL) with being settled to 100mL behind a small amount of physiological saline solution;
(5) get 26 of clean small test tubes, add the 0-2.5mL sample solution successively according to the incremental change of 0.1mL, every then pipe is added the physiological saline of respective amount respectively, makes the volume of each test tube all reach 2.5mL.Add the red cell suspension of 2.5mL while vibrating, make each pipe volume reach 5mL.Add back jog 15min,, put that (20-25 ℃) leaves standstill 12hr under the room temperature so that it mixes (shake and avoid producing foam in the process) fully;
(6) with the centrifugal 5min of 2500rpm, careful absorption supernatant liquor is measured its light absorption value at the 540nm place (hereinafter to be referred as A540).Reference solution is the supernatant of suspension after centrifugal of 2.5mL physiological saline and 2.5mL red cell suspension;
(7) volume with saponin(e solution is an X-coordinate, and A540 is the ordinate zou mapping, promptly gets saponin(e and causes hemolytic dosage-effect (A540) curve, finds out the minimum volume S (mL) that A540 reaches the required saponin(e solution of maximum value.Can try to achieve the haemolytic index of sample according to following calculation formula.
Salangane saponin of the present invention has following drug effect, (the used Salangane saponin of following experiment is the preparation of embodiment 1 method):
1, the phlegm-dispelling functions of Salangane saponin:
Experimental principle: adopt the mouse phenolsulfonphthalein to drain method, utilize phenolsulfonphthalein mouse peritoneal injection rear section, measure the excretion of airway of mice phenolsulfonphthalein, to judge the Salangane saponin phlegm-dispelling functions from air flue excretory characteristics.
1.1 experiment material:
JIZHI TANGJIANG, Tai Ji group Fuling Pharmaceutical Factory, lot number 0312101;
Voltoide, Xi Bohua Pharmaceutical Co, lot number 030602;
Salangane saponin is made into the solution of different concns with 0.5% Xylo-Mucine;
Phenolsulfonphthalein, Shanghai reagent three factories, it is standby to be mixed with 2.5% concentration with physiological saline;
Sodium hydroxide, Yantai three and chemical reagent company limited are made into 1mol/L with deionized water.
Laboratory apparatus: BIO-RAD Model 550, USA;
Laboratory animal: cleaning level Kunming mouse, male and female have concurrently, body weight 18-22g;
1.2 experimental technique
1.2.1 the phenolsulfonphthalein typical curve practice: phenolsulfonphthalein is diluted to i.e. 12.5,6.25,3.13,1.56, the 0.78 μ g/ml of 5 concentration with physiological saline, respectively pipette 1ml with sample injector, drip 0.1ml sodium hydroxide (1mol/L) respectively, the vibration mixing, survey the 570nm A of place value with BIO-RAD Model 550, ask straight-line regression.
1.2.2 the phenol red excretion of tracheae: get 50 of mouse, be divided into 5 groups at random: the blank group, JIZHI TANGJIANG group (0.15ml/10g), Salangane saponin 1 (20mg/kg) group, Salangane saponin 2 (40mg/kg) group and ammonium chloride group (1000mg/kg), all the other respectively organize equal gastric infusion 2 days except that the ammonium chloride group, the 3rd day together with the administration of ammonium chloride group after 1 hour, mouse peritoneal is injected 2.5% phenol red normal saline solution 0.2ml/10g mouse, mouse is put to death in dislocation after 30 minutes, separate tracheae, cut off again along the little edge of thyroid cartilage and to prolong 0.5cm to proximal part and cut off, put into the 1ml normal saline solution, vibrated 10 minutes, add 1mol/L sodium hydroxide 0.1ml, measure content with BIO-RAD Model 550 at 570nm behind the mixing.
