CN104605284A - Preparation method for cranberry pomace polyphenol extract - Google Patents
Preparation method for cranberry pomace polyphenol extract Download PDFInfo
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- CN104605284A CN104605284A CN201510078483.1A CN201510078483A CN104605284A CN 104605284 A CN104605284 A CN 104605284A CN 201510078483 A CN201510078483 A CN 201510078483A CN 104605284 A CN104605284 A CN 104605284A
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Abstract
The invention discloses a preparation method for a cranberry pomace polyphenol extract. The preparation method comprises the following steps: step (1), squeezing fresh cranberry fruits, separating pomace from juice, preparing to obtain cranberry pomace, and drying the cranberry pomace at a low temperature; step (2), adding water in the pomace dried at the low temperature in the step (1), with the material-water ratio of the pomace to the water being (1 to 5)-(1 to 10)(g/ml), ultrasonically extracting for 15 minutes by virtue of an ultrasonic wave with the power of 1.8-2.0KW, and filtering to obtain a cranberry extract; step (3), carrying out the first-stage ultrafiltration; step (4), carrying out the second-stage ultrafiltration; step (5), carrying out the third-stage ultrafiltration; and step (6), drying in a vacuum, and then preparing the cranberry pomace polyphenol extract. The purity of polyphenol in the extract prepared by adopting the method disclosed by the invention is high and can be up to 8-12.2%; moreover, the method disclosed by the invention is especially suitable for industrialized production.
Description
Technical field
The present invention relates to effective ingredients in plant extractive technique, particularly a kind of preparation method of Cranberry pomace polyphenol extract.
Background technology
Cranberry, also known as mossberry, cranberry, european cranberry, English name (Cranberry), its title derives from former title " the crane certain kind of berries ", and the flower because of Cranberry resembles the head of crane and mouth and gains the name very much.Be being commonly called as of Ericaceae Vaccinium crowberry subgenus (formal name used at school: Oxycoccos having another name called littlefruit craneberry subgenus), the species of this subgenus are evergreen shrubs, in primary growth nice and cool area acid peat soil earth on the Northern Hemisphere.Flower rediance, raceme.Red fruit can cook fruit and eat.Current some areas in North America are by a large amount of plantations.The fruit of results is used for making fruit juice, jam etc.Cranberry sauce (cranberrysauce) is the traditional proportioning of U.S. entree in Thanksgiving Day turkey.Because the tart flavour of Cranberry itself is comparatively strong, as generally converting the sweeter composition such as syrup or cider in the fruit juice of beverage.Cranberry is a kind of natural antibacterial health fruit, is the best nature food therapy of preventing and treating the various bacteriological infection of the daily urinary system of women, urethritis, cystitis, chronic nephropyelitis.Cranberry is the crops that can grow in acid earth few in number, and they need a large amount of water.Once branches and tendrils start growth, it is by many for continued propagation years.Some branches and tendrils can grow 75 to 100 years just can result.
Though Cranberry originates in North America, cultivate successfully in China at present, its industrialization plantation is within sight; Also there are the natural resources of other huckleberry plants in China in addition, and therefore from huckleberry plant, especially extracting polyphenol in Cranberry has wide market prospects.
Therefore, exploitation is needed to be suitable for the preparation method of the Cranberry pomace polyphenol extract of industrial applications.
Summary of the invention
Technical problem to be solved of the present invention is to provide a kind of preparation method of Cranberry pomace polyphenol extract, the present invention adopts ultrasonic extraction to carry out Isolation and purification in conjunction with three grades of Ultra filtration membrane methods to Cranberry pomace, prepares Cranberry pomace polyphenol extract; The inventive method preparation method is suitable for suitability for industrialized production, and in the extract obtained, polyphenol purity is higher, and purity reaches 8% ~ 12.2%.
The present invention solves the problems of the technologies described above adopted technical scheme:
A preparation method for Cranberry pomace polyphenol extract, comprises the following steps:
Step (1), get Cranberry fresh fruit and squeeze, make pomace and fruit juice separating; Prepare Cranberry pomace; And by the low temperature drying of described Cranberry pomace;
Water is added in step (2), pomace after described step (1) low temperature drying, the solid-liquid ratio of described pomace and described water is 1:5-1:10 (g/ml), utilize the ultrasonic wave that power is 1.8KW-2.0KW, ultrasonic extraction 15 minutes, filter, obtain Cranberry extract;
Step (3), one-level ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 100000Da to carry out one-level ultra-filtration and separation to the Cranberry extract that described step (2) prepares, obtain filtrate I, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (4), two-stage ultrafiltering: use the hollow fiber form milipore filter that molecular cut off is 10000Da to carry out two-stage ultrafiltering separation to the filtrate I that described step (3) obtains, obtain filtrate I I, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (5), three grades of ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 1500Da to carry out three grades of ultra-filtration and separation to the filtrate I I that described step (4) obtains, obtain filtrate I II, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (6), described filtrate I II to be concentrated, after vacuum drying, namely prepare Cranberry pomace polyphenol extract of the present invention.
