CN104086664A - Gracilaria lemaneiformis polysaccharide extract and preparation method and application thereof - Google Patents
Gracilaria lemaneiformis polysaccharide extract and preparation method and application thereof Download PDFInfo
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- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 41
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000605 extraction Methods 0.000 title claims description 12
- 241000206611 Gracilariopsis lemaneiformis Species 0.000 title 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the field of deep processing of asparagus and discloses an asparagus polysaccharide extract and a preparation method and application thereof. The polysaccharide extract of the asparagus is prepared by drying and crushing the asparagus, and then extracting the dried and crushed asparagus by organic acid, neutralizing by alkali, extracting by ultrasonic, ultrafiltering, separating by ion exchange resin, concentrating and precipitating by alcohol. The preparation method of the asparagus polysaccharide extract is simple and efficient, and is suitable for industrial production, and the obtained asparagus polysaccharide extract has strong antioxidant activity and hypoglycemic activity, has high inhibition rate on dipeptidyl peptidase IV, and can be used for preparing hypoglycemic drugs or health care products.
Description
Technical field
The invention belongs to Thallus Gracilariae deep processing field, be specifically related to a kind of Thallus Gracilariae polyoses extract and preparation method thereof and application.
Background technology
Thallus Gracilariae (GracialriaLemaneofimrsi) belongs to rhodophyta, Gigartinales, and river hedge belongs to (Gracaialri), originates in China's Shandong coastal waters and okinawa of japan.Due to the small scale of Thallus Gracilariae cultivation in the past, output is not high and palatability is poor, thus seldom directly edible, be mainly used in extracting agar-agar, separately there is small part to be used as abalone culture feed, among the people being used for is used as medicine.In < < Compendium of Materia Medica > >, describe these flavour of a drug sweet cold in nature, have the effect of softening and eliminating sputum, clearing away heat and promoting diuresis, for controlling goitre knot hot gas, dysuria, yin asthenia generating intrinsic heat.At the beginning of 2000, marine resources research centre of development, Institute of Oceanology of the Chinese Academy of Sciences Guangdong Province and science and technology Xinghai County, Nanao County office cooperation development Thallus Gracilariae are transplanted the research of In The Eastern Guangdong Sea Area, project succeeds, and has started the south China sea area Thallus Gracilariae successful precedent of growing seedlings.After the popularization of 3 years, the cultivation of Nan'ao Thallus Gracilariae has reached large-scale production level, and mean yield reaches 525t/1000m
2, and driven the rise of coastland, Fujian, Guangdong large-scale farming.At present, Thallus Gracilariae has become the fourth-largest cultivation marine alga after sea-tangle, laver, wakame in China.
Because early stage Thallus Gracilariae output rareness is not taken seriously always, both at home and abroad to the research of Thallus Gracilariae all seldom.Along with propagating in recent years the continuous expansion of scale and increasing sharply of output artificially, about the research of Thallus Gracilariae function and application also causes people's interest gradually, but at present relevant research report mainly concentrates on plantation and processing aspect, research report to the extraction of asparagus active material and physiological function is very few, only has a small amount of patent open.As State Oceanic Administration Bureau The Third Oceanography Institute discloses a kind of Thallus Gracilariae agaropectin oligose and preparation method thereof, can be applicable in anti-oxidant, uvioresistant healthcare products and makeup (number of patent application 201210347105.5); Li Xuejiao discloses a kind of method (number of patent application 201210089080.3) of extracting cancer-resisting substance in Thallus Gracilariae; Zhengzhou Tobacco Research Institute of CNTC discloses the preparation method of asparagus rough polysaccharide and has been applied in cigarette, can improve humid keeping performance and the sucking quality (number of patent application 201010204566.8) of cigarette; Zhu Yisheng discloses a kind of method (number of patent application 201010188414.3) that improves the anti-oxidant composition of Thallus Gracilariae extraction liquid; Shanghai Ocean University discloses a kind of extraction and separation purification method of Thallus Gracilariae polysaccharide, and gained polysaccharide has good raising immune effect (number of patent application 200810042987.8); Shanghai Aquatic Products Univ. 9CN) discloses a kind of preparation method of Thallus Gracilariae polysaccharide, and gained Polysaccharides on Mice lymphocyte has higher cultivation effect (number of patent application 200710044610.1); Guangdong Pharmaceutical University disclose a kind of Thallus Gracilariae and working method, can be applicable to snackfoods (number of patent application 200710027284.3).
