CN1330670C - Process for extracting polygonatum polysaccharides, preparing process for medical preparation and use thereof - Google Patents
Process for extracting polygonatum polysaccharides, preparing process for medical preparation and use thereof Download PDFInfo
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Abstract
The present invention relates to an extraction method for polygonatum polysaccharides, a preparation method for medical preparation and the usage thereof. The present invention has the extraction method for the polygonatum polysaccharides that polygonatum crude drug is chopped into small blocks to be added in 4 to 16 times of water, the polygonatum crude drug blocks are boiled and extracted for 1 hour to 4 hours, the extract is filtered, the residue is additionally added in 6 to 12 times of water to be boiled and extracted for 1 hour to 2 hours, the extract is filtered, and the two kinds of extract are combined to carry out centrifugal treatment. Obtained supernatant is decompressed and concentrated to the relative density of 1.08 to 1.25 (at the temperature of 45 to 60 DEG C.), the supernatant is placed to the room temperature to be added in 4 times to 8 times of 95% of ethanol solution to be stirred and settled for 12 hours to 48 hours, the precipitate is taken by separation, the precipitate is added in 0.5 to 2 times cold distilled water to be washed, and the precipitate is dissolved in the distilled water by heating, and 0.5 time to 4 times of 95% of ethanol is added for precipitation to be settled for 12 hours to 48 hours. The precipitate is taken and separated to be washed for three times by 0.5 time to 3 times of 95% of ethanol, and the alcohol lotion is discarded. After the precipitate is frozen and dried for a period of time, the precipitate is dried in a vacuum way to be dry at the temperature of 60 DEG C, the precipitate is taken out to be pulverized and white powder is obtained. The present invention has the preparation method for medical polygonatum polysaccharide preparation that the prepared polygonatum polysaccharide is added with proper auxiliary materials to be prepared into solid preparation classes of tablets, capsules, granules, buccal tablets, chewable tablets and dispersible tablets, and the polygonatum polysaccharide can also be prepared.
Description
Technical field
The present invention relates to extracting method, preparation of pharmaceutical formulations method of a kind of fragrant solomonseal rhizome polyoses and uses thereof.
Background technology
Cardiovascular disorder has become one of main disease that influences China's people ' s health at present, hyperlipidaemia is a kind of common cardiovascular disorder, it is again the important paathogenic factor of atherosclerosis (AS) and coronary heart disease, hypolipidemic can delay to rotate with Partial Inverse the progress of pulse atherosclerosis focus, prevent plaque rupture and improve endothelial function, and obviously reduce the M ﹠ M of cardiovascular diseases.Lipid lowering agent can be divided into by its effect at present: the medicine that 1. mainly reduces blood cholesterol: comprise cholic acid complexing agent, hydroxyl first pentanedioyl acyl coenzyme (HMG-CoA) reductase inhibitor, steroid derivative, sitosterol etc.; 2. blood TG medicine falls: comprise nicotinic acid class, fibric acid, polyunsaturated fatty acid class, mucopolysaccharide and polyose etc.; 3. the medicine that has lipoid peroxidization resistant; 4. other lipid lowering agents.Wherein first kind medicine has peculiar smell or gastrointestinal reaction mostly and takes inconvenience, and costs an arm and a leg, and takes the absorption that can hinder fat-soluble A, D, E, K for a long time, uses not extensive.At present clinically widespread use be statins, belong to the HMG-CoA reductase inhibitor, transfer the blood fat determined curative effect, but prolonged application has hepatotoxicity and other side effects.In addition; nicotinic acid class, mucopolysaccharide and polyose Antiatherosclerosis medicine; as heparin; have effects such as the blood fat of accent, antithrombotic, protection arterial endothelium, inhibition arterial wall smooth muscle cell hyperplasia; but because of its blood coagulation resisting function strong; can cause the hemorrhage untoward reaction of Denging, and transformation period weak point in the body, limited its clinical application.Steroid derivative, sitosterol, fibric acid, polyunsaturated fatty acid class, probucol, vitamin medicaments then lack clinical widely support.Chinese medicine is very promising aspect the treatment of hyperlipidemia, forms unusually from improving lipoprotein metabolism and lipoprotein, and Chinese medicine has the pharmacological action characteristics that chemical synthetic drug does not possess.Hyperlipidaemia belongs to the category of traditional Chinese medicine " phlegm ", and that the rules of treatment have promoting digestion and removing indigestion, invigorating spleen to remove dampness, Wen Yangyi unit, the phlegm that slits is dispelled is turbid, the clearing liver cholagogic, protect that the moonization is turbid, diuresisization is turbid, lead to internal organs and wash turbid, the stagnation resolvation fat etc. of dispelling.The single reducing blood-fat Chinese medicine of having reported has genseng, radix bupleuri, the root of large-flowered skullcap, gynostemma pentaphylla, the root of bidentate achyranthes, garlic, hawthorn etc., and compound hypolipidemic Chinese medicine has dachaihu decoction, Herba Sidae Rhombifoliae soup etc.Gone on the market Chinese medicine and prescribed preparation has SHANZHAJING JIANGZHI PIAN, Xuezhikang etc., but effective constituent is indeterminate, lacks strict contrast and pharmacological research foundation, and mechanism is unclear, has hindered the further investigation of lipid lowering agent.
