CN105029635A - Clamworm ultrahigh pressure extraction method and clamworm extractive prepared according to method - Google Patents
Clamworm ultrahigh pressure extraction method and clamworm extractive prepared according to method Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
The invention relates to the technical field of extraction processes, and particularly discloses a clamworm ultrahigh pressure extraction method and a clamworm extractive prepared according to the method. The method comprises the following steps: grinding freeze-dried clamworm into powder, dissolving the powder in an organic solvent, carrying out extraction for 20-40 minutes under the conditions of 300-400 MPa and 10-30 DEG C, and carrying out centrifugation and concentration to obtain the clamworm extractive, wherein the organic solvent is n-hexane, cyclohexane, ethyl acetate, acetone or methanol. The clamworm extractive obtained according to the method is a crude extractive, and can be directly used without being purified; tests show that when the concentration of the clamworm extractive is 6.25 mg/mL, the DPPH clearance rate is up to 87.28%; when the concentration of the clamworm extractive is 100 mg/mL, the oxygen anion free radical clearance rate reaches 71.32%; when the concentration of the clamworm extractive is 250 mg/mL, the hydroxy radical clearance rate reaches 62.18%; the obtained clamworm extractive is extremely high in antioxidant capability.
Description
Technical field
The present invention relates to extraction process technology field, more specifically, the superhigh pressure extracting method relating to a kind of clam worm and the extracts from Perinereis aibuhitensis prepared thereof.
Background technology
Oxidative stress (Oxidativestress) is a series of adaptive reaction that in body cell, between enzymatic oxidation composition and antioxidant content, dysequilibrium causes, the oxidative damage of oxidative stress and mediation thereof is that a basic pathology metabolic process with development occurs body different system disease, in view of oxidative stress and many chronic diseases closely related, therefore people are constantly finding the efficient antioxidant of exploitation always, but the chemical synthesis antioxidant commonly used in food has at present been proved to be has potential harm, and the natural derived from organism has higher security, and have more benefits to health, therefore, from organism, find natural safely and efficiently in recent years become study hotspot.
At present, countries in the world have developed a large amount of natural products, these products are also used widely, but these product majorities derive from terrestrial plant, as carrotene, lycopene, anthocyanidin, resveratrol, flavonoids etc., and lower to the research and development rate of the aquatic products in a large number with biologically active effect, from aquatic products, therefore find the research and development tool that the product with anti-oxidation efficacy carries out antioxidant be of great significance.
Clam worm belongs to Annelida, polychaeta animal, is a kind of nutritious, the seafood of delicious flavour, is also that a kind of dietotherapy is held concurrently excellent herbal cuisine simultaneously.The protein content of clam worm is high, and its amino acid composition is substantially complete, and containing abundant polyunsaturated fatty acid.Multinomial research shows that clam worm has very strong enriching heavy metal and the effect of other pollutants, and clam worm presents powerful antioxidation activity when heavy metal tolerance and Assessment of Organic Pollution, and therefore clam worm may be the desirable feedstock preparing edible natural antioxidant.
Clam worm is at present mainly as the important foodstuffs source of cultivating fish, shrimp, the parent of crab and fish, shrimp, crab, and in the cultivation busy season, supply falls short of demand for clam worm; But aquaculture exists seasonal, cultivating dull season, there is unsalable phenomenon in clam worm, therefore clam worm further technological processing way is urgently sought by nereis culture enterprise.
Summary of the invention
The object of the invention is to overcome the deficiency existing for clam worm deep process technology in prior art, the superhigh pressure extracting method of a kind of clam worm is provided.
Second object of the present invention is to provide the extracts from Perinereis aibuhitensis that said method prepares.
3rd object of the present invention is to provide the natural containing above-mentioned extracts from Perinereis aibuhitensis.
4th object of the present invention is to provide the application of above-mentioned extracts from Perinereis aibuhitensis as natural.