DPP IV (dipeptidyl peptidase IV, DPP-IV) glucagon-like peptide 1 (GLP-1 that can fast and effeciently degrade, glucagon-like peptide-1), GLP-1 is that Regular Insulin generates and secretion one of the most effective stimulant, therefore suppress the effect that DPP-IV can strengthen endogenous GLP-1, thereby the level of Regular Insulin in raising blood, and then reduce and maintain diabetics's glucose level.Medical science has confirmed that DPP-IV inhibitor is a kind of novel antidiabetic treatment medicine at present, clinical effectiveness shows that such medicine has good hypoglycemic effect, does not find that common body weight that other diabetes medicament produces increases and the untoward reaction such as hypoglycemia simultaneously.
Summary of the invention
In order to improve the deep process technology of Thallus Gracilariae, widen the range of application of Thallus Gracilariae, primary and foremost purpose of the present invention is to provide a kind of Thallus Gracilariae polyoses extract;
Another object of the present invention is to provide the preparation method of above-mentioned Thallus Gracilariae polyoses extract;
A further object of the present invention is to provide the application of above-mentioned Thallus Gracilariae polyoses extract.
Object of the present invention is achieved through the following technical solutions:
A Thallus Gracilariae polyoses extract, described Thallus Gracilariae polyoses extract is prepared from through extracting by Thallus Gracilariae, and main monosaccharide component is D-semi-lactosi and 3,6-inner ether-L semi-lactosi;
Described Thallus Gracilariae polyoses extract is prepared from by the preparation method who comprises following steps:
(1) Thallus Gracilariae is dried, pulverized and sieved, degreasing decoloring obtains Thallus Gracilariae powder;
(2) with organic acid soln, extract Thallus Gracilariae powder, then, with alkali neutralization, filter, obtain filter residue and extracting solution for the first time;
(3) step (2) gained filter residue is carried out to ultrasonic extraction method in water, filter to obtain extracting solution for the second time, described extracting solution for the first time and extracting solution are for the second time merged and obtain final extracting solution;
(4) the described final extracting solution of step (3) is carried out to ultrafiltration, collect and see through liquid;
(5) described in spent ion exchange resin separation, see through liquid, get high-activity component and carry out vacuum concentration, obtain concentrated solution;
(6) described concentrated solution is mixed with ethanol, standing, filter and obtain polysaccharide precipitation;
(7) described polysaccharide precipitation is dried, obtains described Thallus Gracilariae polyoses extract.
The preparation method of above-mentioned Thallus Gracilariae polyoses extract, comprises the steps:
(1) Thallus Gracilariae is dried, pulverized and sieved, degreasing decoloring obtains Thallus Gracilariae powder;
Preferably, described in, pulverize and sieve as pulverizing rear mistake 20～60 mesh sieves;
Wherein, the concrete steps of described degreasing decoloring are: adopt ethanolic soln or acetone soln, Thallus Gracilariae is carried out to micro-extraction of boiling, filter to obtain slag, dry for standby; Preferably, the volume mass of the volume of described ethanolic soln or acetone soln and the quality of described Thallus Gracilariae is than being (2～6): 1; Described ethanolic soln is the ethanolic soln of volume fraction 95%; Described micro-time of extracting of boiling is 2～4 hours;
(2) with organic acid soln, extract Thallus Gracilariae powder, then, with alkali neutralization, filter, obtain filter residue and extracting solution for the first time;
Preferably, the pH value of described organic acid soln is 1.5～3.5;
Preferably, described organic acid soln is citric acid solution or malic acid solution;
Preferably, the quality of described organic acid soln is 20～50 times of described Thallus Gracilariae opaque amount;
(3) step (2) gained filter residue is carried out to ultrasonic extraction method in water, filter to obtain extracting solution for the second time, described extracting solution for the first time and extracting solution are for the second time merged and obtain final extracting solution;
Preferably, the control condition of described ultrasonic extraction method is: ultrasonic power 320～640W, and extracting temperature is 30～70 ℃, extraction time is 20～60 minutes;
(4) the described final extracting solution of step (3) is carried out to ultrafiltration, collect and see through liquid;
Preferably, described ultrafiltration adopts the ultra-filtration membrane of molecular weight cut-off 20kDa;
(5) described in spent ion exchange resin separation, see through liquid, get high-activity component and carry out vacuum concentration, obtain concentrated solution;
Preferably, the model of described ion exchange resin is DEAE-fast flow or 717;
Preferably, described vacuum concentration gained concentrated solution be described see through liquid long-pending 1/5～1/3;
(6) described concentrated solution is mixed with ethanol, standing, filter and obtain polysaccharide precipitation;
Preferably, the consumption of described ethanol account for described concentrated solution mix with ethanol after cumulative volume 50%～80%;
Preferably, described standing concrete operations are: at 0～4 ℃ standing 8～14 hours;
(7) described polysaccharide precipitation is dried, obtains described Thallus Gracilariae polyoses extract;
Preferably, described be dried into vacuum lyophilization or spraying dry.