1.3 result and discussion
1.3.1 phenolsulfonphthalein typical curve:
Typical curve:
| Phenolsulfonphthalein concentration g/ml) | 0.78 | 1.56 | 3.13 | 6.25 | 12.5 |
| The OD value | 0.097 | 0.183 | 0.351 | 0.651 | 1.125 |
1.3.2 the phenol red excretion result of tracheae:
Table 1 Salangane saponin is to the influence of mouse phlegm-dispelling functions (n=10, x ± s)
| Group | Dosage | Number of animals (only) | Phenolsulfonphthalein OD value | Tracheae phenolsulfonphthalein excretion (μ g/ml) |
| 2 groups of ammonium chloride groups of 1 group of Salangane saponin of blank group JIZHI TANGJIANG group Salangane saponin | —— 15ml/kg 20mg/kg 40mg/kg 1000mg/kg | 10 10 10 10 10 | 0.184±0.012 0.206±0.017 * 0.242±0.012 * 0.297±0.015 * 0.220±0.020 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Table 1 is the result show, Salangane saponin 20mg/kg dosage group increases mouse tracheae phenolsulfonphthalein excretion amount, has stronger phlegm-dispelling functions; Starfish saponin 40mg/kg dosage group can make mouse tracheae phenolsulfonphthalein excretion amount obviously increase, and has significant phlegm-dispelling functions.
2, the antitussive effect of Salangane saponin
This experiment is that with Salangane saponin strong aqua to be caused the influence of coughing mouse be model, estimates the antitussive effect of Salangane saponin.
Experimental principle:
Ammoniacal liquor pungent aerosols such as (25%-28%) sucks in the respiratory tract, stimulates the susceptor under the airway epithelial, can cause cough.Measure the variation of mouse cough number of times in mouse administration front and back cough latent period and the 2min, observe Salangane saponin and strong aqua is caused the influence of coughing mouse.
2.1 experiment material
Codeine phosphate, Qinghai Pharmaceutic Plant, lot number 960605;
Salangane saponin is made into the solution of different concns with 0.5% Xylo-Mucine;
Ammoniacal liquor, Yantai three and chemical reagent company limited, lot number 030618;
Laboratory apparatus: ultrasonic atomizer, PARIMASTER;
Laboratory animal: cleaning level Kunming mouse, male and female have concurrently, body weight 18-22g;
2.2 experimental technique
Get 40 of mouse, be divided into 4 groups at random: the blank group, codeine phosphate group (5mg/kg), Salangane saponin 1 (20mg/kg) group and Salangane saponin 2 (40mg/kg) group, each organizes continuous gastric infusion 2 days, respectively organized administration after 60 minutes on the 3rd day, mouse is put into 500ml bell glass (each 1), connect the PARIMASTER ultrasonic atomizer, constant voltage sprays into ammoniacal liquor (25%-28%) in the bell glass uniformly, spraying 5S observes and writes down cough latent period (s) (beginning to the required time of cough occurring from spraying ammoniacal liquor) and the interior cough of the 2min number of times of mouse then.Respectively be subjected to the difference of reagent group and blank group with the T check.
2.3 result and discussion
Table 2 Salangane saponin causes strong aqua and coughs mouse influence (n=10, x ± s)
| Group | Dosage | Cause and cough latent period (s) | Cause and cough number of times | ||
| Before the administration | After the administration | Before the administration | After the administration | ||
| 2 groups of 1 group of Salangane saponins of blank group codeine phosphate group Salangane saponin | —— 5mg/kg 20mg/kg 40mg/kg | 24.5±3.4 24.0±3.7 24.8±3.0 25.0±2.6 | 25.1±2.8 28.4±2.3 28.0±3.0 31.8±5.0 | 21.7±3.1 21.0±3.6 21.8±3.7 25.0±2.7 | 20.3±6.4 13.1±5.9 * 17.0±4.1 * 13.6±3.4 * |
*P＜0.05,
*Compare with the blank group P＜0.01.
Table 2 is the result show, Salangane saponin (20mg/kg) can prolong to cause coughs latent period, reduces cough number of times in the 2min (comparing P＜0.05 with the NS group); Salangane saponin (40mg/kg) obviously prolongs to cause coughs latent period, reduce cough number of times in the 2min (with the NS group relatively, P＜0.01), illustrate that Salangane saponin (40mg/kg) has stronger antitussive effect.
3, the antiasthmatic effect of Salangane saponin;
This experiment is with Salangane saponin histamine to be caused the model that act as of breathing heavily cavy, and estimates the antiasthmatic effect of Salangane saponin.