The object of the invention is to be achieved by the following technical programs:
A superhigh pressure extracting method for clam worm, be by freeze-drying after clam worm abrasive dust, be dissolved in acetone, extract at pressure 300 ~ 400MPa, temperature 10 ~ 30 DEG C after 20 ~ 40min through centrifugal, concentrate and get final product.
Clam worm selected by the present invention is that perinereis aibihitensis Grube belongs to Annelida (Annelida), encloses nereis.Polyphenoils nature is unstable, be subject to the impact of external environment and cause active reduction or disappearance, therefore extracting clam worm oxidation-resistant active ingredient needs its activity of strict protection unaffected, ultra high pressure extraction applies hydrostatic pressure rapidly to material liquid at normal temperatures, solvent rapid permeability under super-pressure effect is inner to solid material, dissolubility increases, and reaches dissolution equilibrium at short notice; Simultaneously under super-pressure effect, the structures such as cell membrane, cell membrane and intracellular fluid bubble change, and permeability increases, thus reach and extract fast and efficiently and do not destroy the object of Small molecular active ingredient physiologically active.Therefore ultra high pressure extraction technology is selected can to improve extraction efficiency as the extractive technique of clam worm polyphenoils.
Ultra high pressure extraction is widely used, but for concrete raw material, need to research and develop a set of suitable ultra high pressure extraction scheme, first clam worm is carried out freeze drying and makes powdery by the present invention, freeze drying can ensure that clam worm active ingredient is not affected by environment, also can multiple batches ofly use simultaneously, clam worm is animal body, want to extract its active ingredient, the screening of organic solvent seems particularly important, inventor is in the characteristic according to clam worm, choose the organic solvent with suitable polarity scope, and by experiment, specify that acetone as organic solvent, the high efficiency extraction of extracts from Perinereis aibuhitensis can be reached.
Preferably, described simmer down to decompression distillation concentrates, and removes organic solvent after concentrated.
Preferably, the mass volume ratio of described clam worm powder and acetone is 1g:30 ~ 50ml.
Preferably, described organic solvent is acetone.
In extracts from Perinereis aibuhitensis, total phenol content is as the index evaluating extracts from Perinereis aibuhitensis active constituent content size, and inventor by the optimal conditions of optimization ultra high pressure extraction, and has carried out response surface analysis, and result shows that ultra high pressure extraction temperature is 28.08 DEG C
,extraction pressure is 378.72MPa, extraction time, when being 20min, in extracts from Perinereis aibuhitensis, total phenol content was the highest.
The extracts from Perinereis aibuhitensis that the present invention also provides said method to obtain.
The present invention also provides the natural containing above-mentioned extracts from Perinereis aibuhitensis.
The extracts from Perinereis aibuhitensis oxidation resistance that the present invention obtains is strong, and therefore, the present invention also provides described extracts from Perinereis aibuhitensis as the application of antioxidant.
Compared with prior art, the present invention has following beneficial effect:
The invention provides the superhigh pressure extracting method of a kind of clam worm, be by freeze-drying after clam worm abrasive dust, be dissolved in acetone, extract at pressure 300 ~ 400MPa, temperature 10 ~ 30 DEG C after 20 ~ 40min through centrifugal, concentrate and get final product; The extracts from Perinereis aibuhitensis that the method obtains is thick extraction, require no purifying, direct use, find 6.25mg/mL time to DPPH clearance rate up to 87.28%, during 100mg/mL, 71.32% is reached to the clearance rate of ultra-oxygen anion free radical, reach 62.18% to the clearance rate of hydroxy radical during 250mg/mL, the extracts from Perinereis aibuhitensis obtained has splendid oxidation resistance.
Accompanying drawing explanation
Fig. 1 is the flow chart that clam worm of the present invention is extracted.
Fig. 2 is the response surface that affects total phenol content of extraction time and the reciprocation extracting pressure and contour map.
Fig. 3 is the response surface that affects total phenol content of the reciprocation of Extracting temperature and extraction time and contour map.