The application of above-mentioned Thallus Gracilariae polyoses extract in preparing inhibitors of dipeptidyl IV;
The application of above-mentioned Thallus Gracilariae polyoses extract in preparing hypoglycemic drug or healthcare products.
The present invention has following advantage and effect with respect to prior art:
(1) preparation method of the present invention adopts organic acid to extract polysaccharide in conjunction with ultrasonic method, and its extraction yield improves 2～4 times than traditional water extraction, can significantly shorten extraction time, reduce energy consumption, and antioxidant effect is better than traditional water extraction simultaneously.
(2) Thallus Gracilariae polyoses extract of the present invention can significantly suppress the activity of DPP IV, has effect of lowering blood sugar, is the reported first of this area, has filled up at present the research of this respect both at home and abroad blank.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
A Thallus Gracilariae polyoses extract, its preparation method is as follows:
(1) Thallus Gracilariae crosses 20 mesh sieves after shining dry grinding, adds volume fraction 95% ethanolic soln with respect to 2 times of volume mass ratios of Thallus Gracilariae, and micro-boiling extracted 3 hours, filters to obtain slag, dries to such an extent that Thallus Gracilariae powder is standby at 60 ℃;
(2) get 50g Thallus Gracilariae powder and be placed in container, mix by the mass ratio of 1:30 with the citric acid of pH2.0, micro-boiling extracted 3 hours, and with NaOH, being neutralized to pH value is neutrality, filters to obtain filter residue and extracting solution for the first time;
(3) by step (2) gained filter residue in water by ultrasonic extraction method, ultrasonic power 500W, extract 40 ℃ of temperature, extract 30 minutes, filter to obtain extracting solution for the second time, with step (2) gained for the first time extracting solution merge, obtain final extracting solution;
(4) the final extracting solution of step (3) gained is carried out to ultrafiltration with the film of molecular weight cut-off 20kDa, collect and see through liquid;
(5) the separated liquid that sees through of spent ion exchange resin DEAE-Fast flow model, gets the highest active component, vacuum concentration to see through liquid long-pending 1/4, obtain concentrated solution;
(6) in concentrated solution, add ethanol, after mixing, at 2 ℃ standing 12 hours, filter, remove supernatant liquid part, obtain polysaccharide precipitation;
(7) by the lyophilize of gained polysaccharide precipitation, obtain described Thallus Gracilariae polyoses extract, be designated as 1# extract.
Embodiment 2
A Thallus Gracilariae polyoses extract, its preparation method is as follows:
(1) Thallus Gracilariae crosses 60 mesh sieves after shining dry grinding, adds volume fraction 95% ethanolic soln with respect to 6 times of volume mass ratios of Thallus Gracilariae, and micro-boiling extracted 2 hours, filters to obtain slag, dries to such an extent that Thallus Gracilariae powder is standby at 40 ℃;
(2) get 50g Thallus Gracilariae powder and be placed in container, mix by the mass ratio of 1:50 with the oxysuccinic acid of pH1.5, micro-boiling extracted 1 hour, and with NaOH, being neutralized to pH value is neutrality, filters to obtain filter residue and extracting solution for the first time;
(3) by step (2) gained filter residue in water by ultrasonic extraction method, ultrasonic power 320W, extract temperature 60 C, extract 60 minutes, filter to obtain extracting solution for the second time, with step (2) gained for the first time extracting solution merge, obtain final extracting solution;
(4) the final extracting solution of step (3) gained is carried out to ultrafiltration with the film of molecular weight cut-off 20kDa, collect and see through liquid;
(5) the separated liquid that sees through of spent ion exchange resin 717 models, gets the highest active component, vacuum concentration to see through liquid long-pending 1/3, obtain concentrated solution;
(6) in concentrated solution, add ethanol, after mixing, at 4 ℃ standing 14 hours, filter, remove supernatant liquid part, obtain polysaccharide precipitation;
(7) by the lyophilize of gained polysaccharide precipitation, obtain described Thallus Gracilariae polyoses extract, be designated as 2# extract.
