CN116023522A - Fucoidin and preparation method thereof - Google Patents
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- CN116023522A CN116023522A CN202310183878.2A CN202310183878A CN116023522A CN 116023522 A CN116023522 A CN 116023522A CN 202310183878 A CN202310183878 A CN 202310183878A CN 116023522 A CN116023522 A CN 116023522A
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- 238000000605 extraction Methods 0.000 claims abstract description 67
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- 241001261506 Undaria pinnatifida Species 0.000 claims abstract description 27
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to the field of fucoidin processing, in particular to fucoidin and a preparation method thereof. The method comprises cleaning Undaria pinnatifida, adding into calcium hydroxide solution, heating and extracting to obtain extractive solution, and introducing CO into the extractive solution 2 Or add H 3 PO 4 To be matched with Ca (0H) 2 Reacting to generate precipitate, and filtering to obtain fucoidin extract. By using Ca (OH) 2 With CO 2 Or H 3 PO 4 The reaction generates the precipitate, the multi-step reaction between the two only generates the white precipitate which is easy to separate, and no other substances are generated, so that the problem of resource waste is effectively solved, the extraction time is short, and the production efficiency is improved. The fucoidin prepared by the method has better effect on cholate and activation on pancreatic lipase than the fucoidin prepared by other existing methods, and has great potential in the application aspect of reducing blood fat.
Description
Technical Field
The invention relates to the field of fucoidin processing, in particular to fucoidin and a preparation method thereof.
Background
Seaweed is an important aquatic product resource in China, mainly comprises three major categories of brown seaweed, red seaweed and green seaweed, and occupies an important position in an economic system in China. The seaweed is nutritious, and contains proteins, dietary fibers, polyunsaturated fatty acids, vitamins and minerals. So seaweed is one of the important resources for extracting functional polysaccharides. The undaria pinnatifida is a seaweed plant and belongs to Phaeophyta. In some countries in Europe and America, undaria pinnatifida is called as 'vegetables in sea', and the undaria pinnatifida is a large brown alga with extremely high medicinal value and economic value. The Undaria pinnatifida is rich in algal polysaccharide, brown algae polyphenol and superoxide dismutase with antioxidant activity. Among them, polysaccharides present in undaria pinnatifida are mostly Fucoidan (fucoidin), also called fucoidin sulfate, which is a sulfate-containing water-soluble heteropolysaccharide present in brown algae, and monosaccharides constituting the structure thereof are fucose, xylose, galactose, glucose, rhamnose and mannose, and uronic acid and sulfate are present in addition to these basic monosaccharides.
Considering that a large amount of fucoidan colloid exists in the medullary cell gap of the brown algae plant cell wall, proper mode (such as alkali/acid extraction process or physical mode) can be adopted to break the wall of the fucoidan in the fucoidan extraction process to obtain fucoidan. There are a great deal of reports on physical-combined chemical extraction methods at present, but new equipment with high price is needed, industrialization cannot be realized temporarily, and the physical methods still only play the role of auxiliary chemical methods. Compared with the water extraction method with long extraction time and low extraction rate, the alkali extraction process is widely applied to obtaining algal polysaccharide, but the alkali extraction process needs to be pointed out that a large amount of alkali liquor generated in the alkali extraction process and a large amount of water is needed to elute alkali liquor (for example, 0.7 ton of sodium hydroxide is needed for each 1 ton of red algae polysaccharide (agar) production, and more than 100 tons of wastewater generated after neutralization by acid) is needed for each production, and soluble salts in the polysaccharide extract are removed, so that serious pollution to the surrounding environment is caused, water resource waste is caused, and seaweed colloid is degraded and lost in a large amount (the extraction yield is reduced). This is a realistic challenge for colloid manufacturing enterprises. In the present day, under the big background of pursuing green cleaning, if the use amount of alkali is reduced in the extraction process, the process is an environment-friendly and development-prospect process.