Radix polygonati officinalis Polygonatum odoratum (Mill.) Druce is the traditional Chinese medicine of China, and the beginning is stated from Shennong's Herbal, classifies as top gradely, and it derives from the dry rhizome of liliaceous plant radix polygonati officinalis.Main steroidal saponin, polysaccharide, flavones and the anthraquinone class chemical ingredients of containing.Nourishing YIN to relieve dryness is arranged, the function that promotes the production of body fluid to quench thirst.Rats gavaged radix polygonati officinalis preserved material, the hyperglycemia that suprarenin, glucose and tetraoxypyrimidine are caused all has restraining effect.Water-soluble part and propyl carbinol part has obvious restraining effect to U-9889 hyperglycemia mouse in the radix polygonati officinalis methanol extract, infers relevant with the liver glycogen glycolysis.Gavage the radix polygonati officinalis decoction for the experimental hyperlipidemia rabbit or can prevent injection liquid 3 to April blood fat to raise and alleviate atherosclerotic plaque formation, triacylglycerol, cholesterol, beta Lipoprotein are descended in the treatment group.Our experimental study shows that first isolating fragrant solomonseal rhizome polyoses can significantly reduce the blood lipid level of experimental hyperlipidemia animal from the radix polygonati officinalis aqueous extract.
Bibliographical information (see the Yu Jing chief editor. modern Chinese herbal medicine research, the Xueyuan Press, 1998) radix polygonati officinalis contains radix polygonati officinalis mucopolysaccharide (Odoratan), and it consists of D-fructose (D-Fructose), D-seminose (D-Mannose), D-glucose (D-Glucose) and D-galacturonic acid (D-Galacluronicacid); Mol ratio is 6: 3: 1: 1.5, other contains radix polygonati officinalis Polylevulosan (Polygonatum-fructan) A, B, C, D, sugar consist of fructose and glucose.
Polysaccharide has different physiological roles, and cytotoxicity is extremely low.Thereby polysaccharide medicine will have more wide prospect as biological response modifier.At present, from natural product or tunning, separate the preparation polysaccharide, the general using polysaccharide is water-soluble, diluted acid, alkali or salts solution, and be insoluble to alcohol, ether, the characteristics of acetone and other organic solvent, with the low polar organic solvent degreasing decoloring element of crude drug, in order to water the solution extraction polysaccharide of main body with residue then, be cold water, hot water, diluted acid, alkali or salts solution extract, and after extracting solution concentrates, use earlier trichoroacetic acid(TCA), Freon 113 method or Sevag method are removed foreign protein, small molecular weight impurity is removed in dialysis then, concentrates the back freeze-drying or with the methyl alcohol or the ethanol of equivalent or several times, the acetone and other organic solvent precipitation promptly obtains the polysaccharide product.Refining ion-exchange, preparation property zone electrophoresis, gel-filtration, ultrafiltration and preparation property high pressure liquid chromatography methods of adopting of polysaccharide more.Above-mentioned polyoses producing method has the following disadvantages: 1, have darker yellow, brown, and be difficult to decolouring; 2, the complicated time of leaching process is long, cost is high, and the large-scale production difficulty is big; 3, in extracting treating process, used organic solvent; 4, contain monose mostly.In a word, above method is difficult for obtaining highly purified polysaccharide.
Simultaneously, the research of radix polygonati officinalis is also had the following disadvantages: 1, more to the Chinese medicine compound prescription research that contains radix polygonati officinalis, few to single radix polygonati officinalis research; Though the report of 2 and blood fat hypoglycemic relevant for radix polygonati officinalis, the activeconstituents or the activeconstituents group that do not understand the radix polygonati officinalis pharmacological action.3, do not see that fragrant solomonseal rhizome polyoses extracts, preparation method's report; 4, radix polygonati officinalis mainly is enriching yin and nourishing kidney in traditional traditional Chinese medical science, in Chinese medicine compound prescription, can be used for hypoglycemic, relevant for the oral report that blood sugar is fallen after rising of radix polygonati officinalis medicinal extract, and the hyperglycemia that medicinal extract causes suprarenin, glucose, tetraoxypyrimidine has inhibiting report (to see the clear an ancient unit of weight of horse, the Wang Shuling chief editor. the clinical practice Chinese materia medica, Jiangxi science tech publishing house, 2002.), but do not see hypoglycemic, the bibliographical information of reducing blood-fat particularly of fragrant solomonseal rhizome polyoses; 5, do not see report about fragrant solomonseal rhizome polyoses composition, molecular weight and pharmacological action relation.The fragrant solomonseal rhizome polyoses molecular weight of the present invention's preparation is 3000～40, and 000 has hypoglycemic and reducing blood lipid, and purity of polysaccharide height (more than 98%).
Summary of the invention
Technical problem to be solved by this invention is the characteristic according to the contained polysaccharide of radix polygonati officinalis, and exploitation is the former extracting method of expecting the fragrant solomonseal rhizome polyoses that is applicable to industrialized production of high purity fragrant solomonseal rhizome polyoses, preparation of pharmaceutical formulations method and uses thereof with the radix polygonati officinalis crude drug.