Embodiment 3
A Thallus Gracilariae polyoses extract, its preparation method is as follows:
(1) Thallus Gracilariae crosses 40 mesh sieves after shining dry grinding, adds volume fraction 95% ethanolic soln with respect to 5 times of volume mass ratios of Thallus Gracilariae, and micro-boiling extracted 4 hours, filters to obtain slag, dries to such an extent that Thallus Gracilariae powder is standby at 60 ℃;
(2) get 50g Thallus Gracilariae powder and be placed in container, mix by the mass ratio of 1:20 with the citric acid of pH3.5, micro-boiling extracted 3 hours, and with NaOH, being neutralized to pH value is neutrality, filters to obtain filter residue and extracting solution for the first time;
(3) by step (2) gained filter residue in water by ultrasonic extraction method, ultrasonic power 640W, extract 30 ℃ of temperature, extract 20 minutes, filter to obtain extracting solution for the second time, with step (2) gained for the first time extracting solution merge, obtain final extracting solution;
(4) the final extracting solution of step (3) gained is carried out to ultrafiltration with the film of molecular weight cut-off 20kDa, collect and see through liquid;
(5) the separated liquid that sees through of spent ion exchange resin DEAE-Fast flow model, gets the highest active component, vacuum concentration to see through liquid long-pending 1/5, obtain concentrated solution;
(6) in concentrated solution, add ethanol, after mixing, at 0 ℃ standing 8 hours, filter, remove supernatant liquid part, obtain polysaccharide precipitation;
(7) by the lyophilize of gained polysaccharide precipitation, obtain described Thallus Gracilariae polyoses extract, be designated as 3# extract.
The traditional water extraction of comparative example 1 is prepared Thallus Gracilariae polyoses extract
A Thallus Gracilariae polyoses extract, adopts traditional water extraction to be prepared, and its preparation method is as follows:
(1) Thallus Gracilariae crosses 20 mesh sieves after shining dry grinding, adds volume fraction 95% ethanolic soln with respect to 2 times of volume mass ratios of Thallus Gracilariae, and micro-boiling extracted 3 hours, filters to obtain slag, dries to such an extent that Thallus Gracilariae powder is standby at 60 ℃;
(2) get Thallus Gracilariae powder hot water in container and boil after 2 hours, filter to obtain filter residue and extracting solution for the first time; Described filter residue boils 1 hour, filters to obtain extracting solution for the second time; Then extracting solution and extracting solution merging for the second time for the first time, obtains final extracting solution;
(3) the final extracting solution of step (2) gained is carried out to ultrafiltration with the film of molecular weight cut-off 20kDa, collect and see through liquid;
(4) the separated liquid that sees through of spent ion exchange resin DEAE-Fast flow model, gets the highest active component, vacuum concentration to see through liquid long-pending 1/4, obtain concentrated solution;
(5) in concentrated solution, add ethanol, after mixing, at 0～4 ℃ standing 12 hours, filter, remove supernatant liquid part, obtain polysaccharide precipitation;
(6) by the lyophilize of gained polysaccharide precipitation, obtain Thallus Gracilariae polyoses extract, be designated as 4# extract.
Experimental example 1 is measured polysaccharide extract rate
Measure the polysaccharide extract rate of each Thallus Gracilariae polyoses extract in embodiment and comparative example.
Adopt phenolsulfuric acid method to measure the polysaccharide content in 1#～4# extract, calculate polysaccharide extract rate, formula is: polysaccharide extract rate (%)=(polysaccharide content in extracting solution (g)/raw material weight (g)) * 100.
