CN105218695A - A kind of lycium ruthenicum polysaccharide extract and preparation method thereof - Google Patents
A kind of lycium ruthenicum polysaccharide extract and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of lycium ruthenicum polysaccharide extract and preparation method thereof, the lycium ruthenicum polysaccharide obtained by preparation methods such as cleaning, drying, fragmentation, removal of impurities, extraction, decolouring, removing protein, concentrated, purifying has the strong kidney of enriching yin, improving eyesight nourishing liver, lipopenicillinase, anti-cancer, anti-ageing effect of waiting for a long time, simultaneously the simple easy handling of lycium ruthenicum polysaccharide preparation method technique of the present invention, yield is higher, quality is good, be conducive to realizing industrialized process for processing.
Description
Technical field
The present invention relates to plant milk extract field, be specially a kind of lycium ruthenicum polysaccharide extract and preparation method thereof with the strong kidney of enriching yin, improving eyesight nourishing liver, lipopenicillinase, anti-cancer, anti-ageing function of waiting for a long time.
Background technology
Black fruit lyceum is the dry fruit of Solanaceae Lycium black fruit lyceum (LyciumRuthenicumMurr), and in the middle part of Gansu, China Jiuquan, East of Qinghai Province, Xinjiang, all there is fragmentary distribution on West Inner Mongolia, the ground such as Ningxia and Tibet.Its grows the barren hill and sandy beach, riverbed that cannot survive the mankind, and have extremely strong vitality, the wild black fruit lyceum of To Golmud of Qinghai is described as grassland " soft gold ".But along with the mankind are to the exploitation of the Nature, the living space of black fruit lyceum is less and less, create the high-grade excellent tonic product of ecosystem of this rare preciousness of black fruit lyceum.Its taste is sweet, property is put down, the strong kidney of tool, nourishing liver, improving eyesight, stomach invigorating, benefit brain, the anti-ageing and function of stimulating the menstrual flow.Uygur medicine is dizzy with its treatment, blurring of vision, positive ruffian of suffering from a deficiency of the kidney, the disease such as in poor health.Tibetan medicine is used for the treatment of heart-heat syndrome, heart trouble, reduction cholesterol, excited cerebral nerve, strengthens immunologic function, anti-curing cancers, anti-ageing, beautifying face and moistering lotion, menoxenia, menelipsis etc. and drug effect is remarkable, the also disease such as conventional black fruit lyceum fruit and the treatment of root skin urethral calculus, tinea scabies, gingival hemorrhage.The various nutritive ingredients such as black fruit lyceum fruit rich in proteins, fat, carbohydrate, total free aminoacids, organic acid, mineral substance, trace element, alkaloid, vitamins C, B1, B2, calcium, magnesium, copper, zinc, manganese, iron, lead, nickel, cadmium, cobalt, chromium, potassium, sodium.Black fruit lyceum with red matrimony vine is the same can tonifying kidney and benefiting sperm; anthocyanidin (Anthocyanosides) in black fruit lyceum has effect of scavenging free radicals; also cancer cells can be allowed to spread smoothly, protect the cell of more health to avoid being corroded by cancer cells whereby.Similarly be the mechanism of causing a disease of mammary cancer be like this, therefore take anthocyanidin and good restraining effect is had for the development of mammary cancer.Black fruit lyceum also can prevent and treat diabetes, and there is obvious antifatigue, protect the liver, antitumor, dredging vascellum, step-down and protection Cardiovascular System.Particularly lycium ruthenicum polysaccharide content is high, has good health value and pharmaceutical use.
Polysaccharide (polysaccharide), also known as saccharan, is the polymkeric substance be connected to form with sugar former times key by the monose of more than 20.It is the most colourful member in composition macromolecular compound family.Polysaccharide comes from the natural macromolecular material in higher plant, animal cell membrane, microbial cell wall, is the important composition composition of all Living organisms and the necessary structured material that sustains life.First people are the energy derive it regarded as in food to the understanding of sugar.To the research of polysaccharide, in the forties in 20th century the earliest, but it causes the very big attention of people to be in the sixties as broad immune promotor, through the development in more than 40 years, people create new understanding to the important living matter of this class of polysaccharide, this subject is become in current life science and studies one of most active field.It is found that carbohydrate is not only as energy matter or structured material in organism, the more important thing is that it take part in the various activities of cell in life science, there is diversified biological function.Therefore the research of sugar is progressively active, and wherein, number molecular weight is more than several thousand, and the research with the active polysaccharide of very strong biological activity receives increasing attention.The physiologically active of these active polysaccharides, chemical structure and structure activity relationship become the forward position of polysaccharide researches, and make great progress.Scientific worker finds that polysaccharide compound has the biological activity of the aspect such as antitumor, anti-ageing, anti-infective, hypoglycemic blood fat and treatment acquired immune deficiency syndrome (AIDS) gradually.In recent years, find that again the sugar chain of polysaccharide is controlling division and the differentiation of cell, regulate the growth of cell and old and feeble aspect to play decisive role, polysaccharide demonstrates application prospect more and more widely gradually.