The technical scheme that solution the technology of the present invention problem is adopted is that the extracting method of this fragrant solomonseal rhizome polyoses has following two kinds:
1. be that the radix polygonati officinalis crude drug is cut into small pieces, place 4～16 times of water gagings, boil and extracted 1-4 hour, extracting liquid filtering, residue add 6～12 times water in addition, boil and extract 1～2 hour, extracting liquid filtering, No. 2 extracting solutions are merged, and centrifugal treating gets the supernatant liquor concentrating under reduced pressure, to relative density 1.08～1.25 (45-60 ℃), be placed to room temperature, add 4～8 times 95% ethanol liquid, stir and left standstill 12-48 hour, separate taking precipitate, add 0.5～2 times of washing of cold distilled water, throw out heating dissolved in distilled water, 95% ethanol sedimentation of 0.5～4 times of amount of adding, left standstill 12～48 hours, divide taking precipitate,, discard pure washing lotion with 95% washing with alcohol of 0.5～3 times of amount three times, after throw out lyophilize for some time, be that 60 ℃ of following vacuum-dryings are to doing taking-up in temperature again, pulverize, get white powder.
2. ultrafiltration process: the extracting solution that gets relative density 1.08～1.25 (45-60 ℃) by 1 legal system is placed room temperature, and adding 95% medical ethanol to determining alcohol is 80%, places 8-16 hour (spending the night).Abandoning supernatant, with the dissolving of pure hypostasis water, be made into 1: 10 (pure hypostasis: suspension water), centrifugal, remove insolubles.Be that 40,000 Hollow Fiber Ultrafiltration post is removed relative molecular weight greater than 40,000 macromolecular substance such as natural gum with the relative molecular weight cutoff value earlier, flow velocity is 20ml/min, and pressure is 0.15 * 10
6Pa; Be that 3000 hollow fiber membrane ultrafiltration devices are removed relative molecular weight less than 3000 small-molecule substance with the relative molecular weight cutoff value again, flow velocity is 15ml/min, and pressure is 0.1 * 10
6Pa.Merge, concentrate relative molecular weight 3000～40,000 fractions, freezing, dry, get fragrant solomonseal rhizome polyoses.
The fragrant solomonseal rhizome polyoses that obtains with method of the present invention is white powder, and is water-soluble, is soluble in hot water especially, is insoluble to the ethanol and the acetone of high density, and the Molish reaction becomes positive with anthrone-strong sulfuric acid response, illustrate to contain polysaccharide in the white powder; Ninhydrin reaction is negative, and no protein is described.Do not contain monose after testing, molecular weight is that 3000～40,000 fragrant solomonseal rhizome polyoses becomes to hive off, and polysaccharide content is more than 98%.
The preparation method of fragrant solomonseal rhizome polyoses pharmaceutical preparation: the above-mentioned fragrant solomonseal rhizome polyoses that makes is added suitable auxiliary material, can be prepared into solid dosages such as tablet, capsule, granule, buccal tablet, chewable tablet, dispersible tablet class, also can be prepared into liquid dosage forms such as oral liquid, mixture class.
The preparation prescription and the technology of pharmaceutical preparation:
Capsule prescription (weight part): 50～300 parts of fragrant solomonseal rhizome polyoses
50～200 parts of micropowder silica gels
50～200 parts in dextrin
Micropowder silica gel, dextrin mixing with recipe quantity join in the polysaccharide of recipe quantity again, mixing, and vacuum-drying (vacuum tightness 0.08-0.09Mpa) is pulverized, mixing, encapsulated (zero～No. 2) get 1000 approximately.Every capsules weighs 0.15～0.7g, contains fragrant solomonseal rhizome polyoses 0.05 g～0.3g.
Tablet formulation (weight part):
50～300 parts of fragrant solomonseal rhizome polyoses
30～60 parts of hypromelloses (K4M)
50～240 parts of lactose
The 3% hypromellose aqueous solution is an amount of
1～5 part of Magnesium Stearate
Every heavy 0.13～0.60g, every contains fragrant solomonseal rhizome polyoses 0.05g～0.3g
Making step comprises in detail:
A, get fragrant solomonseal rhizome polyoses, lactose, hypromellose, Magnesium Stearate respectively and cross 120 mesh sieves, at 105 ℃ of baking 1h, standby.
B, take by weighing main ingredient, lactose, hypromellose by formula rate, thorough mixing is even;
C, add the roughly 3% hypromellose aqueous solution of recipe quantity, thorough mixing is even, the system softwood;
D, 16 mesh sieves are granulated, and 60 ℃ of dryings with the whole grain of order, add the Magnesium Stearate mixing, compressing tablet;
E, quality inspection, packing, signature, promptly.
Purposes of the present invention and service requirements: the present invention has extracted molecular weight from the radix polygonati officinalis medicinal material be 3000～40,000 fragrant solomonseal rhizome polyoses becomes to hive off, purity is more than 98%, above-mentioned polysaccharide is added suitable auxiliary material, solid dosages such as tablet, capsule, granule, buccal tablet, chewable tablet, dispersible tablet can be prepared into, also liquid dosage forms such as oral liquid, mixture can be prepared into.Hypoglycemic, particularly reducing blood-fat that the fragrant solomonseal rhizome polyoses medicament is used for to hyperlipidemia and hyperglycemia patient, can be played hypoglycemic and reducing blood lipid.Above preparation is all with the oral way administration.Usage and consumption: oral, take fragrant solomonseal rhizome polyoses 0.1～0.5g, three times on the one at every turn.
The present invention from radix polygonati officinalis separation and Extraction fragrant solomonseal rhizome polyoses, and it is prepared into oral administration solid or liquid preparation by certain requirement, can reduce blood sugar and the blood fat of hyperglycemia, hyperlipidemia animal, be applicable to diabetic subject and hyperlipemic patients.The present invention has confirmed the above-mentioned beneficial effect of the fragrant solomonseal rhizome polyoses of extraction with experimentation on animals described below.