In addition, the alkali treatment can remove the sulfate radical with active function naturally contained in the seaweed polysaccharide structure in the extraction process, however, after the sulfate radical is removed, the active function of the polysaccharide is obviously reduced or even lost. Therefore, how to adopt an environment-friendly extraction process to prepare fucoidin with better biological activity is an important bottleneck in the development process of fucoidin functional products.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of fucoidin, which comprises the steps of cleaning undaria pinnatifida, adding the undaria pinnatifida into calcium hydroxide solution, heating and extracting to obtain an extracting solution, and introducing CO into the extracting solution 2 Or add H 3 PO 4 To be matched with Ca (0H) 2 Reacting to generate precipitate, and filtering to obtain fucoidin extract.
In one embodiment, the calcium hydroxide solution consists of Ca (0H) 2 And water in 1g: mixing in a proportion of 25mL to 500 mL.
In one embodiment, the undaria pinnatifida and Ca (OH) 2 The weight-to-volume ratio of the solution is 1g to 20mL to 35mL.
In one embodiment, the temperature of the heated extraction is 50 ℃ to 100 ℃.
In one embodiment, the heating extraction time is 3 hours to 8 hours.
In one embodiment, CO is introduced into the extract 2 Until a milky white precipitate formed.
In one embodiment, the H 3 PO 4 And Ca (0H) 2 The neutralization condition is H 3 PO 4 And Ca (0H) 2 The molar ratio of (2) is 3:2 or 1:1.
In one embodiment, the fucoidan extract is further concentrated under reduced pressure and dried to obtain a solid fucoidan.
The invention provides a fucoidin prepared by any of the preparation methods.
In one embodiment, the fucoidan has a sulfate content of 18.5% to 24.9%.
Based on the above, compared with the prior art, the preparation method of fucoidin provided by the invention has the following technical principles and effects:
by using Ca (OH) 2 With CO 2 Generating CaCO by reaction 3 Precipitation, or H 3 PO 4 With Ca (OH) 2 Reacting in the solution to generate Ca 3 (PO 4 ) 2 Or 3CaHPO 4 The precipitation, the multi-step reaction between the two only produces white precipitation which is easy to separate, no other substances are produced, the desalination treatment of a large amount of water required in the extraction process and after the neutralization treatment of fucoidin is avoided, the problem of resource waste is effectively relieved, the extraction time is short, and the production efficiency is improved. Moreover, the extraction mode can reduce the removal of active group sulfate radicals of the fucoidin, so that the fucoidin prepared by the method has a certain blood fat reducing function.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
FIG. 1 is Ca (OH) 2 -CO 2 A columnar schematic diagram of the effect of extraction temperature on fucoidan extraction effect in the method.
FIG. 2 is Ca (OH) 2 -H 3 PO 4 Ca (OH) at different concentrations in the process 2 A columnar schematic of the effect of the solution on fucoidan extraction.
FIG. 3 is Ca (OH) 2 -H 3 PO 4 A columnar schematic diagram of the effect of extraction temperature on fucoidan extraction effect in the method.
FIG. 4 is a diagram of Ca (OH) 2 -H 3 PO 4 A columnar schematic of the effect of extraction time on fucoidan extraction effect in the process.
FIG. 5 is Ca (OH) 2 And H is 3 PO 4 A histogram of the effect of the molar ratio on the extraction effect of fucoidan.
FIG. 6 is a bar graph showing the activation of pancreatic lipase by different fucoidan samples.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention; the technical features designed in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that all terms used in the present invention (including technical terms and scientific terms) have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs and are not to be construed as limiting the present invention; it will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
In order to embody that the preparation method of the fucoidin provided by the invention has outstanding technical effects compared with the prior art, the invention combines the following examples and comparative examples, and the method for testing and calculating specific related indexes, namely the extraction rate, sulfate radical content, alkali consumption and water consumption of the whole preparation process, are evaluated as follows:
(1) Extraction rate:
1) Preparation of fucose standard curve
Accurately weighing and drying to constant weight of 0.01-g L-fucose standard substance, and fixing volume to 100mL with pure water to obtain fucose standard solution. And transferring 0mL, 1mL, 3mL, 5mL, 7mL and 9mL of the fucose standard solution into a 10mL volumetric flask by using a pipette, and fixing the volume to 10mL by pure water to obtain the standard solution to be measured. Respectively taking 1mL of the standard solution to be detected with each concentration into a test tube, respectively adding 1mL of phenol water solution with the concentration of 5%, then adding 5mL of concentrated sulfuric acid (with the mass concentration of 98%), uniformly mixing, standing at room temperature for 30min, measuring absorbance at 490nm, taking the fucose concentration as an abscissa, and taking A as an index 490 And drawing a standard curve on the ordinate.