Lycium ruthenicum polysaccharide is the principle active component of black fruit lyceum, and pharmacology and clinical study are very noticeable.Lycium ruthenicum polysaccharide has pharmacotoxicological effect widely, can promote hematopoiesis, reducing blood-fat, protect the liver and the effect improving eyesight nourishing liver such as anticancer, lipopenicillinase, anti-cancer and anti-ageing function of waiting for a long time.
The extracting method that currently available technology prepares polysaccharide conventional has: Hot water extraction, acidleach formulation, alkali method and enzyme process.These methods all also exist many problems, such as destroy polysaccharide structures, Polyose extraction inefficiency, and extraction time, process that is long and that extract was complicated etc.
Summary of the invention
The object of this invention is to provide the extracting method of the lycium ruthenicum polysaccharide that a kind of loss of effective components is few, quality is high, extraction cost is low.The lycium ruthenicum polysaccharide that the method extracts possesses and has the strong kidney of enriching yin, improving eyesight nourishing liver, lipopenicillinase, anti-cancer and anti-ageing function of waiting for a long time.
Concrete, extracting method of the present invention is as follows:
An extracting method for lycium ruthenicum polysaccharide, is characterized in that, adopts black fruit lyceum, after fragmentation, adopts circumfluence method to extract.
An extracting method for lycium ruthenicum polysaccharide, is characterized in that comprising the following steps:
1, clear up: black fruit lyceum is screened out silt, clean with clear water;
2, dry: by the black fruit lyceum cryodrying 10 ~ 24h at 5 ~ 30 DEG C cleaned up;
3, broken: black fruit lyceum step 2 obtained carries out micronizing, and obtaining particle size range is 1 ~ 75 μm of powder;
4, removal of impurities: under powder step 3 obtained is placed in curved continuous box girder 450 ~ 650W power, extracts 15 ~ 30min by aether backflow, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 15 ~ 30min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5, extract: the water dregs of a decoction III obtained being added 10 ~ 15 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1 ~ 2h, ultrasonic power 0.5 ~ 1.5KW, and Extracting temperature 40 ~ 60 °, obtains filtrate I;
6, decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7, removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8, concentrated: put by filtrate II I in microwave vacuum dryer, the span of Microwave Power Density and vacuum tightness is (2 ~ 8w/g) and (0.02 ~ 0.08Mpa), obtains lycium ruthenicum polysaccharide concentrated extracting solution;
9, purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the different in flow rate loading of 0.3 ~ 0.9ml/min, with the ethanol of 80% concentration with the different in flow rate wash-out of 0.4 ~ 1.5ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
In the first step, if carefully do not clean, the silt dead leaf etc. of doping can affect extraction efficiency.
In second step, under low temperature, carry out drying, the preservation of polysaccharide effective constituent can be ensured.
In 3rd step, superfine communication technique can make powder diameter little (generally below 15 μm) and be evenly distributed, ball degree and homogeneity obviously improve, loose density and specific surface significantly improve, plant cell wall breaking rate is high, dissolving and the release of the effective constituent (particularly refractory components) in black fruit lyceum are accelerated, and the dissolution rate of effective constituent is accelerated.
In 5th step, combine advantage that is ultrasonic and refluxing extraction, extraction efficiency is higher.
In addition, for the consideration of controlling cost, the cryodrying in each step of the present invention, backflow, ultrasonic, etc. are all proven technique, simple to operate, easy left-hand seat.But compared with prior art, simplify leaching process and but obtain higher yield and the good product of quality.