(1) experimental study of fragrant solomonseal rhizome polyoses effect for reducing fat
1, materials and methods
1.1 laboratory animal
30 of purebred new zealand rabbits, half and half, 5 monthly age of male and female, body weight (2.4 ± 0.2) kg.Divide 5 groups at random: 3 groups of Xuezhikang group, Zocor group, 1 group of radix polygonati officinalis, 2 groups of radix polygonati officinalis and radix polygonati officinalis, 6 every group.
1.2 method
1.2.1 the foundation of hyperlipemia model adds 5% lard and 0.5% cholesterol nutrition purposes, especially for feeding animals with conventional feed, serum lipid concentrations was measured in fasting in 10 hours after 10 days, treat to give lipopenicillinase and experiment medicine after it has significant blood fat to raise, and keep high fat diet to experiment and finish.
1.2.2 medication Xuezhikang group: 300mgkg
-1D
-1Xuezhikang adds the dissolving of 40ml tap water, divides two inferior to feeding after the animal feed; Zocor group: 5mgkg
-1D
-1Zocor is dissolved in the 20ml tap water, once feeds after the animal feed; 1,2,3 groups of radix polygonati officinalis: respectively with 0.2g, 0.4g, 0.4gkg
-1D
-1Fragrant solomonseal rhizome polyoses be dissolved in the 40ml tap water, divide two inferior to feeding after the animal feed.
1.2.3 select 12 animal fasting to measure its blood-sugar content in 10 hours at random before the lipid determination experiment, to test last fasting and checked whole laboratory animal lipids contents in 10 hours, measuring method is the hour method.
1.2.4 all animals is put to death in aorta form and om observation experiment back, get its aorta and carry out general form and observe, and get its part aorta with 10% formaldehyde fixed after the paraffin look bury section, HE dyes and om observation.
1.3 statistical treatment
Experimental data represents that with x ± s statistical study is q check and a plurality of sample χ relatively that compares in twos between paired t-test, a plurality of mean
2Check.
2 results
2.1 animal lipid changes (table 1) after the hypercholesterolemia diet
Can find out that from table 1 after the hypercholesterolemia diet was fed, experimental animal CHO, LDL, Lp (a) all significantly raise, and have formed tangible hyperlipidaemia.
2.2 respectively organize the Blood Lipid (table 2) before and after the laboratory animal medication
Can find out that from table 2 blood fat CHO, LDL, Lp (a) concentration significantly reduce before and after 3 groups of treatments of fragrant solomonseal rhizome polyoses; Except that Lpa) descend, each index does not all have noticeable change before and after 1,2 groups of treatments of radix polygonati officinalis.
2.3 each treated animal Blood Lipid of experiment back is (table 3) relatively
The variation of serum lipid concentrations does not have significant difference between each treatment group of table 3 expression experiment end, illustrates that each group all has reducing blood lipid.
2.4 the situation of atherosclerosis of aorta
Have the visible a small amount of lipid striped of a routine sample aorta to form 2.4.1 general form is observed the Xuezhikang group, surplus laboratory animal there is no tangible lipid striped or atheromatous plaque forms.
2.4.2 om observation part laboratory animal aortic tunica intima sees that foam inner membrance in various degree forms, it the results are shown in Table 4.
Can find out that from table 4 fragrant solomonseal rhizome polyoses group aortic tunica intima foam cell forms and significantly is less than Xuezhikang group, Zocor group (P＜0.05), and be dose-dependence between each group of fragrant solomonseal rhizome polyoses group.
(2) experimental study of fragrant solomonseal rhizome polyoses blood sugar reducing function
1, materials and methods
1.1 laboratory animal
24 of BALB/C mice, at half and half, 2 monthly age of male and female, body weight (25.2 ± 2.4) g divides 4 groups: 1,2 groups of glipizide groups, TANGMAIKANG group, fragrant solomonseal rhizome polyoses, 6 every group at random.
1.2 method
1.2.1 the mouse peritoneal injection urea of setting up of diabetes model is helped rhzomorph 40mgkg
-1D
-1, continuous 5 days.Fasting was cut tail in 6 hours and is measured its blood-sugar content after 10 days, had treated to contrast and test medicine behind the obvious blood sugar increasing.
1.2.2 medication glipizide group: 8mgkg
-1D
-1Glipizide adds physiological saline 0.5ml dissolving, irritates stomach once a day and gives; TANGMAIKANG group: 12.5gkg
-1D
-1TANGMAIKANG adds the 1ml physiological saline solution, divides secondary to irritate stomach and gives, and 1,2 groups of fragrant solomonseal rhizome polyoses are respectively with 0.2g, 1gkg
-1.d
-1Fragrant solomonseal rhizome polyoses dissolve in physiological saline 1ml, divide secondary to irritate stomach and give.
1.2.3 select 3 animal fasting to cut tail after 6 hours at random to measure its blood-sugar content for every group before the detection method experiment, the same method test experience animal blood glucose content behind the injection streptozotocin is tested last fasting and was got the socket of the eye arterial blood in 6 hours and measure blood sugar and HbA
1CAmount.Detection method is respectively glucose oxidase method and chromatography column method.
1.3 statistical treatment
Experimental data represents that with x ± s statistical study is relatively q check in twos between paired t-test and a plurality of mean.