2) Determination of fucoidin content in sample to be measured
The fucoidin obtained by adopting the scheme is prepared into 0.1mg/mL polysaccharide solution by deionized water, 1mL polysaccharide solution is accurately sucked by a pipette, 1mL of 5% phenol water solution is added, 5mL concentrated sulfuric acid is added, vortex mixing is carried out, after 30min at room temperature, absorbance is measured at 490nm, and meanwhile, blank control is carried out. Fucoidan content X1 (μg/mL) =u/c×100% based on fucose
Polysaccharide extraction X2 = m2/m1×100%
Fucoidin yield = X1/X2
U-fucoidan concentration in samples (. Mu.g/mL) was obtained from standard curves.
C-actual concentration of sample solution (. Mu.g/mL).
m 1-weight the mass (g) of undaria pinnatifida.
m 2-quality of crude fucoidan extracted from m1 (g)
(2) Sulfate radical
1)K 2 SO 4 Preparation of standard solution: accurately weighing 1.088g of K dried to constant weight 2 SO 4 Dissolved in 1mol/L HCl solution (500 mL).
2) Preparation of gelatin-barium chloride solution: accurately preparing 0.5% (w/v) gelatin solution, standing at 4deg.C overnight, and preparing 1% gelatin-barium chloride solution as solvent, and standing at 4deg.C.
3) Respectively measuring 0, 0.2, 0.4, 0.6, 0.8 and 1.0mLK 2 SO 4 Standard solution to 10mL of stoppered tube, less than 1mL of sample was made up to 1mL with ultrapure water. Subsequently, 3mL of gelatin-barium chloride solution was added to the test tube, and after mixing, the mixture was allowed to stand for 10 minutes to measure the absorbance of the sample at 360 nm. Drawing to obtain SO 4 2- Content standard curve.
4) Measuring the sulfate radical content: accurately weighing 0.050g fucoidin sample to be measured in a 25mL colorimetric tube, adding 25mL of 1mol/L HCl solution, placing in a water bath at 100 ℃ for acidolysis digestion for 5h, cooling to room temperature, decolorizing with active carbon, and filtering to collect filtrate. 1mL of the filtrate was measured, and the mixture was thoroughly mixed with 3mL of a gelatin-barium chloride solution, and after standing for 10min, the absorbance of the sample at 360nm was measured. The sulfate content of fucoidan was determined according to the standard curve described above.
(3) Percentage reduction of alkali consumption and water consumption:
percent (%) reduction= [ (A1-A0)/A1 ] X100%;
a1-alkali consumption (water consumption) of the traditional scheme; a0-improvement of alkali consumption (water consumption).
The invention provides the following examples
Example 1-Effect of extraction temperature on fucoidan extraction Effect (Ca (OH) 2 -CO 2 Method of
Respectively weighing 50g of undaria pinnatifida, cleaning for standby, and preparing 6 parts of Ca (OH) 2 Solution of Ca (OH) 2 The solution is composed of Ca (OH) 2 Mixing with water according to the proportion of 1g to 150 mL.
Subsequently, the groups were prepared from Undaria pinnatifida and Ca (OH) 2 The solution was prepared according to 1g:25mL, mixing and stirring, and respectively placing in a container at 50deg.C, 60deg.C, 70deg.C, 80deg.C, 90deg.C and 100deg.C for 6 hr. CO is introduced into 2 Filtering after the gas until the milky white precipitate is generated, and obtaining clear fucoidin extract.
And concentrating under reduced pressure and drying the fucoidin extract obtained in each group to obtain solid fucoidin.