Fig. 4 is the response surface that affects total phenol content of Extracting temperature and the reciprocation extracting pressure and contour map.
Fig. 5 is the scavenging action of extracts from Perinereis aibuhitensis to superoxide anion.
Fig. 6 is the scavenging action of extracts from Perinereis aibuhitensis to hydroxy radical.
Detailed description of the invention
Further illustrate content of the present invention below in conjunction with Figure of description and specific embodiment, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, the simple modification do the inventive method, step or condition or replacement, all belong to scope of the present invention; If do not specialize, the conventional means that technological means used in embodiment is well known to those skilled in the art.
embodiment 1
The perinereis aibihitensis Grube selecting Zhanjiang region to cultivate is raw material, and clean freeze-drying, then grind into powder is for subsequent use, and concrete extraction operating procedure is as follows:
(1) Extraction solvent is determined: take clam worm respectively in Polythene Bag, in 1:30(quality: volume) ratio add n-hexane respectively, cyclohexane, ethyl acetate, acetone, methyl alcohol 5 kinds of organic solvents, sealing machine seals, ultra high pressure extraction condition is: 300MPa, room temperature, 20min, extract respectively with this understanding, extract the rear centrifugal supernatant obtained through decompression distillation concentrated removing organic solvent, obtain extracts from Perinereis aibuhitensis, with ethanol stripping extracts from Perinereis aibuhitensis, measure the total phenol content in each extracts from Perinereis aibuhitensis respectively, selective extraction obtains the Extraction solvent of the highest organic solvent of total phenol content as clam worm, described mass unit is gram, volume unit is milliliter.
Respectively 5 kinds of extractive with organic solvent are carried out to the mensuration (using gallic acid as content criterion) of polyphenoils-total phenol content with Folin-Ciocalteu colorimetric method.Result shows, the content of polyphenoils in n-hexane, cyclohexane, ethyl acetate, acetone, methyl alcohol 5 kinds of extractive with organic solvent-total phenol is 3.39,3.61,4.22,6.09 and 5.04mg gallic acid equivalant/g clam worm dry product respectively, illustrates that to utilize acetone the highest as the extracts from Perinereis aibuhitensis polyphenoils-total phenol content of Extraction solvent.
Also the TAC of the extracts from Perinereis aibuhitensis that 5 kinds of organic solvents obtain is detected simultaneously, adopt ammonium phosphomolybdate-ultraviolet spectrophotometry, the change of its absorbance and the content of reducing substances are proportionate relationship, can according to the power of absorbance size calculation sample reducing power.Result shows, n-hexane, cyclohexane, ethyl acetate, acetone, methyl alcohol 5 kinds of extractive with organic solvent (1mg/mL) TAC when same concentrations are equivalent to 0.585,0.615,0.783,1.053,0.534 gallic acid concentration (mg/g) respectively, illustrate that the oxidation resistance of the extracts from Perinereis aibuhitensis that acetone extraction obtains is the strongest.
(2) optimization of ultra high pressure extraction condition:
1. the determination of solid-liquid ratio (ratio of clam worm quality and Extraction solvent volume): using acetone as Extraction solvent, respectively at 1:10, 1:20, 1:30, 1:40, ultra high pressure extraction is carried out under the solid-liquid ratio of 1:50, ultra high pressure extraction condition is: 300MPa, room temperature, 20min, extract the rear centrifugal supernatant obtained through decompression distillation concentrated removing organic solvent, obtain different feed liquid than under extracts from Perinereis aibuhitensis, with ethanol stripping extracts from Perinereis aibuhitensis, measure the total phenol content of different feed liquid than lower extracts from Perinereis aibuhitensis respectively, found that: be before 1:40 at solid-liquid ratio, along with the increase of solid-liquid ratio, total phenol content and the TAC of extract increase all gradually, be that 1:40 reaches maximum at solid-liquid ratio, when being 1:50 to solid-liquid ratio, total phenol content and TAC decline, visible solid-liquid ratio is that the extract total phenol content of 1:40 is the highest, determines that solid-liquid ratio 1:40 is as the solid-liquid ratio extracting clam worm antioxidant content.
