CN102776298B - Extractive of apple pomace fructose - Google Patents
Extractive of apple pomace fructose Download PDFInfo
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- CN102776298B CN102776298B CN 201210281547 CN201210281547A CN102776298B CN 102776298 B CN102776298 B CN 102776298B CN 201210281547 CN201210281547 CN 201210281547 CN 201210281547 A CN201210281547 A CN 201210281547A CN 102776298 B CN102776298 B CN 102776298B
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- fructose
- apple residue
- countercurrent extraction
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- leaching
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Abstract
The invention discloses extractive of apple pomace fructose. The extractive is prepared by a countercurrent extraction method which comprises the following steps of (1) boiling apple pomace through water at the temperature of 85-90 DEG C for 10 minutes, smashing the apple pomace in the liquid state, and drying at the low temperature; and (2) adding ethanol water with the PH of 1.0-3.0 and the mass fraction of 65-85%, performing countercurrent extraction at the temperature of 30-60 DEG C for 4-6 hours, filtering, mixing and collecting filtrate, and concentrating to obtain the extractive of the apple pomace fructose. By means of the countercurrent extraction method, anthocyanin components can be fully extracted. Compared with the prior art, the countercurrent extraction method has the advantages of saving solvent and being high in extraction efficiency, low in cost and the like, and is suitable for industrial production.
Description
Technical field
The present invention relates to the technical field that effective ingredients in plant extracts, particularly a kind of apple residue fructose extract.
Background technology
Fructose has another name called sinistrose, is a kind of common natural sugar, the integral part of Chang Zuowei diet.It is separated from sucrose at first, and abundant content is all arranged in various fruit and the plant.For example approximately contain 40% fructose in honey, cherry, banana, pears, apple and glucose etc. then contain 5-7%.Fructose is nutritive carbohydrate, do not increase the digestion burden of stomach, be delivered to liver through intestinal absorption by arterial circulation, do not increase blood glucose value, therefore it is very suitable that diabetic subject, baby, gravid woman, the elderly and the administration of patient's Postoperative Intravenous are supplemented the nutrients.Fructose is a kind of monose, is generally thick liquid, soluble in water, ethanol and ether, and the extracting method of fructose has multiplely in the prior art, technique is loaded down with trivial details, process is complicated, the high in cost of production problem but all exist.
Summary of the invention
Technical problem to be solved of the present invention provides a kind of apple residue fructose extract, the present invention uses the fructose in the counter-current extraction apple residue, it can extract the fructose composition more fully, compare the characteristics such as have the solvent of saving, extraction efficiency is high, cost is low with art methods, be suitable for suitability for industrialized production.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of apple residue fructose extract, and standby the obtaining of employing countercurrent extraction legal system, described countercurrent extraction method may further comprise the steps:
Step (1): with apple residue 85-90 ℃ of poach 10min, liquid grinding, cryodrying; With
Step (2): the adding pH value is that 1.0-3.0, massfraction are the aqueous ethanolic solution of 65-85%, and 30-60 ℃ of lower countercurrent extraction 4-6h merges after filtering and collect filtrate, and be concentrated, gets apple residue fructose extract.
Further, in described step (2), add pH value and be 1.0, massfraction is 75% aqueous ethanolic solution, 40 ℃ of lower countercurrent extraction 6 hours.
Further, the fructose content of described apple residue fructose extract is 7.92% ~ 8.17%.
" concentrating " described herein is concentrated for cryogenic vacuum, and its temperature is controlled at 10 ~ 20 ℃.Concentrated degree is: make the solid content of the final apple residue fructose extract of gained be controlled at 0.4% ~ 1% of its weight.
The present invention compared with prior art has following advantage:
(1) China is apple production and processing big country, the a large amount of apple residue of annual generation, utilization contain the abundant apple residue of fructose and make raw material production fructose, have important productive value, therefore the present invention extracts fructose from apple residue, can improve the utility value that fructose output can improve again apple residue.
(2) the present invention adopts the countercurrent extraction method, can extract the anthocyanogen composition more fully, compares with art methods to have the characteristics such as save solvent, extraction efficiency is high, cost is low, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the mass percent (%) of ethanol and the graph of a relation of leach liquor fructose content (g).