The effect of different extraction temperatures on fucoidin extraction effect is shown in figure1, the fucoidan sulfate content (in SO 4 2- Calculated as) the tendency of increasing and then decreasing with increasing temperature, the sulfate radical of fucoidin reaches a maximum value of 23.8% when the extraction temperature is 80 ℃. The temperature also has an effect on the extraction rate of polysaccharide, and when the extraction temperature is 90 ℃, the yield of fucoidin reaches the maximum value of 8.7 percent.
EXAMPLE 2 Ca (OH) at various concentrations 2 Effect of solution on fucoidan extraction Effect (Ca (OH) 2 -H 3 PO 4 Method of
Weighing 5 parts of undaria pinnatifida 50g respectively, cleaning for standby, and adding Ca (OH) respectively 2 And water were arranged in 5 sets of Ca (OH) at different concentrations in a ratio of 1g:500mL,1g:250mL,1g:150mL,1g:75mL,1g:25mL 2 A solution.
Subsequently, the undaria pinnatifida and Ca (OH) were combined in a ratio of 1g:35mL 2 The solution is mixed and stirred evenly, and then is placed in a container at 90 ℃ for 8 hours. Then, add H 3 PO 4 Solution and Ca (OH) 2 The reaction generates milky Ca 3 (PO 4 ) 2 Precipitation (Ca (OH) therein 2 And H is 3 PO 4 The molar ratio of (2) is 3:2), and then filtering to obtain clear fucoidin extract.
And finally, concentrating and drying the fucoidin solution obtained in each group under reduced pressure to obtain a fucoidin finished product.
Ca (OH) of different concentrations 2 The effect of the solution on fucoidan extraction is shown in FIG. 2, and the fucoidan sulfate content (in SO 4 2- Meter) with Ca (OH) 2 The increase in concentration tends to increase and decrease, when Ca (OH) 2 The concentration of the sulfate radical reaches 22.4% of the highest value when the concentration is 1:150 (unit: g/mL). Ca (OH) 2 The solution also has a significant effect on the extraction rate and yield of polysaccharide, but when the alkali liquor ratio is 1:75, the yield of fucoidin reaches an optimal value of 8.2%.
Example 3-Effect of extraction temperature on fucoidan extraction Effect (Ca (OH) 2 -H 3 PO 4 Method of
Respectively weighing 50g of undaria pinnatifida, cleaning for standby, and preparing 6 parts of Ca (OH) 2 Solution of Ca (OH) 2 The solution is composed of Ca (OH) 2 Mixing with water according to the proportion of 1g to 150 mL.
Subsequently, the groups were prepared from Undaria pinnatifida and Ca (OH) 2 The solution was prepared according to 1g:25mL, mixing and stirring, and respectively placing in a container at 50deg.C, 60deg.C, 70deg.C, 80deg.C, 90deg.C and 100deg.C for 6 hr. Then respectively adding H 3 PO 4 Solution and Ca (OH) 2 The reaction generates milky Ca 3 (PO 4 ) 2 Precipitation (Ca (OH) therein 2 And H is 3 PO 4 The molar ratio of (2) is 3:2), and then filtering to obtain clear fucoidin extract.
And finally, concentrating and drying the fucoidin solution obtained in each group under reduced pressure to obtain a fucoidin finished product.
The effect of different extraction temperatures on fucoidan extraction effect is shown in FIG. 3, and the fucoidan sulfate content (in SO 4 2- Calculated) with the increasing temperature, the sulfate radical of the fucoidin reaches the highest value of 24.4 percent when the extracting temperature is 80 ℃, the yield of the fucoidin also reaches the optimal value of 8.9 percent, and the extracting rate of the fucoidin reaches the optimal value of 17.8 percent when the extracting temperature is 90 ℃.
Example 4-Effect of extraction time on fucoidan extraction effect (Ca (OH) 2 -H 3 PO 4 Method of
Respectively weighing 50g of undaria pinnatifida, cleaning for standby, and preparing 6 parts of Ca (OH) 2 Solution of Ca (OH) 2 The solution is composed of Ca (OH) 2 Mixing with water according to the proportion of 1g to 150 mL.