Experimental principle:
Many medicines can cause bronchospasm, suffocate when giving cavy with aeroponics, thereby cause twitching and fall.This animal model can be used for observing the bronchial smooth muscle relexation of medicine.It is histamine and vagusstoff that medicine is breathed heavily in the most frequently used drawing at present.This experiment is used to observe Salangane saponin and histamine is caused the effect of breathing heavily cavy.
3.1 experiment material
The aminophylline sheet, guilin pharmacy factory, lot number 030201
Salangane saponin is made into the solution of different concns with 0.5% Xylo-Mucine;
Histamine,
Laboratory apparatus: ultrasonic atomizer, PARIMASTER;
Laboratory animal: cavy, male and female have concurrently, body weight 200-250g;
3.2 experimental technique:
50 of cavys are measured it one by one and draw and breathe heavily latent period, and it is standby with interior cavy to get its latent period 150s.
Choose 40 of cavys, body weight 200-250g, be divided into 4 groups at random, every group 10, the blank group, aminophylline group (125mg/kg), Salangane saponin 1 (20mg/kg) group and Salangane saponin 2 (40mg/kg) group, each organizes continuous gastric infusion 2 days, respectively organizes administration after 60 minutes on the 3rd day, and cavy is put into glass cover (the about 4L of volume) one by one, spray into 1g/L histamine and 20g/L vagusstoff equivalent mixed liquor 20S with the PARIMASTER ultrasonic atomizer with constant voltage, keep a close eye on the reaction of cavy then, observation begins to breathe heavily latent period to drawing of panting property convulsions generation from the spray medicine, respectively is subjected to the difference of reagent group and blank group with the T check.
3.3 result and discussion
Table 3 Salangane saponin draws cavy breathes heavily preclinical influence (n=10, x ± s)
| Group | Dosage | Draw and breathe heavily latent period (s) |
| 2 groups of 1 group of Salangane saponins of blank group aminophylline group Salangane saponin | —— 125mg/kg 20mg/kg 40mg/kg | 54.1±14.9 83.3±12.1 ** 69.4±8.0 * 80.3±13.9 ** |
*P＜0.05,
*Compare with the blank group P＜0.01.
Table 3 is the result show, Salangane saponin (20mg/kg) can prolong to draw to be breathed heavily latent period (comparing P＜0.05 with the NS group); Salangane saponin (40mg/kg) obviously prolongs to draw to be breathed heavily latent period (comparing P＜0.01 with the NS group); The antiasthmatic effect that Salangane saponin (40mg/kg) is described is stronger.
According to above experiment as can be known, Salangane saponin of the present invention eliminates the phlegm in treatment, antibechic, good effect is arranged aspect relievining asthma, and it can add vehicle that pharmaceutics allows and make other various formulations such as oral liquid except that injection, tablet, capsule, aerosol.Because the big multipotency of the aqueous solution of saponin(e destroys red corpuscle and has hemolytic action, if its aqueous solution is injected in the vein, toxicity is very big, and the low concentration aqueous solution just can produce haemolysis.The aqueous solution intramuscularly of saponin(e easily causes tissue necrosis, and oral then do not have a hemolytic action.Saponin(e can haemolysis be to generate insoluble molecular complex because most saponin(es can combine with cholesterol.When the saponin(e aqueous solution contacts with red corpuscle, combine with cholesterol on the erythrocyte membrane, generate water-fast mixture precipitation, destroyed the normal infiltration of erythrocyte, make osmotic pressure increase and generation disintegration in the cell, thereby cause haemolysis, thereby can not make injection.
Compared with the prior art Salangane saponin of the present invention and its production and use has outstanding substantive distinguishing features and marked improvement, and 1, preparation technology is simple, extracting cycle is short, and solvent consumption is little, productive rate height and steady quality; 2, experimentation on animals confirm Salangane saponin have clear and definite eliminate the phlegm, antibechic, antiasthmatic effect, can be used for the manufacturing of the functional food and the medical supplies of correlation function, the application and development of Salangane saponin, can turn waste into wealth, give full play to biological activity and unique curative effect of Salangane saponin, improve the human life quality, benefit the people, benefit society; 3, Salangane saponin preparation technology improve and Salangane saponin eliminates the phlegm, this EXPLOITATION AND UTILIZATION OF MARINE LIVING RESOURCES of petrel that is found to be of antibechic, antiasthmatic effect provides a new approach.