Each Thallus Gracilariae polyoses extract measure and calculation result is as shown in table 1:
The polysaccharide extract rate of each extract of table 1.
| Extract | 1# extract | 2# extract | 3# extract | 4# extract |
| Polysaccharide extract rate (%) | 14.12±0.67 | 10.57±0.58 | 12.24±0.49 | 4.36±0.65 |
Note: in table, data are mean value ± standard deviation (n=3)
As can be known from the table data, the Thallus Gracilariae polysaccharide extract rate of the method for the invention is apparently higher than the polysaccharide extract rate of traditional water extraction.
Experimental example 2 is measured DPPH radical scavenging activity
The removing ability of measuring the DPPH free radical of each Thallus Gracilariae polyoses extract in embodiment and comparative example, the removing ability of DPPH free radical is a kind of method of comparatively general survey anti-oxidant activity.
Get the removing ability that 1～4# extract carries out DPPH free radical and measure, measuring method is as follows:
Getting 2mL concentration is that the aqueous solution of Thallus Gracilariae polyoses extract of 0.1～2.0mg/mL and the DPPH solution of the 0.2mmol/L of 2mL mix, vibration, and under room temperature, lucifuge is placed 30min, surveys light absorption value (Ai) under 517nm wavelength; Sample and 2mL dehydrated alcohol with 2mL same concentrations mix (Aj) as a control group, after mixing in addition, survey light absorption value (Ac) with 2mL DPPH solution and 2mL dehydrated alcohol.
Calculation formula is: DPPH clearance rate (%)=[1-(Ai-Aj)/Ac] * 100.The DPPH radical scavenging activity IC of each Thallus Gracilariae polyoses extract of determination and analysis gained
50be worth as shown in table 2:
The DPPH radical scavenging activity IC of each extract of table 2.
50value
From table data analysis known, the DPPH free radical scavenging activity of Thallus Gracilariae polyoses extract of the present invention is better than the polyoses extract of traditional water extraction gained.
Experimental example 3 is measured oxyradical receptivity (ORAC)
Measure the oxyradical receptivity of each Thallus Gracilariae polyoses extract in embodiment and comparative example.
Get respectively 1～4# extract and carry out oxyradical receptivity (ORAC) mensuration, adopt fluorescence microplate reader to measure, concrete steps comprise as follows:
In each micropore of 96 orifice plates, add respectively the Thallus Gracilariae polyoses extract sample that 20 μ L concentration are 0.05mg/mL, add again the phosphate buffer soln 20 μ L of pH7.4 and the luciferin solution 20 μ L that concentration is 7nmol/L, at 37 ℃ after preset 15min, with multichannel pipettor, in each hole, add rapidly the AAPH140 μ L of 12mmol/L to start reaction, and by microwell plate be placed in microplate reader at 37 ℃ with excitation wavelength 485nm, emission wavelength 538nm carries out METHOD FOR CONTINUOUS DETERMINATION, every 2min measures once each hole fluorescence intensity, and minute is 2h altogether.Each extract oxyradical receptivity (ORAC value) measurement result is as shown in table 3:
The oxyradical receptivity measurement result of each extract of table 3.
Note: in table, data are mean value ± standard deviation (n=3)
From table data analysis known, the anti-oxidant activity of Thallus Gracilariae polyoses extract of the present invention is better than the polyoses extract of traditional water extraction gained.
Experimental example 4 is measured the molecular weight of gained Thallus Gracilariae polyoses extract product
Measure the molecular weight of each Thallus Gracilariae polyoses extract in embodiment and comparative example.
Get respectively 1～4# extract and carry out molecular weight determination, the dextran standard of known molecular amount is mixed with respectively to the solution of 2.0mg/mL by moving phase, adopt gel permeation chromatography (GPC) determining molecular weight, location parameter comprises as follows:
Chromatographic condition: tsk gel guard column (PW * L6.0 * 40), TSK G-4000K PW * L7.8 * 300 gel column, TSKG-2500K PW * L7.8 * 300 gel column; Moving phase is 0.2mol/LKH2PO4 solution, pH6.0; Flow velocity 0.6mL/min; 35 ℃ of column temperatures; Sample introduction 30 μ L; Standard specimen is the dextran standard (Dextran, molecular weight is 4400Da, 9900Da, 21400Da, 43500Da, 124000Da, 196000Da, 277000Da, 401000Da, 1285000Da, Sigma company) of known molecular amount; Detector is Waters2414 differential refraction detector.The molecular-weight average result of measuring is as shown in table 4:
The molecular weight of each extract of table 4.