Subsequently, the groups were prepared from Undaria pinnatifida and Ca (OH) 2 The solution was prepared according to 1g:25mL, mixing and stirring, and then placing in a container at 80 ℃ for respectively treating for 3h, 4h, 5h, 6h, 7h and 8h. Then add H 3 PO 4 Solution and Ca (OH) 2 The reaction generates milky Ca 3 (PO 4 ) 2 Precipitation (Ca (OH) therein 2 And H is 3 PO 4 Is of the mole of (2)The molar ratio is 3:2) and filtering to obtain clear fucoidin extract.
And finally, concentrating and drying the fucoidin solution obtained in each group under reduced pressure to obtain a fucoidin finished product.
The effect of different extraction times on fucoidan extraction effect is shown in FIG. 4, and the fucoidan sulfate content (in SO 4 2- Calculated) with the increase of the heat treatment time, the trend of increasing and then decreasing appears, and when the heat treatment time is 5 hours, the detected sulfate radical content reaches the highest value of 24.9 percent. The extraction time is different, the yield of fucoidin is also different, and the fucoidin reaches the optimal value when the extraction time is 7h, and is about 8.6 percent
Example 5-Ca (OH) 2 And H is 3 PO 4 Effect of molar ratio on fucoidan extraction effect
Respectively weighing 50g of undaria pinnatifida, cleaning for standby, and preparing 2 parts of Ca (OH) 2 Solution of Ca (OH) 2 The solution is composed of Ca (OH) 2 Mixing with water according to the proportion of 1g to 150 mL.
Subsequently, the undaria pinnatifida and Ca (OH) were combined in a ratio of 1g:20mL for each group 2 The solutions are mixed and stirred evenly, and then are respectively placed in a container at 80 ℃ for 5 hours.
Then respectively adding H 3 PO 4 Solution and Ca (OH) 2 The reaction generates milky Ca 3 (PO 4 ) 2 Precipitation (Ca (OH) of one group 2 And H is 3 PO 4 The molar ratio of (2) is 3:2, another group of Ca (OH) 2 And H is 3 PO 4 The molar ratio of 1:1) and then filtering to obtain a clear fucoidan extract.
And finally, concentrating the fucoidin extracting solution obtained in each group under reduced pressure, and drying to obtain a fucoidin finished product.
Different Ca (OH) 2 And H is 3 PO 4 The effect of the molar ratio of the fucoidin on the extraction effect of fucoidin is shown in FIG. 5, and the added amount of phosphoric acid in the fucoidin obtained in the two groups of this example was measured for the sulfate radical content (in SO 4 2- Calculated) have no obvious influence, are about 24.8, and are polysaccharideThe extraction yield and yield of (a) are also substantially the same.
The invention also provides the following comparative examples
Comparative example 1-conventional NaOH-HCl extraction
Firstly, 50g of undaria pinnatifida is respectively weighed and cleaned, and NaOH solution with the mass concentration of 3% is prepared for standby.
Then, the undaria pinnatifida and the NaOH solution are mixed and stirred uniformly according to the proportion of 1g to 25mL, the undaria pinnatifida and the NaOH solution are placed in a container at 80 ℃ for 5 hours, hydrochloric acid (0.5M) is used for adjusting the pH value of the filtrate to 6-7, and the clear fucoidin solution is obtained after nanofiltration and desalination.
And finally, concentrating the obtained fucoidin solution under reduced pressure, and drying to obtain a fucoidin finished product.
The detection shows that the sulfate radical content of fucoidin obtained in this comparative example is 14.1%, which indicates that the extraction method is easy to remove a large amount of sulfate radical.
Further, it was calculated that the alkali consumption of each of examples 1 to 5 was reduced by about 85% and the water consumption was reduced by about 96% as compared with comparative example 1.
From this, it can be seen that comparative example 1, which uses NaOH and HCl to extract fucoidin, requires subsequent desalting by nanofiltration, and not only consumes a large amount of alkali and water, but also causes a decrease in fucoidin extraction rate and sulfate loss during the treatment. The method for extracting fucoidin can not only greatly reduce alkali consumption and water consumption, but also improve the extraction rate of fucoidin and avoid sulfate radical removal.