Preferably, a kind of extracting method of lycium ruthenicum polysaccharide, is characterized in that comprising the following steps:
1, clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2, dry: by the black fruit lyceum cryodrying 10h at 20 DEG C cleaned up;
3, broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 30 μm of powder;
4, removal of impurities: powder step 3 obtained extracts 20min by aether backflow under being placed in curved continuous box girder 450W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 20min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5, extract: the water dregs of a decoction III obtained being added 10 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1h, ultrasonic power 0.5KW, and Extracting temperature 40 °, obtains filtrate I;
6, decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7, removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8, concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 8w/g and 0.02Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution;
9, purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.3ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 1.5ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
Preferably, a kind of extracting method of lycium ruthenicum polysaccharide, is characterized in that comprising the following steps:
1, clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2, dry: by the black fruit lyceum cryodrying 10h at 30 DEG C cleaned up;
3, broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 35 μm of powder;
4, removal of impurities: powder step 3 obtained extracts 25min by aether backflow under being placed in curved continuous box girder 500W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 25min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5, extract: the water dregs of a decoction III obtained being added 9 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1.5h, ultrasonic power 1.5KW, and Extracting temperature 50 °, obtains filtrate I;
6, decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7, removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8, concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 5w/g and 0.05Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution;
9, purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.5ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 1.0ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
Embodiment
The present invention is further detailed explanation by the following examples, but protection scope of the present invention is not by any restriction of specific embodiment, but be limited by claim.
Embodiment 1: the preparation of lycium ruthenicum polysaccharide
1, clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2, dry: by the black fruit lyceum cryodrying 10h at 30 DEG C cleaned up;
3, broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 35 μm of powder;
4, removal of impurities: powder step 3 obtained extracts 25min by aether backflow under being placed in curved continuous box girder 500W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 25min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5, extract: the water dregs of a decoction III obtained being added 9 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1.5h, ultrasonic power 1.5KW, and Extracting temperature 50 °, obtains filtrate I;
6, decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7, removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8, concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 5w/g and 0.05Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution.
9, purifying: will through pretreated macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.5ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 1.0ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
The extraction yield of the lycium ruthenicum polysaccharide that embodiment 1 is extracted is 3.89% far above 1.37% of prior art, therefore the present invention for lycium ruthenicum polysaccharide extract extraction have good beneficial effect.
Embodiment 2: the preparation of lycium ruthenicum polysaccharide
1, clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2, dry: by the black fruit lyceum cryodrying 10h at 20 DEG C cleaned up;
3, broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 30 μm of powder;
4, removal of impurities: powder step 3 obtained extracts 20min by aether backflow under being placed in curved continuous box girder 450W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 20min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent.
5, extract: the water dregs of a decoction III obtained being added 10 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1h, ultrasonic power 0.5KW, and Extracting temperature 40 °, obtains filtrate I.
6, decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II.
7, removing protein: filtrate II Sevage method removing protein is obtained filtrate II I.
8, concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 8w/g and 0.02Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution.
9, purifying: will through pretreated macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.8ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 0.8ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
The extraction yield of the lycium ruthenicum polysaccharide that embodiment 2 is extracted is 3.78% far above 1.37% of prior art, therefore the present invention for lycium ruthenicum polysaccharide extract extraction have good beneficial effect.
Embodiment 3
Phenol-sulfuric acid and colorimetric method measures the polysaccharide content of different macroporous resin type purifying
The preparation of 1 phenol liquid
Get phenol 200g, add 0.2g aluminium flake and the distillation of 0.1g sodium bicarbonate, collect 182 DEG C of cuts.Take 5g, adding distil water is settled to 100mL and dissolves, mix and be transferred in brown bottle, puts in refrigerator for subsequent use.
The preparation of 2 standardized solution
Accurately take 105 DEG C of analytical pure glucose 100.00mg of drying to constant weight, with distilled water dissolve and in 100mL volumetric flask constant volume, obtain the standardized solution of 1mg/mL, pipette 2mL, 4mL, 6mL, 8mL, 10mL respectively, in 100mL volumetric flask, constant volume obtains the standard sugar solution of 20 μ g/mL, 40 μ g/mL, 60 μ g/mL, 80 μ g/mL, 100 μ g/mL.