2 results
2.1 change of blood sugar (table 5) behind the laboratory animal injection streptozotocin
Can find out that from table 5 fasting plasma glucose significantly raises behind the experiment mice injection streptozotocin, has formed typical experimental diabetes disease model.
2.2 respectively organize laboratory animal treatment front and back change of blood sugar (table 6)
Can find out that from table 6 after fragrant solomonseal rhizome polyoses and glipizide treatment, FBS has significant differences (p＜0.01), TANGMAIKANG group treatment back FBS decline no significance meaning (P＞0.05).
2.3 experiment back each treated animal FBS and HbA
1CThe variation (table 7) of content
Can find out that from table 7 hypoglycemic effect of each treatment group does not relatively have significance meaning (P＞0.05); But radix polygonati officinalis reduces HbA for 1,2 groups
1cEffect and glipizide group and TANGMAIKANG group meaning (P＜0.01) that highly significant is relatively arranged.
Embodiment
The invention will be further described below in conjunction with embodiment.
Specific embodiment 1
Dry radix polygonati officinalis crude drug 9Kg is cut into small pieces, and places 10 times of water gagings, boils and extracts 1 hour, extracting liquid filtering, the dregs of a decoction add 10 times water in addition, boil and extract 1 hour, extracting liquid filtering merges centrifugal treating with No. 2 extracting solutions, get the supernatant liquor concentrating under reduced pressure,, be placed to room temperature to relative density 1.15 (50 ℃), it is 80% that the ethanol liquid of adding 95% makes it to contain the alcohol amount, stirring was left standstill 12 hours, separated taking precipitate, added 1.5 times of washings of cold distilled water, throw out heating dissolved in distilled water, adding 95% ethanol, to make it to contain alcohol amount be 70%, left standstill 12 hours, divides taking precipitate, with 95% washing with alcohol of 3 times of amounts three times, discard pure washing lotion, the throw out lyophilize is that 60 ℃ of following vacuum-dryings are to doing in temperature again after 12 hours, take out, pulverize, get white powder 340 grams, yield 3.8%, polysaccharide content is 98.6%.
Specific embodiment 2
Dry radix polygonati officinalis crude drug 10Kg is cut into small pieces, place 10 times of water gagings, boil and extracted 1 hour, extracting liquid filtering, the dregs of a decoction add 10 times water in addition, boil and extracted 1 hour, extracting liquid filtering merges No. 2 extracting solutions, centrifugal treating, get the supernatant liquor concentrating under reduced pressure,, be placed to room temperature to relative density 1.15 (50 ℃), it is 80% that the ethanol liquid of adding 95% makes it to contain the alcohol amount, left standstill 12 hours, and separated taking precipitate, add 1.5 times of washings of cold distilled water, with pure hypostasis water dissolving, be made into 1: 10 (pure hypostasis: suspension water), centrifugal, remove insolubles.Be that 40,000 Hollow Fiber Ultrafiltration post is removed relative molecular weight greater than 40,000 macromolecular substance such as natural gum with the relative molecular weight cutoff value earlier, flow velocity is 20ml/min, and pressure is 0.15 * 10
6Pa; Be that 3000 hollow fiber membrane ultrafiltration devices are removed relative molecular weight less than 3000 small-molecule substance with the relative molecular weight cutoff value again, flow velocity is 15ml/min, and pressure is 0.1 * 10
6Pa.Merge, concentrate relative molecular weight 3000～40,000 fractions, freezing, dry, get fragrant solomonseal rhizome polyoses 400 grams, yield 4.0%, polysaccharide content is 98.5%.
Specific embodiment 3
Capsule preparation: fragrant solomonseal rhizome polyoses 50g
Micropowder silica gel 50g
Dextrin 50g
Can make 1000 approximately
Micropowder silica gel, dextrin mixing with recipe quantity join in the polysaccharide of recipe quantity again, mixing, and vacuum-drying (vacuum tightness 0.08-0.09Mpa) is pulverized, mixing, encapsulated (No. 2) get 1000 approximately.The heavy 0.15g of every capsules, every contains fragrant solomonseal rhizome polyoses 0.05g.
Specific embodiment 4
Capsule preparation: fragrant solomonseal rhizome polyoses 300g
Micropowder silica gel 200g
Dextrin 200g
Make 1000 approximately
Micropowder silica gel, dextrin mixing with recipe quantity join in the polysaccharide of recipe quantity again, mixing, and vacuum-drying (vacuum tightness 0.08-0.09Mpa) is pulverized, mixing, encapsulated (No. zero) gets 1000 approximately.The heavy 0.7g of every capsules contains fragrant solomonseal rhizome polyoses 0.3g.
Specific embodiment 5
Tablet formulation, technology:
Fragrant solomonseal rhizome polyoses 50g
Hypromellose (K4M) 30g
Lactose 50g
The 3% hypromellose aqueous solution is an amount of
Magnesium Stearate 1g
Make 1000 altogether, every heavy 0.13g, every contains fragrant solomonseal rhizome polyoses 0.05g.
The detail operations step
1, get fragrant solomonseal rhizome polyoses, lactose, hypromellose, Magnesium Stearate respectively and cross 120 mesh sieves, at 105 ℃ of baking 1h, standby.