2. the determination of ultra high pressure extraction pressure: using acetone as Extraction solvent, solid-liquid ratio 1:40, Extracting temperature: under the condition of room temperature, extraction time: 20min, clam worm antioxidant content is extracted respectively under ultra high pressure 50MPa, 100MPa, 150MPa, 200MPa, 250MPa, 300MPa, 350MPa, 400MPa, 450MPa, 500MPa, measure the total phenol content of the extracts from Perinereis aibuhitensis under each pressure, total phenol content when wherein pressure is 350MPa is the highest, determines that pressure 350MPa is the extraction pressure extracting clam worm antioxidant content.
3. the determination of Extracting temperature: using acetone as Extraction solvent, solid-liquid ratio 1:40, extract pressure: 350MPa, under the condition of extraction time: 20min, clam worm antioxidant content is extracted respectively at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, at 10 ~ 50 DEG C the total phenol content of extracts from Perinereis aibuhitensis be 7.62 respectively, 8.04,7.44,7.20,7.31 gallic acid equivalants/g clam worm dry product, the total phenol content of 20 DEG C of extracts from Perinereis aibuhitensis is apparently higher than the extracts from Perinereis aibuhitensis of other temperature; At 10 ~ 50 DEG C, the TAC of extracts from Perinereis aibuhitensis is 1.564,1.688,1.672,1.645,1.691 gallic acid concentration (mg/g) respectively, the TAC of 50 DEG C of extracts from Perinereis aibuhitensis is a little more than the extracts from Perinereis aibuhitensis of 20 DEG C, the total phenol content of comprehensive extracts from Perinereis aibuhitensis and TAC result, determine that temperature 20 DEG C is extract the Extracting temperature of clam worm antioxidant content.
4. the determination of extraction time: using acetone as Extraction solvent, solid-liquid ratio 1:40, Extracting temperature: under the condition of 20 DEG C, clam worm antioxidant content is extracted respectively under extraction time 5min, 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, measure the total phenol content of the extracts from Perinereis aibuhitensis under each extraction time, total phenol content when wherein extraction time is 30min and TAC all the highest, determine that extraction time 30min is the extraction time of extracting clam worm antioxidant content.
(3) Bekmen response surface experiment: using the extraction pressure of experiment of single factor optimization, extraction time, Extracting temperature as independent variable, total phenol content is as dependent variable, carry out the experiment of Bekmen response surface, finally obtain the optimal conditions that clam worm antioxidant content extracts.
Selective extraction temperature 10,20,30 DEG C, extract pressure 300,350,400MPa, extraction time 20,30,40min, carry out the Bekmen response surface experiment of Three factors-levels, experimental result as shown in figs. 2 to 4, time and temperature are conspicuousness impact on total phenol content, and wherein temperature is pole conspicuousness impact on total phenol content, and pressure affects without conspicuousness total phenol content; The reciprocation of time and pressure is pole conspicuousness impact on total phenol content, and the reciprocation of pressure and temperature is pole conspicuousness impact on total phenol content, and the reciprocation of time and temperature affects without conspicuousness total phenol content.The extraction conditions selecting optimization according to response surface result finishing screen is: Extracting temperature 28.08 DEG C
,extract pressure 378.72MPa, extraction time 20min.