The drafting of 3 typical curves
Get 2mL standard sugar solution add massfraction be 5% phenol solution 1mL shake up, add rapidly the 5mL vitriol oil, shake up, after room temperature places 5min, boiling water bath 15min, is cooled to room temperature rapidly, carries out length scanning with ultraviolet-visual spectrometer, record 485nm place for maximum absorption band, blank replaces sugar soln with distilled water.Obtain typical curve equation.
4 Different Extraction Method polysaccharide determinations (except resin types all adopts embodiment 1 method to prepare)
Experimental result is as shown in table 1, and the D101 macroporous resin that the present invention adopts can significantly improve the extraction yield of lycium ruthenicum polysaccharide.
The contrast of the total polysaccharides content that table 1 Different Extraction Method obtains
| Extracting method | H-30 | XDA-1 macroporous adsorbent resin | XDA-7 equal hole decolorizing resin | D101 macroporous resin |
| Absorbancy | 0.254 | 0.242 | 0.343 | 0.461 |
| Account for raw medicinal herbs content (%) | 1.49 | 1.29 | 1.61 | 3.78 |
Polysaccharide content under phenol-sulfuric acid and colorimetric method mensuration Different Extraction Method
The preparation of 1 phenol liquid
Get phenol 200g, add 0.2g aluminium flake and the distillation of 0.1g sodium bicarbonate, collect 182 DEG C of cuts.Take 5g, adding distil water is settled to 100mL and dissolves, mix and be transferred in brown bottle, puts in refrigerator for subsequent use.
The preparation of 2 standardized solution
Accurately take 105 DEG C of analytical pure glucose 100.00mg of drying to constant weight, with distilled water dissolve and in 100mL volumetric flask constant volume, obtain the standardized solution of 1mgmL ~ 1, pipette 2mL, 4mL, 6mL, 8mL, 10mL respectively, in 100mL volumetric flask, constant volume obtains the standard sugar solution of 20 μ g/mL, 40 μ g/mL, 60 μ g/mL, 80 μ g/mL, 100 μ g/mL.
The drafting of 3 typical curves
Get 2mL standard sugar solution add massfraction be 5% phenol solution 1mL shake up, add rapidly the 5mL vitriol oil, shake up, after room temperature places 5min, boiling water bath 15min, is cooled to room temperature rapidly, carries out length scanning with ultraviolet-visual spectrometer, record 485nm place for maximum absorption band, blank replaces sugar soln with distilled water.Obtain typical curve equation.
4 different extract lower polysaccharide determination (all adopting embodiment 1 method to prepare except extracting method)
Experimental result: as shown in table 2, adopts the present invention greatly can improve the extraction efficiency of lycium ruthenicum polysaccharide,
The content balance of the total polysaccharides that table 2 Different Extraction Method obtains
| Extracting method | Supersound extraction | Refluxing extraction | Microwave extraction | (the present invention) |
| Absorbancy | 0.249 | 0.243 | 0.350 | 0.459 |
| Account for raw medicinal herbs content (%) | 1.55 | 1.37 | 1.70 | 3.89 |
Embodiment 4
Lycium ruthenicum polysaccharide is to the research of experimental mouse aging oxidation-resistance
The foundation of 1 subacute aging animal model and grouping
Healthy kunming mice 96, body weight 25 ± 5g, female (♀) male (♂) half and half, after feeding normal diet adaptation, weigh on an empty stomach, eyeground vein is taken a blood sample, in survey serum after MDA, be divided into 6 groups at random, often organize 16, ♀ ♂ half and half. body weight, the horizontal no significant difference of serum MDA between group.Grouping and administrations as follows:
1 group: Normal group (Normalgroup): physiological saline+distilled water
2 groups: aging model group (Controlgroup): D (+) semi-lactosi 200mg/kg+ distilled water
3 groups: positive controls (positivegroup): D (+) semi-lactosi 200mg/kg+ vitamin e1 00mg/kg
4 groups: polysaccharide experimental group (preparation of embodiment 1 method) (Testgroup): D (+) semi-lactosi 200mg/kg+ lycium ruthenicum polysaccharide extract 400mg/kg
Above-mentioned lycium ruthenicum polysaccharide extract is all adopt the prepared acquisition of embodiment 1 method.