In described step (2), the solid-liquid ratio of described pomace and described water is 1:5 (g/ml);
In described step (3), described ultra-filtration conditions is: pressure 0.1Mpa, temperature 35 DEG C; Membrane flux is 350 ls/h;
In described step (4), described ultra-filtration conditions is: pressure 0.3Mpa, temperature 35 DEG C; Membrane flux is 300 ls/h;
In described step (5), described ultra-filtration conditions is: pressure 0.5Mpa, temperature 35 DEG C; Membrane flux is 250 ls/h.
" squeezing " of the present invention refers to and adopts squeezer of the prior art or juice extractor to carry out mechanical expression.
Compared with prior art, tool has the following advantages in the present invention:
(1) the present invention adopts ultrasonic extraction in conjunction with three grades of Ultra filtration membrane methods, can extract the polyphenol component in Cranberry more fully, there is the features such as Feedstock treating is more prone to, extraction efficiency is high, cost is low compared with art methods, and be more suitable for suitability for industrialized production.
(2) the inventive method not only increases the stability of polyphenol in leaching process, and improves the purity of polyphenol in final extract.
(3) in the extract for preparing of the inventive method, polyphenol purity is higher, and purity reaches 8% ~ 12.2%.
(4) the inventive method improves extraction efficiency, shortens extraction time.
(5) solvent of the present invention only needs water, does not need extra organic solvent, more environmental protection.
Detailed description of the invention
Below by way of specific embodiment, the present invention is described in further detail.
Embodiment 1:
Step (1), get 10kg Cranberry fresh fruit and squeeze, make pomace and fruit juice separating; Obtain Cranberry pomace; And by the low temperature drying of described Cranberry pomace; Described low temperature drying refers to and is being no more than drying at the temperature of 30 DEG C;
Water is added in step (2), pomace after described step (1) low temperature drying, the solid-liquid ratio of the pomace after described low temperature drying and described water is 1:8 (g/ml, namely the ratio of 8ml water is added in 1g pomace), utilize the ultrasonic wave that power is 1.8KW, ultrasonic extraction 15 minutes, filter, obtain Cranberry extract;
Step (3), one-level ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 100000Da to carry out one-level ultra-filtration and separation to the Cranberry extract that described step (2) prepares, obtain filtrate I, ultra-filtration conditions: pressure 0.1Mpa, temperature 35 DEG C; Membrane flux is 350 ls/h;
Step (4), two-stage ultrafiltering: use the hollow fiber form milipore filter that molecular cut off is 10000Da to carry out two-stage ultrafiltering separation to the filtrate I that described step (3) obtains, obtain filtrate I I, ultra-filtration conditions: pressure 0.3Mpa, temperature 35 DEG C; Membrane flux is 300 ls/h;
Step (5), three grades of ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 1500Da to carry out three grades of ultra-filtration and separation to the filtrate I I that described step (4) obtains, obtain filtrate I II, ultra-filtration conditions: pressure 0.5Mpa, temperature 35 DEG C; Membrane flux is 250 ls/h;
Step (6), described filtrate I II is concentrated into proportion 10 (B measurement), after 35 DEG C of vacuum drying, obtains 2.2kg extract, i.e. Cranberry pomace polyphenol extract of the present invention.
Measure through HPLC, in final Cranberry pomace polyphenol extract, the purity of polyphenol is 9.1%.
Embodiment 2:
Step (1), get 10kg Cranberry fresh fruit and squeeze, make pomace and fruit juice separating; Obtain Cranberry pomace; And by the low temperature drying of described Cranberry pomace; Described low temperature drying refers to and is being no more than drying at the temperature of 30 DEG C;
Water is added in step (2), pomace after described step (1) low temperature drying, the solid-liquid ratio of the pomace after described low temperature drying and described water is 1:5 (g/ml, namely the ratio of 5ml water is added in 1g pomace), utilize the ultrasonic wave that power is 1.9KW, ultrasonic extraction 15 minutes, filter, obtain Cranberry extract;
Step (3), one-level ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 100000Da to carry out one-level ultra-filtration and separation to the Cranberry extract that described step (2) prepares, obtain filtrate I, ultra-filtration conditions: pressure 0.1Mpa, temperature 35 DEG C; Membrane flux is 350 ls/h;
Step (4), two-stage ultrafiltering: use the hollow fiber form milipore filter that molecular cut off is 10000Da to carry out two-stage ultrafiltering separation to the filtrate I that described step (3) obtains, obtain filtrate I I, ultra-filtration conditions: pressure 0.3Mpa, temperature 35 DEG C; Membrane flux is 300 ls/h;
Step (5), three grades of ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 1500Da to carry out three grades of ultra-filtration and separation to the filtrate I I that described step (4) obtains, obtain filtrate I II, ultra-filtration conditions: pressure 0.5Mpa, temperature 35 DEG C; Membrane flux is 250 ls/h;
Step (6), described filtrate I II is concentrated into proportion 10 (B measurement), after 35 DEG C of vacuum drying, obtains 2.15kg extract, i.e. Cranberry pomace polyphenol extract of the present invention.