Fig. 2 is the graph of a relation of duration of contact (h) and leach liquor fructose content (g).
Fig. 3 be temperature (℃) with the graph of a relation of leach liquor fructose content (g).
Fig. 4 is the schematic diagram of the device of a kind of apple residue fructose of the present invention method for preparing extractive use.
Embodiment
One, the extraction process condition is investigated
1, leaching condition experiment
(1) the ethanol mass percent is on the impact of fructose compound leaching effect
In the industrial production, owing to often containing certain moisture in the raw material, ethanol also contains certain moisture after recycling, there is very large impact in the ethanol mass percent to the leaching of fructose compound, therefore with different mass percentage ratio aqueous ethanolic solution the fructose material is carried out leaching experiment, with the fructose content trace analysis.In the ethanol mass percent is tested the impact of leaching fructose from raw material, get respectively 5 parts of raw materials, every part of 50.00g, test, take different mass percentage ratio, pH value each 200.00ml of aqueous ethanolic solution as 1.0, lixiviate 6h, compare the amount of gained fructose, its result as shown in Figure 1.
As shown in Figure 1, under the same terms, leaching ability power is followed successively by 75%〉80%〉70%〉85%〉65%, therefore, select 75% aqueous ethanolic solution as leaching agent.
(2) duration of contact is on the impact of fructose compound leaching effect
Get respectively 6 parts of raw materials, every part of 50.00g, each adds, and mass percent is 75%, pH value is that 1.0 aqueous ethanolic solution 200.00ml leaches, and is respectively 1h duration of contact, 2h, 3h, 4h, 5h, 6h, it leaches the result as shown in Figure 2.
As shown in Figure 2, under the room temperature (26 ℃), extraction time is 6h, and Leaching reaction reaches balance substantially; Prolong extraction time, leaching yield is substantially constant.
(3) temperature is on the impact of fructose compound leaching effect
Get respectively 6 parts of raw material powders, every part of 50.00g, each adds, and the 200.00ml mass percent is 75%, pH value is 1.0 aqueous ethanolic solution, under different temperature, leach, extraction time is 2h, and sampling detects apple residue fructose content in the leach liquor, and the result as shown in Figure 3.
As shown in Figure 3, along with the increase of extraction temperature, the leaching yield of fructose also increases accordingly; When temperature reaches 40 ℃, increase temperature, the leaching yield increase of fructose is tending towards slow.
2, four sections adverse current percolations (process diagram is seen Fig. 4)
6 ф 25.4mm * 1000mm glass have been installed have altogether been drawn together a mouthful pipe, as the leacher (leaching post) of four sections adverse current diacolation leaching experiments, wherein four operations are done the week conversion for two.The 150.00g apple residue raw material powder of packing in every post particle (be called for short raw material, as follows), with volume pump with leaching agent (65-85% aqueous ethanolic solution), with about 5mlmin
-1Flow squeeze in first leaching post, 65-85% is with about 1cmmin
-1The speed diacolation after the first post flows out the 450ml leach liquor, is connected the first post and the second post.The new leaching agent that volume pump is squeezed into is through the first post, and outflow enters the second post; With upper identical, after the second post flows out 450ml black leach liquor, the second post and the 3rd post are connected.The rest may be inferred, after the 4th post flows out the 450ml effluent liquid by the time, the 4th post and the 5th post connected.Simultaneously, the volume pump outlet pipe is moved to the second post upper end from the first post upper end and connect (the first post is withdrawn from) with the second post from system.At this moment, new leaching agent advances the second post through volume pump, behind three, four, five posts, flows out from the 5th post, gets equally the 450ml leach liquor; After this, new leaching agent advances the 3rd post, goes out leach liquor from the 6th post.The rest may be inferred, constantly loops four sections adverse current diacolation leaching experiments to reaching the leaching balance.The 9th post begins to end to the 12 post in this test, the leach liquor that these four posts flow out is the leach liquor during approximate equilibrium, thus when new leaching agent from advancing from the 9th post, through ten, 11,12 posts, and after flowing out 450ml black leach liquor under the 12 post, stop leaching test.With the leach liquor sampling that nine, ten, 11,12 posts flow out, censorship, the content of mensuration fructose.(annotate: cylinder is and recycles, and nine, ten, 11,12 only represent label, do not have practical significance)
3, four sections adverse current diacolation leaching test results
Counter-current described above is tested.Every duplicate samples is 150.0g, take 75% aqueous ethanolic solution as leach liquor, and 40 ℃ of lower lixiviate 6h, liquid-solid ratio is 5.Get the leach liquor of nine, ten, 11,12 posts outflow and measure, its result is as shown in table 1.