2 medications
Lycium ruthenicum polysaccharide to be dissolved in distilled water respectively at morning every day to mouse stomach, gavage amount controls in 4ml/d, continuous 8 weeks.Simultaneously abdominal injection D (+) semi-lactosi 200mg/kg, vitamin-E is dissolved in salad oil and is made into the respective concentration same time and gives gavage 8 weeks.
The mensuration of MDA, SOD, GSH-PX in 3 blood plasma
After eight weeks, mouse fasting be can't help water 12 hours, get blood 1.5 ~ 2.0ml from eyeground vein clump, prepare blood plasma, carry out the mensuration of indices.When getting blood, with anticoagulant heparin, 4 DEG C, centrifugal 15 minutes of 3000r/min, getting supernatant liquor, to put into refrigerator to be measured.In blood plasma, MDA, SOD, GSH-PX content all illustrates by test kit and adopts enzymatic assays.
The mensuration of 4 liver homogenate preparations and wherein MDA, SOD, GSH-PX
Administration 8 weeks rear mouse are got blood collare spondyloschisis from eyeground vein clump and put to death, win mouse liver 0.5g, put into mill, add 4.5ml physiological saline, the liver homogenate of 10% is made in grinding, vibration, placement is spent the night, 6 DEG C, centrifugal 30 minutes of 3000r/min, get supernatant liquor, adopt MDA, SOD, GSH-PX to measure the content of MDA, SOD, GSH-PX in kit measurement liver.Protein quantification measures by test kit explanation biuret method.
Experimental result
1 lycium ruthenicum polysaccharide is on the impact of subacute aging model mice serum and Liver MDA
Serum MDA determination data shows: model group serum lipid peroxide MDA content has than Normal group and obviously increases (P<0.001), positive controls and lycium ruthenicum polysaccharide group all can obviously reduce serum MDA level, more all have significant (P<0.01) with model group; Hepatic tissue MDA determination data shows: have than Normal group MDA after the modeling of model group Liver MDA and obviously increase (P<0.001), and positive controls, all obviously can reduce hepatic tissue MDA level to lycium barbarum polysaccharide group, with the more equal significance of model group (P<0.01), (table 3).
Table 3 lycium ruthenicum polysaccharide is on the impact (nmol/ml, X ± s) of subacute aging model mice serum and Liver MDA
| N | Serum MDA | Hepatic tissue MDA | |
| Normal group | 15 | 3.85±0.33 | 2.28±0.25 |
| Aging model group | 14 | 6.79±0.88*** | 4.17±0.35*** |
| Positive controls | 13 | 4.63±0.61△△△ | 3.56±0.35△△△ |
| Polysaccharide control group | 16 | 4.80±0.49△△△ | 2.68±0.14△△△ |
Note: compare with Normal group: * * * is P<0.001, * * be P<0.01, * is P<0.05; Compare with hyperlipidemia model group: △ is P<0.05, △ △ is P<0.01; Compare with positive controls: ## is P<0.01
2 lycium ruthenicum polysaccharide groups affect determination of serum SOD data presentation to subacute aging model mouse superoxide-dismutase (SOD) content: have obvious reduction (P<0.001) than Normal group after the modeling of model group SOD in serum content, positive controls and polysaccharide group be energy obviously increasing serum SOD activity level all, more all has remarkable statistical significance (P<0.05) with model group; Hepatic tissue SOD determination data shows: have obvious reduction (P<0.001) than Normal group SOD after the modeling of model group hepatic tissue SOD content, and positive controls, polysaccharide amount group all obviously can raise hepatic tissue SOD activity level, with the more equal significance of model group (P<0.01), (table 4)
Table 4 lycium ruthenicum polysaccharide is on the impact (nmol/ml, X ± s) of subacute aging model mouse superoxide-dismutase (SOD) content
| N | SOD in serum | Hepatic tissue SOD | |
| Normal group | 15 | 330.45±55.67 | 266.38±33.71 |
| Aging model group | 14 | 260.03±58.03*** | 131.59±16.57*** |
| Positive controls | 13 | 310.55±31.98△△ | 193.7±19.74*△△ |
| Polysaccharide control group | 16 | 320.02±32.86△△ | 251.11±26.70△△ |
Note: compare with Normal group: * * * is P<0.001, * * be P<0.01, △ be P<0.05, △ △ is P<0.01; Compare with positive controls: ## is P<0.01
3 lycium ruthenicum polysaccharide are on the impact of subacute aging model mice serum and hepatic tissue GSH-PX content
Serum GSH-PX determination data shows: have obvious reduction (P<0.001) than Normal group after the modeling of model group serum GSH-PX content, positive controls and lycium ruthenicum polysaccharide group be energy obviously increasing serum GSH-PX level all, with the more equal significance of model group (P<0.001); Hepatic tissue GSH-PX determination data shows: have obvious reduction (P<0.001) than Normal group GSH-PX after the modeling of model group hepatic tissue GSH-PX content, and positive controls amount group all obviously can raise hepatic tissue GSH-PX activity level, with the more equal significance of model group (P<0.001), (table 5).