2, the prescription ratio takes by weighing main ingredient, lactose, hypromellose, and thorough mixing is even;
3, add the roughly 3% hypromellose aqueous solution of recipe quantity, thorough mixing is even, the system softwood;
4,16 mesh sieves are granulated, and 60 ℃ of dryings with the whole grain of order, add the Magnesium Stearate mixing, compressing tablet;
5, quality inspection, packing, signature, promptly.
Specific embodiment 6
Tablet formulation, technology:
Fragrant solomonseal rhizome polyoses 300g
Hypromellose (K4M) 60g
Lactose 240g
The 3% hypromellose aqueous solution is an amount of
Magnesium Stearate 5g
Make 1000 altogether, every heavy 0.60g, every contains fragrant solomonseal rhizome polyoses 0.3g
The detail operations step
1, get main ingredient, lactose, hypromellose, Magnesium Stearate respectively and cross 120 mesh sieves, at 105 ℃ of baking 1h, standby.
2, take by weighing main ingredient, lactose, hypromellose in the prescription ratio, thorough mixing is even;
3, add the roughly 3% hypromellose aqueous solution of recipe quantity, thorough mixing is even, the system softwood;
4,16 mesh sieves are granulated, and 60 ℃ of dryings with the whole grain of order, add the Magnesium Stearate mixing, compressing tablet;
5, quality inspection, packing, signature, promptly.
Usage and consumption: this product is oral, takes fragrant solomonseal rhizome polyoses 0.1～0.5g at every turn.
Animal lipid changes after table 1 high fat diet
| n | TG(mmol/L) | CHO(mmol/L) | HDL(mmol/L) | LDL(mmol/L) | Lp(a)(mg/L) | |
| Before the high fat diet | 12 | 0.68±0.23 | 1.38±0.27 | 0.63±0.13 | 0.46±0.20 | 163.7±25.3 |
| After the high fat diet | 30 | 0.41±0.12 | 11.32±1.34 * | 0.91±0.14 | 9.18±124 * | 681.5±124.3 * |
*P＜0.01
Blood Lipid before and after each experimental group treatment of table 2
| n | TG | CHO | HDL | LDL | Lp(a) | ||||||
| Before the treatment | After the treatment | Before the treatment | After the treatment | Before the treatment | After the treatment | Before the treatment | After the treatment | Before the treatment | After the treatment | ||
| The Xuezhikang group | 6 | 0.39±0.67 | 0.27±0.07 | 11.45±1.67 | 8.33±5.12 | 0.85±0.14 | 1.14±0.36 | 10.25±2.12 | 7.31±5.25 | 752.4±111.3 | 37.4±10.5 * |
| The Zocor group | 6 | 0.46±0.15 | 0.37±0.10 | 10.73±1.54 | 6.41±3.66 △ | 0.81±0.08 | 0.97±0.22 | 9.87±1.41 | 5.24±3.52 △ | 727.1±125.3 | 477+12.8 * |
| 1 group of radix polygonati officinalis | 6 | 0.48±0.08 | 0.53±0.12 | 11.21±1.21 | 12.4±5.84 | 0.78±0.08 | 0.66±0.21 | 9.48±1.32 | 10.36±5.48 | 613.5±137.3 | 44.7+8.6 * |
| 2 groups of radix polygonati officinalis | 6 | 0.54±0.06 | 0.41±0.23 | 10.92±1.38 | 6.83±3.87 | 0.84±0.14 | 1.46±0.27 | 9.56±1.24 | 5.27±3.13 △ | 652.8±134.8 | 49.6+2.4 * |
| 3 groups of radix polygonati officinalis | 6 | 0.51±0.06 | 0.69±0.31 | 11.71±1.75 | 5.42±1.63 * | 0.87±0.12 | 1.62±0.43 | 10.63±1.48 | 4.51±1.34 * | 640.5±107.8 | 35.8+13.1 * |
It is relatively preceding with treatment,
*P＜0.01,
△P＜0.05
Each treated animal Blood Lipid of table 3 experiment back relatively
| n | TG | CHO | HDL | LDL | Lp(a) | |
| The Xuezhikang group | 6 | 0.27±0.07 | 8.33±5.12 | 1.14±0.36 | 7.31±5.25 | 37.4±10.5 |
| The Zocor group | 6 | 0.37±0.10 | 6.41±3.66 | 0.97±0.22 | 5.24±3.52 | 47.7±12.8 |
| 1 group of radix polygonati officinalis | 6 | 0.53±0.12 | 12.47±5.84 | 0.66±0.21 | 10.36±5.48 | 44.7±8.6 |
| 2 groups of radix polygonati officinalis | 6 | 0.41±0.23 | 6.83±3.87 | 1.46±0.27 | 5.27±3.13 | 49.6±12.4 |
| 3 groups of radix polygonati officinalis | 6 | 0.69±0.31 | 5.42±1.63 | 1.62±0.43 | 4.51±1.34 | 35.8±12.1 |
P all＞0.05
Table 4 aortic tunica intima foam cell forms situation
| Grouping | The test samples number | Add up to | Incidence | |
| There is foam cell to form | The non-foam cell forms | |||
| The Xuezhikang group | 5 | 1 | 6 | 83.3％ |
| The Zocor group | 3 | 3 | 6 | 50％ |
| 1 group of radix polygonati officinalis | 2 | 4 | 6 | 33.3％ |
| 2 groups of radix polygonati officinalis | 1 | 5 | 6 | 16.7％ * |
| 3 groups of radix polygonati officinalis | 1 | 5 | 6 | 16.7％ * |
Compare for 1 group with Xuezhikang group, Zocor group, radix polygonati officinalis,
*P＜0.05
Table 5 experimental diabetic animal change of blood sugar
| n | FBS(mmol/L) | The P value | |
| Before the injection | 12 | 5.83±0.44 | 0.001 |
| After the injection | 24 | 9.14±0.82 |
Change of blood sugar before and after each experimental group medication of table 6
| n | FBS(mmol/L) | The P value | |
| Before the treatment | After the treatment | ||
| Glipizide group 6 | 8.71±0.54 | 6.12±0.93 | 0.001 |