Measure through HPLC, in final Cranberry pomace polyphenol extract, the purity of polyphenol is 8.5%.
Embodiment 3:
Step (1), get 10kg Cranberry fresh fruit and squeeze, make pomace and fruit juice separating; Obtain Cranberry pomace; And by the low temperature drying of described Cranberry pomace; Described low temperature drying refers to and is being no more than drying at the temperature of 30 DEG C;
Water is added in step (2), pomace after described step (1) low temperature drying, the solid-liquid ratio of the pomace after described low temperature drying and described water is 1:10 (g/ml, namely the ratio of 10ml water is added in 1g pomace), utilize the ultrasonic wave that power is 2.0KW, ultrasonic extraction 15 minutes, filter, obtain Cranberry extract;
Step (3), one-level ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 100000Da to carry out one-level ultra-filtration and separation to the Cranberry extract that described step (2) prepares, obtain filtrate I, ultra-filtration conditions: pressure 0.1Mpa, temperature 35 DEG C; Membrane flux is 350 ls/h;
Step (4), two-stage ultrafiltering: use the hollow fiber form milipore filter that molecular cut off is 10000Da to carry out two-stage ultrafiltering separation to the filtrate I that described step (3) obtains, obtain filtrate I I, ultra-filtration conditions: pressure 0.3Mpa, temperature 35 DEG C; Membrane flux is 300 ls/h;
Step (5), three grades of ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 1500Da to carry out three grades of ultra-filtration and separation to the filtrate I I that described step (4) obtains, obtain filtrate I II, ultra-filtration conditions: pressure 0.5Mpa, temperature 35 DEG C; Membrane flux is 250 ls/h;
Step (6), described filtrate I II is concentrated into proportion 10 (B measurement), after 35 DEG C of vacuum drying, obtains 2.25kg extract, i.e. Cranberry pomace polyphenol extract of the present invention.
Measure through HPLC, in final Cranberry pomace polyphenol extract, the purity of polyphenol is 12.2%.
As mentioned above, just the present invention can be realized preferably.
Claims (2)
1. a preparation method for Cranberry pomace polyphenol extract, is characterized in that, comprises the following steps:
Step (1), get Cranberry fresh fruit and squeeze, make pomace and fruit juice separating; Prepare Cranberry pomace; And by the low temperature drying of described Cranberry pomace;
Water is added in step (2), pomace after described step (1) low temperature drying, the solid-liquid ratio of described pomace and described water is 1:5-1:10 (g/ml), utilize the ultrasonic wave that power is 1.8KW-2.0KW, ultrasonic extraction 15 minutes, filter, obtain Cranberry extract;
Step (3), one-level ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 100000Da to carry out one-level ultra-filtration and separation to the Cranberry extract that described step (2) prepares, obtain filtrate I, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (4), two-stage ultrafiltering: use the hollow fiber form milipore filter that molecular cut off is 10000Da to carry out two-stage ultrafiltering separation to the filtrate I that described step (3) obtains, obtain filtrate I I, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (5), three grades of ultrafiltration: use the hollow fiber form milipore filter that molecular cut off is 1500Da to carry out three grades of ultra-filtration and separation to the filtrate I I that described step (4) obtains, obtain filtrate I II, ultra-filtration conditions: pressure 0.1 ~ 0.6Mpa, temperature 35 ~ 55 DEG C; Membrane flux is 250 ~ 350 ls/h;
Step (6), described filtrate I II to be concentrated, after vacuum drying, namely prepare Cranberry pomace polyphenol extract of the present invention.
2. the preparation method of a kind of Cranberry pomace polyphenol extract as claimed in claim 1, is characterized in that, in described step (2), the solid-liquid ratio of described pomace and described water is 1:5 (g/ml);
In described step (3), described ultra-filtration conditions is: pressure 0.1Mpa, temperature 35 DEG C; Membrane flux is 350 ls/h;
In described step (4), described ultra-filtration conditions is: pressure 0.3Mpa, temperature 35 DEG C; Membrane flux is 300 ls/h;
In described step (5), described ultra-filtration conditions is: pressure 0.5Mpa, temperature 35 DEG C; Membrane flux is 250 ls/h.
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