Table 5 lycium ruthenicum polysaccharide is on the impact (nmol/ml, X ± s) of subacute aging model mice serum and hepatic tissue GSH-PX content
| N | Serum GSH-PX | Hepatic tissue GSH-PX | |
| Normal group | 15 | 680.1±113.08 | 342.24±45.6 |
| Aging model group | 14 | 510.54±36.30*** | 266.69±69.69*** |
| Positive controls | 13 | 645.05±47.52△△△ | 257.49±23.22*△△ |
| Polysaccharide control group | 16 | 697.58±63.95** | 263.09±18.52* |
Note: compare with Normal group: * * * is P<0.001, * * be P<0.01, * is P<0.05; Compare with hyperlipidemia model group: △ is P<0.05, △ △ is P<0.01; Compare with positive controls: ## is P<0.01
The foregoing is only preferred embodiment of the present invention, and be not used to limit substantial technological context of the present invention, substantial technological content of the present invention is broadly defined in the right of application, any technology entities that other people complete or method, if with application right define identical, also or a kind of change of equivalence, be all covered by being regarded as among this right.
Claims (6)
1. an extracting method for lycium ruthenicum polysaccharide, is characterized in that, adopts black fruit lyceum, after fragmentation, adopts circumfluence method to extract.
2. a preparation method for lycium ruthenicum polysaccharide extract, is characterized in that comprising the following steps:
1) clear up: black fruit lyceum is screened out silt, clean with clear water;
2) dry: by the black fruit lyceum cryodrying 10 ~ 24h at 5 ~ 30 DEG C cleaned up;
3) broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 1 ~ 75 μm of powder;
4) removal of impurities: under powder step 3 obtained is placed in curved continuous box girder 450 ~ 650W power, extracts 15 ~ 30min by aether backflow, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 15 ~ 30min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5) extract: the water dregs of a decoction III obtained being added 10 ~ 15 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1 ~ 2h, ultrasonic power 0.5 ~ 1.5KW, and Extracting temperature 40 ~ 60 °, obtains filtrate I;
6) decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7) removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8) concentrated: put by filtrate II I in microwave vacuum dryer, the span of Microwave Power Density and vacuum tightness is (2 ~ 8w/g) and (0.02 ~ 0.08Mpa), obtains lycium ruthenicum polysaccharide concentrated extracting solution;
9) purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the different in flow rate loading of 0.3 ~ 0.9ml/min, with the ethanol of 80% concentration with the different in flow rate wash-out of 0.4 ~ 1.5ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
3. the preparation method of lycium ruthenicum polysaccharide extract according to claim 2, its feature, the preparation method of described lycium ruthenicum polysaccharide extract is:
1) clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2) dry: by the black fruit lyceum cryodrying 10h at 20 DEG C cleaned up;
3) broken: carry out micronizing to black fruit lyceum prepared by step 2, obtaining particle size range is 30 μm of powder;
4) removal of impurities: what step 3 obtained be placed in curved continuous box girder 450W power by powder under, extract 20min by aether backflow, obtain dregs of a decoction I; Dregs of a decoction I aether backflow extracts 20min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5) extract: the water dregs of a decoction III obtained being added 10 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1h, ultrasonic power 0.5KW, and Extracting temperature 40 °, obtains filtrate I;
6) decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7) removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8) concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 8w/g and 0.02Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution;
9) purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.3ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 1.5ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
4. the preparation method of lycium ruthenicum polysaccharide extract according to claim 2, its feature, the preparation method of described lycium ruthenicum polysaccharide extract is:
1) clear up: black fruit lyceum 1kg is screened out silt, clean with clear water;
2) dry: by the black fruit lyceum cryodrying 10h at 30 DEG C cleaned up;
3) broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 35 μm of powder;
4) removal of impurities: powder step 3 obtained extracts 25min by aether backflow under being placed in curved continuous box girder 500W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 25min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5) extract: the water dregs of a decoction III obtained being added 9 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1.5h, ultrasonic power 1.5KW, and Extracting temperature 50 °, obtains filtrate I;
6) decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7) removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8) concentrated: filtrate II I to be put in microwave vacuum dryer, Microwave Power Density 5w/g and 0.05Mpa, obtain lycium ruthenicum polysaccharide concentrated extracting solution;
9) purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the flow velocity loading of 0.5ml/min, with the ethanol of 80% concentration with the flow velocity wash-out of 1.0ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
5. the preparation method of lycium ruthenicum polysaccharide extract according to claim 2, its feature, the preparation method of described lycium ruthenicum polysaccharide extract is:
1) clear up: black fruit lyceum is screened out silt, clean with clear water;
2) dry: by the black fruit lyceum cryodrying 15h at 20 DEG C cleaned up;
3) broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 1 ~ 75 μm of powder;
4) removal of impurities: powder step 3 obtained extracts 20min by aether backflow under being placed in curved continuous box girder 500W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 25min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5) extract: the water dregs of a decoction III obtained being added 14 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1.5h, ultrasonic power 1.0KW, and Extracting temperature 50 °, obtains filtrate I;
6) decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7) removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8) concentrated: put by filtrate II I in microwave vacuum dryer, the span of Microwave Power Density and vacuum tightness is (5w/g) and (0.05Mpa), obtains lycium ruthenicum polysaccharide concentrated extracting solution;
9) purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the different in flow rate loading of 0.6ml/min, with the ethanol of 80% concentration with the different in flow rate wash-out of 0.9ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
6. have a lycium ruthenicum polysaccharide extract for improving eyesight nourishing liver, lipopenicillinase, anti-cancer, anti-aging effects, its special type is, described lycium ruthenicum polysaccharide method for preparing extractive comprises the following steps:
1) clear up: black fruit lyceum is screened out silt, clean with clear water;
2) dry: by the black fruit lyceum cryodrying 23h at 20 DEG C cleaned up;
3) broken: carry out micronizing to the black fruit lyceum that step 2 obtains, obtaining particle size range is 1 ~ 75 μm of powder;
4) removal of impurities: powder step 3 obtained extracts 28min by aether backflow under being placed in curved continuous box girder 600W power, obtains dregs of a decoction I; Dregs of a decoction I aether backflow extracts 28min; Obtain dregs of a decoction II; Dregs of a decoction II alcohol reflux is obtained dregs of a decoction III; Dregs of a decoction III volatilizes solvent;
5) extract: the water dregs of a decoction III obtained being added 12 times, is placed in ultrasonic refluxing extraction system, ultrasonic refluxing extraction 1 ~ 2h, ultrasonic power 1.2KW, and Extracting temperature 45 °, obtains filtrate I;
6) decolour: in filtrate I, add 0.1% gac, decolouring, obtains filtrate II;
7) removing protein: filtrate II Sevage method removing protein is obtained filtrate II I;
8) concentrated: put by filtrate II I in microwave vacuum dryer, the span of Microwave Power Density and vacuum tightness is (7w/g) and (0.07Mpa), obtains lycium ruthenicum polysaccharide concentrated extracting solution;
9) purifying: will through pretreated D101 macroporous resin wet method dress post, get above-mentioned crude extract in the different in flow rate loading of 0.8ml/min, with the ethanol of 80% concentration with the different in flow rate wash-out of 1.4ml/min, elutriant is merged, concentrated, be drying to obtain the more much higher sugar extract of purity.
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| CN111777695A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院上海药物研究所 | Lycium ruthenicum polysaccharide LRP3-S1, and preparation method and application thereof |
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| CN111925457A (en) * | 2020-07-24 | 2020-11-13 | 哈工大机器人南昌智能制造研究院 | Method for preparing high-purity lycium ruthenicum polysaccharide |
| CN113397206A (en) * | 2021-07-09 | 2021-09-17 | 广西中烟工业有限责任公司 | Preparation method of carboxymethylated momordica grosvenori polysaccharide and application of carboxymethylated momordica grosvenori polysaccharide in tobacco humectant |
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