Extracting temperature 28.08 DEG C
,the extraction of three clam worm polyphenoils is carried out under extracting the condition of pressure 378.72MPa, extraction time 20min, the total phenol content of three extracts is respectively 8.365 gallic acid equivalants/g clam worm dry product, 8.41 gallic acid equivalants/g clam worm dry product, 8.385 gallic acid equivalants/g clam worm dry product, only differ 0.06% ~ 0.60% with the total phenol content 8.360 predicted under optimal conditions, optimum results is credible.
embodiment 2
The extracts from Perinereis aibuhitensis of ultra high pressure extraction under extraction conditions is optimized in Example 1, the TAC of extracts from Perinereis aibuhitensis when concentration is (1mg/mL) extracted under this optimal conditions for three times is respectively 17.40,17.61,17.58 gallic acid equivalants (ug/mL), DPPH Scavenging activity increases along with extract concentrations, it is 37.65% that clearance rate increases the inhibiting rate when 1.25mg/mL gradually, when 3.75mg/mL, inhibiting rate rises to 68.40%, 87.28%, IC is reached when 6.25mg/mL
50for 2.00(mg/mL).
embodiment 3
Optimize the extracts from Perinereis aibuhitensis of ultra high pressure extraction under extraction conditions in Example 1, adopt mouse thymus cells-spectrophotometry extracts from Perinereis aibuhitensis to ultra-oxygen anion free radical scavenging action (using Vc as positive control) (Fig. 5).Ultra-oxygen anion free radical is first free radical in active oxygen radical chain, and can generate other oxygen radical through series reaction, be the free radical that in human body, the life-span is longer, harmfulness is large.Therefore, antioxidation activity evaluation is also usually used in.Result shows, extracts from Perinereis aibuhitensis can reduce the autoxidation speed of pyrogallol, and along with extract concentrations increase, clearance rate increases gradually.During low concentration (10mg/L), the Scavenging activity of extracts from Perinereis aibuhitensis to ultra-oxygen anion free radical is lower, the clearance rate of ultra-oxygen anion free radical only has 11.08%, but along with extracts from Perinereis aibuhitensis concentration increases, it is very fast to the Scavenging activity amplification of ultra-oxygen anion free radical, during high concentration (100mg/L), the clearance rate of extracts from Perinereis aibuhitensis to ultra-oxygen anion free radical reaches 71.32%, IC
50for 39.29mg/L.
embodiment 4
Optimize the extracts from Perinereis aibuhitensis of ultra high pressure extraction under extraction conditions in Example 1, adopt Phen-spectrophotometry extracts from Perinereis aibuhitensis to hydroxy radical scavenging action (using Vc as positive control) (Fig. 6).Result shows, along with extract concentrations increases, the clearance rate of hydroxy radical increases gradually.During low concentration (50mg/L), the Scavenging activity of extracts from Perinereis aibuhitensis to hydroxy radical is lower, the clearance rate of hydroxy radical only has 12.36%, but along with extracts from Perinereis aibuhitensis concentration increases, the Scavenging activity amplification of extracts from Perinereis aibuhitensis to hydroxy radical is very fast, during high concentration (250mg/L), the clearance rate of extracts from Perinereis aibuhitensis to hydroxy radical reaches 62.18%.
Claims (7)
1. a superhigh pressure extracting method for clam worm, is characterized in that, by the clam worm abrasive dust after freeze-drying, is dissolved in organic solvent, extract at pressure 300 ~ 400MPa, temperature 10 ~ 30 DEG C after 20 ~ 40min through centrifugal, concentrate and get final product; Described organic solvent is n-hexane, cyclohexane, ethyl acetate, acetone or methyl alcohol.
2. superhigh pressure extracting method according to claim 1, is characterized in that, described organic solvent is acetone.
3. superhigh pressure extracting method according to claim 1, is characterized in that, the mass volume ratio of described clam worm powder and acetone is 1g:30 ~ 50ml.
4. superhigh pressure extracting method according to claim 1, is characterized in that, described ultra high pressure extraction temperature is 28.08 DEG C
,extraction pressure is 378.72MPa, extraction time is 20min.
5. the extracts from Perinereis aibuhitensis of method acquisition described in any one of Claims 1-4.
6. the natural containing extracts from Perinereis aibuhitensis described in claim 5.
7. extracts from Perinereis aibuhitensis described in claim 5 is as the application of antioxidant.
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