From table 4, data analysis is known, and the molecular weight of Thallus Gracilariae polyoses extract of the present invention is significantly less than the molecular weight of the traditional water extraction gained of comparative example 1 polyoses extract.
The monose that experimental example 5 is measured gained Thallus Gracilariae polyoses extract product forms
Get respectively embodiment 1～3 products therefrom Thallus Gracilariae polyoses extract and carry out monose composition measuring, measuring method and parameter comprise as follows:
Take Thallus Gracilariae polyoses extract sample 20mg, add 4M trifluoroacetic acid 5mL, sealing, 110 ℃ of hydrolysis 2h; Hydrolyzed solution, in 50 ℃ of rotary evaporation in vacuo to dry, adds methyl alcohol 3mL, then is spin-dried for, and repeats 3 times to obtain Thallus Gracilariae polysaccharide hydrolysis thing.
In Thallus Gracilariae polysaccharide hydrolysis thing, add oxammonium hydrochloride 10mg, interior mark inositol six acetic ester 1mg and pyridine 2mL, sealing, 90 ℃ of water-bath 30min, add again after 2mL acetic anhydride 90 ℃ of water-bath 30min again, add 2mL water termination reaction, add 2mL dichloromethane extraction, repeat twice, discard water layer, be settled to 5ml, add anhydrous sodium sulfate drying to cross film standby.
Gas chromatographic detection program: HP-5 quartz capillary column (30m * 0.32mm * 0.25 μ m); Constant voltage mode, 20PSI; Temperature programming: 100 ℃ of initial column temperatures, keep 0.5min; Then with 20 ℃/min, heat up, keep 5min; With 3 ℃/min, rise to 160 ℃; With 10 ℃/min, be raised to 250 ℃ again, keep 5min; Injection port adopts not shunt mode, 250 ℃ of temperature, and carrier gas is nitrogen; 250 ℃ of the temperature of fid detector, hydrogen, air and nitrogen flow rate are respectively 30,400 and 25mL/min; Sampling volume 1 μ L.
Various standard monose (rhamnosyl, pectinose, Fucose, wood sugar, seminose, glucose and semi-lactosi) carries out asccharin acetic ester derivatization treatment, the same terms gas chromatographic analysis under the same conditions.
Known to determination and analysis result, the main monose of 1#～3# extract consists of: semi-lactosi and 3,6-inner ether semi-lactosi.
Experimental example 6 is measured the inhibition ability of Thallus Gracilariae polysaccharide to DPP IV
Get respectively 1～4# extract sample and control sample hypoglycemic drug gliclazide and carry out the mensuration of the inhibition ability of DPP IV, measuring method and parameter comprise as follows:
It is in the DPP IV solution of 1UL/L that the sample of different concns is added to enzyme activity unit, make final concentration be followed successively by 1nmol/L, 10nmol/L, 20nmol/L, 100nmol/L and 500nmol/L, with water belongs with yin contrast, ice bath is hatched 30min, be added in 96 orifice plates every hole 100 μ L; Add 100 μ L substrate solutions, with 50mmol/L Tris-HCl, 1mol/LEDTA, it is blank that pH8.3 replaces substrate solution, establishes 4 multiple holes for every group, hatches after 1h for 37 ℃, and 405nm place surveys light absorption value, and calculates inhibiting rate according to formula.
Calculation formula: DPP IV inhibiting rate=(A
negative control-A
polysaccharide)/A
negative control* 100%.
Each sample is as shown in table 5 to the inhibition ability of DPP IV:
The DPP IV inhibiting rate result of each sample of table 5.
| Sample | 1# extract | 2# extract | 3# extract | 4# extract | Gliclazide |
| Inhibiting rate (%) | 75.49±1.44 | 70.57±1.89 | 64.23±1.11 | 50.24±2.43 | 77.68±1.94 |
Note: in table, data are mean value ± standard deviation (n=3)
As can be known from the table data, products therefrom Thallus Gracilariae polyoses extract of the present invention to the inhibiting rate of DPP IV higher than traditional extraction process products therefrom, can be suitable with hypoglycemic drug gliclazide.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (7)
1. a Thallus Gracilariae polyoses extract, is characterized in that: described Thallus Gracilariae polyoses extract is prepared from through extracting by Thallus Gracilariae, and main monosaccharide component is D-semi-lactosi and 3,6-inner ether-L semi-lactosi.