Embodiment:
In order to understand better and to implement, describe the present invention in detail below in conjunction with embodiment, it is emphasized that following examples are for more detailed description implementation method of the present invention, rather than in order to limit the present invention.
Embodiment 1, fresh petrel is put shady and cool drying to be located air-dry, be ground into 20-40 order particle with medicinal herb grinder, take by weighing 10Kg petrel dry powder, 80% ethanol that adds 200Kg, room temperature is extracted 144h, with extracting solution at 0.08MPa, concentrating under reduced pressure under 50 ℃ of conditions, get the 10L concentrated solution, above-mentioned concentrated solution is adsorbed with AB-8 macroporous resin column on the speed of 5L/h, and the macroporous resin consumption is 10Kg, and adsorption volume is 5000ml after measured, after absorption is finished, earlier with 50L distilled water macroporous resin column is carried out wash-out, the control elution speed is 15L/h, uses 50L 20% ethanol again, 50L 50% ethanol, 50L 80% ethanol is wash-out successively, the control elution speed is 5L/h, collect above-mentioned 50% ethanol eluate, 0.08MPa, concentrating under reduced pressure under 50 ℃ of conditions, 0.08MPa, vacuum-drying under 50 ℃ of conditions gets Salangane saponin, and it is 6800H.I./g that hemolytic activity detects the haemolytic index that shows Salangane saponin.
Embodiment 2, fresh petrel 10Kg is directly rubbed into 20-60 order particle with mincer, 80% ethanol that adds 100L, room temperature was extracted 72 hours, collect extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 2L under 50 ℃ of conditions, above-mentioned concentrated solution is adsorbed with NKA macroporous resin column on the speed of 1L/h, the macroporous resin consumption is 2Kg, and adsorption volume is 800ml after measured, after absorption is finished, earlier macroporous resin column is carried out wash-out with 5L distilled water, the control elution speed is 1.5L/h, uses 20% of 8L more respectively, 50%, 80% ethanol is wash-out successively, and elution requirement is with identical with the distilled water wash-out, collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, lyophilize gets Salangane saponin.
Embodiment 3,20-60 order particle is rubbed into mincer in the freezing back of fresh petrel 10Kg, the methyl alcohol that adds 30L, room temperature was extracted 12 hours, collect extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 2L under 50 ℃ of conditions, above-mentioned concentrated solution is adsorbed with NKA-9 macroporous resin column on the speed of 1L/h, the macroporous resin consumption is 2Kg, and adsorption volume is 1000ml after measured, after absorption is finished, earlier macroporous resin column is carried out wash-out with 4L distilled water, the control elution speed is 1L/h, uses 20% of 4L more respectively, 50%, 80% ethanol is wash-out successively, and elution requirement is with identical with the distilled water wash-out, collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, lyophilize gets Salangane saponin.
Embodiment 4, the freezing back of fresh petrel 10Kg is rubbed, add the distilled water of 30Kg, stir under 80 ℃ of conditions and extract 10h, collect extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 5L under 80 ℃ of conditions, above-mentioned concentrated solution is adsorbed with DA-101 macroporous resin column on the speed of 6L/h, the macroporous resin consumption is 5Kg, and adsorption volume is 2L after measured, after absorption is finished, earlier carry out wash-out with 20L distilled water, the control elution speed is 6L/h, uses 20% of 20L more respectively, 50%, 80% ethanol is wash-out successively, and the control elution speed is 4L/h, collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, lyophilize gets Salangane saponin.