| TANGMAIKANG group 6 | 8.21±0.37 | 7.47±2.03 | 0.587 |
| 1 group 6 of radix polygonati officinalis | 9.22±0.61 | 6.17±0.94 | 0.001 |
| 2 group 6 of radix polygonati officinalis | 8.84±0.46 | 7.37±0.45 | 0.005 |
Respectively organize FBS, HbA after table 7 experiment
1CContent
| n | FBS(mmol/L) | HbA 1C(％) | |
| The glipizide group | 6 | 6.18±0.87 * | 3.08±0.36 |
| The TANGMAIKANG group | 6 | 7.52±2.18 * | 3.23±0.16 |
| 1 group of radix polygonati officinalis | 6 | 6.33±1.12 * | 2.31±0.33 △ |
| 2 groups of radix polygonati officinalis | 6 | 7.25±0.38 * | 1.94±0.27 △ |
*Compare P＞0.05 between each group
△ and glipizide group and TANGMAIKANG group compare, P＜0.01
Claims (6)
1, a kind of extracting method of fragrant solomonseal rhizome polyoses, it is characterized in that the radix polygonati officinalis crude drug is cut into small pieces, place 4～16 times of water gagings, boil and extracted 1～4 hour, extracting liquid filtering, residue adds 6～12 times water in addition, boil and extracted 1～2 hour, extracting liquid filtering merges No. 2 extracting solutions, centrifugal treating, get the supernatant liquor concentrating under reduced pressure, the relative density 1.08～1.25 during to 45～60 ℃ is placed to room temperature, 95% the ethanol liquid that adds 4～8 times, stirring was left standstill 12～48 hours, separated taking precipitate, added 0.5～2 times of washing of cold distilled water, throw out heating dissolved in distilled water, add 95% ethanol sedimentation of 0.5～4 times of amount, left standstill 12～48 hours, divide taking precipitate, with 95% washing with alcohol of 0.5～3 times of amount three times, discarding pure washing lotion, after throw out lyophilize for some time, is that 60 ℃ of following vacuum-dryings are to doing in temperature again, take out, pulverize, get white powder.
2, a kind of extracting method of fragrant solomonseal rhizome polyoses, it is characterized in that the radix polygonati officinalis crude drug is cut into small pieces, place 4～16 times of water gagings, boil and extracted 1～4 hour, extracting liquid filtering, residue add 6～12 times water in addition, boil and extracted 1～2 hour, extracting liquid filtering merges centrifugal treating with No. 2 extracting solutions, get the supernatant liquor concentrating under reduced pressure, the extracting solution of the relative density 1.08～1.25 during to 45-60 ℃ is placed room temperature, and adding 95% medical ethanol to determining alcohol is 80%, places 8-16 hour, abandoning supernatant, with the dissolving of pure hypostasis water, be made into pure hypostasis: the suspension of water=1: 10, centrifugal, remove insolubles, be that 40,000 Hollow Fiber Ultrafiltration post is removed relative molecular weight greater than 40,000 gummy macromolecular substance with the relative molecular weight cutoff value earlier, flow velocity is 20ml/min, and pressure is 0.15 * 10
6Pa: be that 3000 hollow fiber membrane ultrafiltration devices are removed relative molecular weight less than 3000 small-molecule substance with the relative molecular weight cutoff value again, flow velocity is 15ml/min, and pressure is 0.1 * 10
6Pa merges, concentrates relative molecular weight 3000～40,000 fractions, and is freezing, dry, gets fragrant solomonseal rhizome polyoses.
3, the prepared fragrant solomonseal rhizome polyoses of the extracting method of fragrant solomonseal rhizome polyoses according to claim 1 and 2, it is characterized in that being white powder, water-soluble, be insoluble to the ethanol and the acetone of high density, Molish reaction and anthrone one strong sulfuric acid response are positive, illustrate and contain polysaccharide in the white powder: ninhydrin reaction is negative, no protein is described, does not contain monose after testing, molecular weight is 3000～40,000 fragrant solomonseal rhizome polyoses becomes to hive off, and polysaccharide content is more than 98%.
4, a kind of method that adopts the described fragrant solomonseal rhizome polyoses of claim 3 to be used for useful in preparing drug formulations is characterized in that capsule weight part prescription:
50～300 parts of fragrant solomonseal rhizome polyoses
50～200 parts of micropowder silica gels
50～200 parts in dextrin
Micropowder silica gel, dextrin mixing with recipe quantity join in the polysaccharide of recipe quantity again, mixing, and vacuum-drying, vacuum tightness 0.08-0.09Mpa pulverizes, mixing, encapsulated, every capsules weighs 0.15～0.7g, contains fragrant solomonseal rhizome polyoses 0.05g～0.3g.