Comparative example 2 conventional hot water extraction
Respectively weighing 50g of undaria pinnatifida, and cleaning for standby. Mixing undaria pinnatifida and water according to the proportion of 1g to 25mL, stirring uniformly, placing in a container at 90 ℃ for extraction for 24 hours, filtering to obtain clear fucoidin extract, concentrating under reduced pressure, and drying to obtain a fucoidin finished product.
The sulfate content of fucoidan obtained in this comparative example was determined to be 22.3%, whereas the fucoidan extraction rate by the method of this comparative example was only 0.51 times that of example 4, but the extraction time was 6 times that of example 4. Therefore, the conventional hot water leaching method has low extraction efficiency and high time cost.
In order to further illustrate the active function of the fucoidin prepared by the invention, the invention also carries out the following in vitro lipid-lowering activity test, and the specific test contents are as follows:
1. in vitro binding cholic acid experiments
The specific operation is as follows:
1.1, drawing a cholate standard curve: preparing 0.3mmol/L Sodium Taurocholate (STC), sodium Glycocholate (SGC) and Sodium Cholate (SC) solution with phosphoric acid buffer solution (0.1 mol/L, pH 6.3); taking 0mL, 0.1mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL and 2.5mL of the cholate solution respectively in a 10mL test tube with a plug, and supplementing the cholate solution to 2.5mL by using a phosphate buffer solution; 7.5mL of sulfuric acid solution (60% by mass) was then added; water bath at 70 ℃ for 20min and ice bath for 5min; finally, measuring absorbance value at 387 nm; standard curves were plotted with absorbance values and cholate concentration.
1.2 cholate binding experiments: 1mL of polysaccharide solution samples (respectively configured to be 0.5 mg/mL, 1.5 mg/mL and 2.5 mg/mL) are taken out in 10mL test tubes with plugs, 1mL of HCl solution (0.01 mol/L) is added, the temperature is kept constant for 1h at 37 ℃, pH is adjusted to 6.3 by NaOH solution (0.1 mol/L), then 4mL of pancreatin (10 mg/mL and pH of 6.3 are added, the mixture is prepared by 0.1mol/L of phosphate buffer solution), after shaking at 37 ℃ for 1h at constant temperature, 4mL of different cholate solutions (M) are added to each sample, after shaking at 37 ℃ for 1h at constant temperature, after cholate is fully combined, the mixture is centrifuged for 20min at 4000 r/min. The supernatant was assayed for cholate content (M1) as described in step 1.1.
Binding rate (%) =100×m-M1/M
Table 1: binding rate of different polysaccharides to 3 cholates
Note that: (1) (2), (3) and (4) represent fucoidan samples having the largest sulfate group in example 1, example 5, comparative example 1 and comparative example 2, respectively.
As can be seen from Table 1, the polysaccharide obtained by the different extraction methods has a different binding effect on cholate. The combination effect of the samples (1) and (2) and cholate is superior to that of the other samples, and the sample has great potential in the application aspect of reducing blood fat.
2. Determination of the Effect of polysaccharide on pancreatic Lipase Activity
According to Table 2, 1mL soybean oil was added to each of several 250mL Erlenmeyer flasks, and 0.025 mol.L was added -1 Phosphate buffer (ph=7.4) 5mL, after water bath at 37 ℃ for 5min, 50mg·ml was added respectively -1 Fucoidan sample solution 0, 20. Mu.L, 40. Mu.L (corresponding to the addition concentration of 0, 1.000 mg. Multidot.mL) -1 、2.000mg·mL -1 ) The temperature is kept for 5min in a water bath at 37 ℃.1mL of 2mg.mL was added to each flask separately except for the control -1 Pancreatic lipase liquid (from 0.025 mol.L) -1 Is prepared by adding 15mL of 95% ethanol after 5min of reaction to stop enzyme reaction, and finally dripping 2 to 3 drops of 1% phenolphthalein, and using 0.025 mol.L -1 Sodium hydroxide solution was titrated to a pale red color, with a blank.