Embodiment 5, fresh petrel 10Kg crushed after being dried is become 20-60 order particle, add 50Kg 60% ethanol, 5h is extracted in heating under 50 ℃ of conditions, collect extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 5L under 50 ℃ of conditions, above-mentioned concentrated solution is adsorbed with AB-8 macroporous resin column on the speed of 1L/h, the macroporous resin consumption is 2Kg, and adsorption volume is 1L after measured, after absorption is finished, earlier carry out wash-out with 10L distilled water, the control elution speed is 3L/h, uses 20% of 10L more respectively, 50%, 80% ethanol is wash-out successively, and the control elution speed is 1L/h, collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, lyophilize gets Salangane saponin.
Embodiment 6, fresh petrel 10Kg crushed after being dried is become 20-60 order particle, add 200Kg 80% ethanol, 1h is extracted in heating under 50 ℃ of conditions, collects extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 0.5L under 50 ℃ of conditions, above-mentioned concentrated solution is mixed sample with 0.2Kg 60-100 order column chromatography silica gel, volatilize 100-200 order silicagel column on the solvent, the silica gel consumption is 1.5Kg, and adsorption volume is 1.5L after measured, respectively with the 10L ethyl acetate, 15L ethanol carries out gradient elution, collect ethanol eluate, 0.08MPa, concentrating under reduced pressure under 50 ℃ of conditions, 0.08MPa, vacuum-drying under 50 ℃ of conditions gets Salangane saponin.
Embodiment 7, fresh petrel 10Kg is directly rubbed, add 10Kg methyl alcohol, 10h is extracted in heating under 50 ℃ of conditions, collects extracting solution, 0.08MPa, with the extracting solution concentrating under reduced pressure, get concentrated solution 0.8L under 50 ℃ of conditions, above-mentioned concentrated solution is mixed sample with 0.2Kg 60-100 order column chromatography silica gel, volatilize 100-200 order silicagel column on the solvent, the silica gel consumption is 2Kg, and adsorption volume is 2L after measured, respectively with the 10L ethyl acetate, 20L ethanol carries out gradient elution, collect ethanol eluate, 0.08MPa, concentrating under reduced pressure under 50 ℃ of conditions, 0.08MPa, vacuum-drying under 50 ℃ of conditions gets Salangane saponin.
Make Salangane saponin with the inventive method and make spendable preparation by following examples method.
Embodiment 1, the Salangane saponin oral liquid
10 milliliters of Salangane saponin 0.5 gram distilled water
After the Salangane saponin dissolving according to a conventional method through can, step such as seal and produce and promptly get the Salangane saponin oral liquid.
Embodiment 2,1000 prescriptions of Salangane saponin hard capsule
Salangane saponin 100 gram starch 100 grams
Salangane saponin, starch mixing promptly get the Salangane saponin hard capsule in 1000 hard capsule of packing into.
Embodiment 3, the Salangane saponin tablet
Salangane saponin 500 gram starch 25 gram Magnesium Stearates 5 grams
Salangane saponin, starch, Magnesium Stearate compressing tablet, dressing according to a conventional method promptly get the Salangane saponin tablet.
In addition, in spirit of the present invention, can carry out various changes and modifications to given embodiment, the alternate embodiments by those of skill in the art recognize also is included in the scope of claim.
Claims (10)
1, Salangane saponin is characterized in that it is to be made by following method, is raw material with the petrel through pulverizing, and adds an amount of solvent lixiviate, with the extracting solution concentrating under reduced pressure, concentrated solution; The concentrated solution that above-mentioned steps is obtained carries out column chromatography, remove impurity with the elutriant wash-out after, with another elutriant wash-out, collect this elutriant again, concentrating under reduced pressure, after the drying Salangane saponin, the haemolytic index of Salangane saponin is greater than 5000H.I./g.
2, the preparation method of the described Salangane saponin of claim 1, it is characterized in that it is to be made by following method, is raw material with the petrel through pulverizing, and adds an amount of solvent lixiviate, with the extracting solution concentrating under reduced pressure, concentrated solution, the concentrated solution that above-mentioned steps is obtained carries out column chromatography, remove impurity with the elutriant wash-out after, again with another elutriant wash-out, collect elutriant, concentrating under reduced pressure gets Salangane saponin after the drying.