5, a kind of method that adopts the described fragrant solomonseal rhizome polyoses of claim 3 to be used for useful in preparing drug formulations is characterized in that tablet weight part prescription:
50～300 parts of fragrant solomonseal rhizome polyoses
30～60 parts of hypromelloses
50～240 parts of lactose
The 3% hypromellose aqueous solution is an amount of
1～5 part of Magnesium Stearate
Every heavy 0.13～0.60g, every contains fragrant solomonseal rhizome polyoses 0.05g～0.3g.
6, fragrant solomonseal rhizome polyoses according to claim 5 is used for the method for useful in preparing drug formulations, it is characterized in that the tablet making step comprises:
A, get fragrant solomonseal rhizome polyoses, lactose, hypromellose, Magnesium Stearate respectively and cross 120 mesh sieves, at 105 ℃ of baking 1h, standby;
B, take by weighing fragrant solomonseal rhizome polyoses, lactose, hypromellose by formula rate, thorough mixing is even;
C, add the roughly 3% hypromellose aqueous solution of recipe quantity, thorough mixing is even, the system softwood;
D, 16 mesh sieves are granulated, and 60 ℃ of dryings with the whole grain of order, add the Magnesium Stearate mixing, compressing tablet;
E, quality inspection, packing, signature, promptly.
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7378513B2 (en) * | 2005-07-26 | 2008-05-27 | The Chinese University Of Hong Kong | Isolated proteins from a traditional Chinese medicine Yuzhu and use thereof |
| CN101129400B (en) * | 2006-08-23 | 2010-12-08 | 周亚伟 | Application of fragrant solomonseal rhizome polyoses in preparing medicament for treating coronary disease |
| CN101574475B (en) * | 2009-06-18 | 2012-08-29 | 中南大学 | Polygonatum particle and preparation method thereof |
| CN101579116B (en) * | 2009-06-23 | 2013-04-03 | 宽甸玉竹农副产品有限公司 | Polygonatum odoratum health-care food |
| CN101580551B (en) * | 2009-06-23 | 2011-11-30 | 宽甸玉竹农副产品有限公司 | Method for extracting polygonatum odoratum polysaccharide |
| KR100956278B1 (en) * | 2009-08-03 | 2010-05-10 | 대한약품공업 주식회사 | Composition comprising an extract of herbal combination thereof for preventing and treating diabetes mellitus |
| CN101857644B (en) * | 2010-05-24 | 2012-10-03 | 广西大学 | Alcohol alkali extraction method of aspartic polysaccharide and production process |
| CN102755266A (en) * | 2011-04-26 | 2012-10-31 | 上海家化联合股份有限公司 | Chinese herbal medicine extract, preparation method thereof, and application thereof |
| CN102703444B (en) * | 2012-05-25 | 2013-08-14 | 安徽师范大学 | Radix polygonati officinalis microsatellite DNA (deoxyribonucleic acid) molecular marker |
| CN104069347A (en) * | 2014-06-30 | 2014-10-01 | 吉林化工学院 | Preparation method of polygonatum odoratum total saponin dispersible tablet |
| CN105194319A (en) * | 2015-11-08 | 2015-12-30 | 长沙佰顺生物科技有限公司 | Preparation method of polygonatum odoratum polysaccharide medicine composition |
| CN108359023A (en) * | 2018-03-02 | 2018-08-03 | 北京国康本草物种生物科学技术研究院有限公司 | A kind of extracting method and fragrant solomonseal rhizome polyoses extract of fragrant solomonseal rhizome polyoses |
| CN111345424A (en) * | 2020-04-14 | 2020-06-30 | 吉林农业科技学院 | Polygonatum odoratum polysaccharide solid beverage and purification process |
| CN116675782A (en) * | 2023-05-17 | 2023-09-01 | 宁波大学科学技术学院 | Method for extracting polygonatum odoratum polysaccharide and determination method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220890A (en) * | 1998-10-16 | 1999-06-30 | 朱旭 | Pure natural biological preparation for treating diabetes and preparation method thereof |
| CN1398901A (en) * | 2001-07-19 | 2003-02-26 | 中国科学院成都生物研究所 | Prepn and use of curcuma oligosaccharide sulfate derivative |
-
2004
- 2004-02-02 CN CNB2004100228635A patent/CN1330670C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220890A (en) * | 1998-10-16 | 1999-06-30 | 朱旭 | Pure natural biological preparation for treating diabetes and preparation method thereof |
| CN1398901A (en) * | 2001-07-19 | 2003-02-26 | 中国科学院成都生物研究所 | Prepn and use of curcuma oligosaccharide sulfate derivative |
Non-Patent Citations (4)
| Title |
|---|
| 抗粮尿病中药开发前景展望 陈广耀，中国新药杂志，第9卷第7期 2000 * |
| 生药材调节血糖有效成分的研究 侯昕、徐峰、刘根节、鲍丛荫，辽宁实用糖尿病杂志，第11卷第1期 2003 * |
| 黄精玉竹及其制剂的药理学研究进展 刘玉萍，付桂芳，曹晖，时珍国医国药，第9卷第4期 1998 * |
| 黄精玉竹及其制剂的药理学研究进展 刘玉萍，付桂芳，曹晖，时珍国医国药，第9卷第4期 1998;抗粮尿病中药开发前景展望 陈广耀，中国新药杂志，第9卷第7期 2000;生药材调节血糖有效成分的研究 侯昕、徐峰、刘根节、鲍丛荫，辽宁实用糖尿病杂志，第11卷第1期 2003 * |
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