Four sections adverse current diacolations of table 1 leaching test result
As known from Table 1, fructose content is in 6% in the apple residue, and then its leaching yield of four sections adverse current diacolation lixiviation process (in leach liquor) reaches 95.0%.
Detection method:
The fructose content measuring method adopts determined by ultraviolet spectrophotometry, and concrete measuring method is referring to accounting for the content [J] that reaches eastern Fructose in Fruit Juice based on UV-Photometric Method, fine jade state college journal, and 2003,10(2): 23-27
Two, embodiment: following by specific embodiment, the present invention is described in further detail.
Embodiment 1:
Get apple residue 500g, 85 ℃ of poach 10min, liquid grinding, cryodrying adds pH value and is 3.0, massfraction is 65% ethanolic soln 2.5L, and 30 ℃ of lower countercurrent extraction 4h merge after filtering and collect filtrate, and are concentrated, get apple residue fructose extract 105.78g.Measure the fructose content in the described apple residue fructose extract, its fructose content is 8.17%.Fructose content is in 6% in the apple residue, and then its leaching yield of four sections adverse current diacolation lixiviation process (in leach liquor) reaches 96.02%.
Described " concentrating " is concentrated for cryogenic vacuum, and its temperature is controlled at 15 ℃.Concentrated degree is: make the solid content of the final apple residue fructose extract of gained be controlled at 0.4% of its weight.
Embodiment 2:
Get apple residue 500g, 90 ℃ of poach 10min, liquid grinding, cryodrying adds pH value and is 1.0, massfraction is 75% ethanolic soln 2.5L, and 40 ℃ of lower countercurrent extraction 6h merge after filtering and collect filtrate, and are concentrated, get apple residue fructose extract 108.34g.Measure the fructose content in the described apple residue fructose extract, its fructose content is 7.92%.Fructose content is in 6% in the apple residue, and then its leaching yield of four sections adverse current diacolation lixiviation process (in leach liquor) reaches 95.34%.
Described " concentrating " is concentrated for cryogenic vacuum, and its temperature is controlled at 10 ℃.Concentrated degree is: make the solid content of the final apple residue fructose extract of gained be controlled at 0.5% of its weight.
Embodiment 3:
Get apple residue 500g, 90 ℃ of poach 10min, liquid grinding, cryodrying adds pH value and is 1.0, massfraction is 85% ethanolic soln 2.5L, and 60 ℃ of lower countercurrent extraction 6h merge after filtering and collect filtrate, and are concentrated, get apple residue fructose extract 106.11g.Measure the fructose content in the described apple residue fructose extract, its fructose content is 8.04%.Fructose content is in 6% in the apple residue, and then its leaching yield of four sections adverse current diacolation lixiviation process (in leach liquor) reaches 94.79%.
Described " concentrating " is concentrated for cryogenic vacuum, and its temperature is controlled at 20 ℃.Concentrated degree is: make the solid content of the final apple residue fructose extract of gained be controlled at 0.8% of its weight.
As mentioned above, just can realize preferably the present invention.
Claims (1)
1. an apple residue fructose extract is characterized in that, standby the obtaining of employing countercurrent extraction legal system, and described countercurrent extraction method may further comprise the steps:
Step (1): with apple residue 85-90 ℃ of poach 10min, liquid grinding, cryodrying; With
Step (2): add pH value and be 1.0, massfraction is 75% aqueous ethanolic solution, merges and collects filtrate, and is concentrated, gets apple residue fructose extract after 40 ℃ of lower countercurrent extraction were filtered in 6 hours;
The fructose content of described apple residue fructose extract is 7.92% ~ 8.17%.
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