3, the preparation method of Salangane saponin according to claim 2 is characterized in that described pulverizing is that fresh petrel is adopted any one mode in direct rubbing, freezing and pulverizing, the crushed after being dried.
4, the preparation method of Salangane saponin according to claim 2 is characterized in that described solvent is any one in the aqueous methanol of aqueous ethanol, different concns of water, ethanol, methyl alcohol, different concns.
5, the preparation method of Salangane saponin according to claim 2 is characterized in that in the aqueous methanol of the described aqueous ethanol that is extracted as the distilled water that adds 3-20 times of petrel powder weight, ethanol, methyl alcohol, different concns, different concns any one carries out room temperature and extracted 12-144 hour; Extract in the aqueous methanol of the aqueous ethanol also can be the distilled water that adds 3-20 times of petrel powder weight, ethanol, methyl alcohol, different concns, different concns any one and heat and extracted 1-10 hour, Heating temperature is 50-80 ℃.
6, the preparation method of Salangane saponin according to claim 2 is characterized in that described column chromatography is a macroporous resin column chromatography, and applied sample amount is the 1%-100% of macroporous resin weight, and applied sample amount refers to the weight of the concentrated solution of enrichment step.
7, the preparation method of Salangane saponin according to claim 2 is characterized in that described column chromatography is a silica gel column chromatography, and applied sample amount is the 1%-30% of silica gel weight, and applied sample amount refers to the weight of the concentrated solution of enrichment step.
8, the preparation method of Salangane saponin according to claim 6, it is characterized in that described wash-out, be that first distilled water with 2-10 times of macroporous resin adsorption volume carries out wash-out, the control elution speed be 1-3 times of macroporous resin adsorption volume/hour, use 20%, 50%, 80% ethanol wash-out successively again, elution requirement is identical with usefulness distilled water wash-out, and collect above-mentioned 50% ethanol eluate, concentrating under reduced pressure, vacuum-drying or lyophilize get Salangane saponin.
9, the preparation method of Salangane saponin according to claim 7, it is characterized in that described wash-out, carry out gradient elution with ethyl acetate, ethanol respectively, elution volume is 3-10 times of silicagel column adsorption volume, elution speed be 1-3 times of silica gel adsorption volume/hour, collect above-mentioned ethanol eluate, concentrating under reduced pressure, vacuum-drying or lyophilize get Salangane saponin.
10, the described Salangane saponin of claim 1 have in preparation eliminate the phlegm, antibechic, the functional food of antiasthmatic effect and the application aspect the medicine.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335201A (en) * | 2011-09-30 | 2012-02-01 | 宁波餐之皇食品有限公司 | Extract method of asteroid saponins |
| CN102973606A (en) * | 2012-12-31 | 2013-03-20 | 中国科学院南海海洋研究所 | Sea moth extract as well as preparation method thereof and application thereof |
| CN104434983A (en) * | 2014-12-10 | 2015-03-25 | 沈阳药科大学 | Extraction method of asterina pectinifera extract and application of extract in preparing anti-tumor medicines |
| CN113940427A (en) * | 2021-11-01 | 2022-01-18 | 大连海洋大学 | Preparation process of asterias amurensis Lutken saponin with antioxidant activity |
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2005
- 2005-03-29 CN CN 200510042579 patent/CN1840539A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335201A (en) * | 2011-09-30 | 2012-02-01 | 宁波餐之皇食品有限公司 | Extract method of asteroid saponins |
| CN102335201B (en) * | 2011-09-30 | 2013-06-12 | 宁波餐之皇食品有限公司 | Extract method of asteroid saponins |
| CN102973606A (en) * | 2012-12-31 | 2013-03-20 | 中国科学院南海海洋研究所 | Sea moth extract as well as preparation method thereof and application thereof |
| CN104434983A (en) * | 2014-12-10 | 2015-03-25 | 沈阳药科大学 | Extraction method of asterina pectinifera extract and application of extract in preparing anti-tumor medicines |
| CN113940427A (en) * | 2021-11-01 | 2022-01-18 | 大连海洋大学 | Preparation process of asterias amurensis Lutken saponin with antioxidant activity |
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