Table 2: pancreatic lipase activity system
Project | Soybean oil/mL | Phosphate buffer/mL | Polysaccharide solution/. Mu.L | Pancreatic lipase liquid/mL |
Blank pipe | 1.0 | 5.0 | - | 1.0 |
Blank control tube | 1.0 | 5.0 | - | - |
Sample tube | 1.0 | 5.0 | 20/30/40 | 1.0 |
Inhibitor background control | 1.0 | 5.0 | Corresponding inhibitor tube | - |
Sample background control tube | 1.0 | 5.0 | Corresponding sample tube | - |
The activation rate is calculated as follows: activation rate/% = 100× [ a-B- (C-D) ]/(a-B)
Wherein: a is the consumption of sodium hydroxide solution by the sample tube and is mL; b is the amount of sodium hydroxide solution consumed by the background control tube, mL; c is the amount of sodium hydroxide solution consumed by the blank tube, and mL; d is the amount of sodium hydroxide solution consumed by the blank tube, mL.
The activation of pancreatic lipase by different fucoidan samples is shown in FIG. 6, and the activation effect is (2) > (1) > (3) > (4) in this order, (1), (2), (3) and (4) are the fucoidan samples having the largest sulfate group in example 1, example 5, comparative example 1 and comparative example 2, respectively. Compared with fucoidin prepared by other existing methods, the fucoidin prepared by the method has more obvious activation effect on pancreatic lipase, can promote the hydrolysis of fat, is favorable for the discharge of fat, cholesterol and bile acid from feces, and simultaneously promotes the conversion of cholesterol to bile acid, so that the fucoidin has a certain function of reducing blood fat.
In summary, the preparation method of fucoidin provided by the invention not only can improve the extraction rate and sulfate radical content of fucoidin, but also can avoid the problem that a large amount of water is needed for desalination treatment in the neutralization treatment link in the extraction process, and can greatly shorten the extraction time and improve the production efficiency. In addition, the fucoidin prepared by the method has better effects on cholate and pancreatic lipase than the fucoidin prepared by other existing methods, and has great potential in the application aspect of reducing blood fat.
In addition, it should be understood by those skilled in the art that although many problems exist in the prior art, each embodiment or technical solution of the present invention may be modified in only one or several respects, without having to solve all technical problems listed in the prior art or the background art at the same time. Those skilled in the art will understand that nothing in one claim should be taken as a limitation on that claim.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. A method for preparing fucoidin is characterized in that undaria pinnatifida is cleaned and put into calcium hydroxide solution for heating and extraction to obtain extract, and then CO is introduced into the extract 2 Or add H 3 PO 4 To be matched with Ca (0H) 2 Reacting to generate precipitate, and filtering to obtain fucoidin extract.
2. The method for preparing fucoidan according to claim 1, wherein: the calcium hydroxide solution is prepared from Ca (0H) 2 And water in 1g: mixing in a proportion of 25mL to 500 mL.
3. The method for preparing fucoidan according to claim 1, wherein: the undaria pinnatifida and Ca (OH) 2 The weight-to-volume ratio of the solution is 1g to 20mL to 35mL.
4. The method for preparing fucoidan according to claim 1, wherein the temperature of the heat extraction is 50 ℃ to 100 ℃.
5. The method for preparing fucoidan according to claim 1, wherein: the time of the heat extraction is 3 to 8 hours.
6. The method for preparing fucoidan according to claim 1, wherein: introducing CO into the extract 2 Until a milky white precipitate formed.
7. The method for preparing fucoidan according to claim 1, wherein: the H is 3 PO 4 And Ca (0H) 2 The neutralization condition is H 3 PO 4 And Ca (0H) 2 The molar ratio of (2) is 3:2 or 1:1.
8. The method for preparing fucoidan according to claim 1, wherein: the fucoidin extract is also subjected to reduced pressure concentration and drying to obtain solid fucoidin.
9. A fucoidan, characterized by: a process for the preparation of fucoidan as claimed in any one of claims 1 to 9.
10. Fucoidan according to claim 9, characterized in that: the sulfate radical content of the fucoidin is 18.5-24.9%.
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