2. Thallus Gracilariae polyoses extract according to claim 1, is characterized in that: described Thallus Gracilariae polyoses extract is prepared from by the preparation method who comprises following steps:
(1) Thallus Gracilariae is dried, pulverized and sieved, degreasing decoloring obtains Thallus Gracilariae powder;
(2) with organic acid soln, extract Thallus Gracilariae powder, then, with alkali neutralization, filter, obtain filter residue and extracting solution for the first time;
(3) step (2) gained filter residue is carried out to ultrasonic extraction method in water, filter to obtain extracting solution for the second time, described extracting solution for the first time and extracting solution are for the second time merged and obtain final extracting solution;
(4) the described final extracting solution of step (3) is carried out to ultrafiltration, collect and see through liquid;
(5) described in spent ion exchange resin separation, see through liquid, get high-activity component and carry out vacuum concentration, obtain concentrated solution;
(6) described concentrated solution is mixed with ethanol, standing, filter and obtain polysaccharide precipitation;
(7) described polysaccharide precipitation is dried, obtains described Thallus Gracilariae polyoses extract.
3. a preparation method who prepares the Thallus Gracilariae polyoses extract described in claim 1 or 2, is characterized in that comprising the steps:
(1) Thallus Gracilariae is dried, pulverized and sieved, degreasing decoloring obtains Thallus Gracilariae powder;
(2) with organic acid soln, extract Thallus Gracilariae powder, then, with alkali neutralization, filter, obtain filter residue and extracting solution for the first time;
(3) step (2) gained filter residue is carried out to ultrasonic extraction method in water, filter to obtain extracting solution for the second time, described extracting solution for the first time and extracting solution are for the second time merged and obtain final extracting solution;
(4) the described final extracting solution of step (3) is carried out to ultrafiltration, collect and see through liquid;
(5) described in spent ion exchange resin separation, see through liquid, get high-activity component and carry out vacuum concentration, obtain concentrated solution;
(6) described concentrated solution is mixed with ethanol, standing, filter and obtain polysaccharide precipitation;
(7) described polysaccharide precipitation is dried, obtains described Thallus Gracilariae polyoses extract.
4. preparation method according to claim 3, is characterized in that: described in step (1), pulverize and sieve as pulverizing rear mistake 20～60 mesh sieves; The concrete steps of the described degreasing decoloring of step (1) are: adopt ethanolic soln or acetone soln, Thallus Gracilariae is carried out to micro-extraction of boiling, filter to obtain slag, dry for standby;
The pH value of the described organic acid soln of step (2) is 1.5～3.5; The described organic acid soln of step (2) is citric acid solution or malic acid solution; The quality of the described organic acid soln of step (2) is 20～50 times of described Thallus Gracilariae opaque amount;
The control condition of the described ultrasonic extraction method of step (3) is: ultrasonic power 320～640W, and extracting temperature is 30～70 ℃, extraction time is 20～60 minutes;
The described ultrafiltration of step (4) adopts the ultra-filtration membrane of molecular weight cut-off 20kDa;
The model of the described ion exchange resin of step (5) is DEAE-fast flow or 717; The described vacuum concentration gained of step (5) concentrated solution be described see through liquid long-pending 1/5～1/3;
The consumption of the described ethanol of step (6) accounts for described concentrated solution and mixes 50%～80% of rear cumulative volume with ethanol; The described standing concrete operations of step (6) are: at 0～4 ℃ standing 8～14 hours;
Step (7) is described to be dried as vacuum lyophilization or to spray dry.
5. preparation method according to claim 4, is characterized in that: in the concrete steps of the described degreasing decoloring of step (1): the volume of described ethanolic soln or acetone soln is (2～6) with the volume mass ratio of the quality of described Thallus Gracilariae: 1; Described ethanolic soln is the ethanolic soln of volume fraction 95%; Described micro-time of extracting of boiling is 2～4 hours.
6. the application of Thallus Gracilariae polyoses extract according to claim 1 and 2 in preparing inhibitors of dipeptidyl IV.
7. the application of Thallus Gracilariae polyoses extract according to claim 1 and 2 in preparing hypoglycemic drug or healthcare products.
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