CN101648980A - Method for combined preparation of pineapple polyphenol and juice by taking pineapple peel as main material and application thereof - Google Patents
Method for combined preparation of pineapple polyphenol and juice by taking pineapple peel as main material and application thereof Download PDFInfo
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Abstract
The invention discloses a method for combined preparation of pineapple polyphenol and juice by taking pineapple peel as main material and application thereof. The method includes that pineapple peel is cleaned, pressed and separated, so as to respectively obtain pineapple peel slag and pineapple peel juice; the pineapple peel juice is subject to macroporous resin column absorption, powered activated carbon absorption, filtering and the like, so as to obtain clear juice with extremely low clear and brown stain degree; the pineapple peel slag is subject to alcohol digestion, vacuum concentration, dilution, macroporous resin column absorption and the like, so that pineapple polyphenol can be absorbed into the macroporous resin; the macroporous resin column used for absorbing polyphenol substance in the pineapple peel juice and pineapple peel slag digestion solution is eluted by alcohol solution, the elution is subject to methylene dichloride extraction, ethyl acetate extraction, concentrated drying and the like, so that pineapple polyphenol with purity more than 90% can be obtained and extraction ratio is more than 2.5g/kg. The invention has the characteristics of easy industrializedproduction, high yield, high production purity, obvious co-production economic benefit and has important significance on promoting recycling economy development.
Description
Technical field
The invention belongs to the comprehensive utilization technique field of food-processing industry, particularly a kind of is that raw material is united the method and the application thereof of producing pineapple polyphenol and fruit juice with the pineapple peel.
Background technology
Pineapple is one of the torrid zone, semi-tropical four your name fruit, China's pineapple output is above 1,500,000 tons, its converted products mainly contains can, common fruit juice and fruit juice concentrate etc., and tankage such as the pericarp that produces in the course of processing account for 40～60% of full fruit, and visible China pineapple peel resource is very abundant.The nutritive ingredient of pineapple peel and the basal component of pulp are approaching, and the sugar that contains is generally 50～100g/kg, and contain comparatively rich organic acid, amino acid, vitamin B group, C vitamin and polyphenol substance etc., have great exploitation and are worth.If these tankage are not used, will cause the wasting of resources and environmental pollution, thereby the comprehensive utilization of pineapple peel is significant.
The pineapple polyphenol belongs to plant polyphenol, is important secondary metabolite in the pineapple peel, is the general name that has a plurality of hydroxyl phenolic compounds in the molecule.As other plant polyphenol, the pineapple polyphenol has physiologically active such as remove superfluous free radical in the body, antibacterial, antiviral, antitumor, radioprotective, antifatigue, lipopenicillinase, lose weight, delay senility, to preventing that vitamin C deficiency, inhibition atherosclerosis, enhancing capillary vessel toughness and perviousness, treatment cardiovascular and cerebrovascular diseases, removing halitosis etc. from having certain effect, can be widely used in fields such as food, medicine, fine chemistry industries.Plant polyphenol is one of research focus of domestic and international natural product, and is comparatively general about the research that plant polyphenols such as tealeaves, apple, grape, persimmon are produced, but the document that relevant pineapple polyphenol is produced is few.Though can use for reference the preparation method of other plant polyphenol, but pineapple peel ingredient and other plant have very big difference, its polyphenol content is generally 2～4g/kg, and is more much lower than polyphenol content in the tealeaves, obtain higher extraction yield and product purity and is not easy.
Though the nutritive ingredient of pineapple peel juice is near pulp juice because polyphenol and some pigment contents are higher in the pineapple peel juice, influenced its appearance color and local flavor, especially store for some time after, very serious browning phenomenon appears.No matter pineapple peel juice directly is utilized as nectar, or brewing materials as pineapple wine, pineapple vinegar, all must remove polyphenol, some pigments and some influence the impurity of local flavor, maximum amplitude ground reduces browning degree, keeps nutritive substance and appear the distinctive strong local flavor of pineapple suddenly.At present, the polyphenol substance that removes fruit juice, fruit wine etc. can adopt sorbent materials such as polymeric amide, polyvinylpyrrolidone, these sorbent materials are strong to the specificity of polyphenol absorption, the nutritive ingredient loss is extremely low in the fruit juice, but adsorptive power is little, and adopt organic solvent wash-out difficulty, need to adopt alkali lye to carry out wash-out, thereby be unfavorable for reclaiming polyphenol; Activated carbon adsorptive capacity is very strong, but the selectivity extreme difference removes polyphenol substance, pigment etc. simultaneously, also can make the nutritive substance loss bigger.
At present, the comprehensive utilization of relevant pineapple peel mainly is to extract brewageing of bromeline and pineapple peel juice, little research document of producing the pineapple polyphenol, and Shang Weiyou unites the report of producing pineapple polyphenol and fruit juice.As previously discussed, utilize pineapple peel juice to carry out brewed fruit wine, fruit vinegar etc., must be through removing polyphenol substance and some pigments, thereby the preparation method of pineapple peel juice provides good pre-treating technology for the further utilization of pineapple peel juice among the present invention.In addition, in the actual production of pineapple peel comprehensive utilization, the production cost of producing single product is all higher.
Summary of the invention
In order to overcome the problem that the pineapple secondary industry exists a large amount of pineapple peel to go out of use, it is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel that primary and foremost purpose of the present invention is to provide a kind of.This method is pollution-free, product yield height, and the pineapple polyphenol purity height of preparation and the browning degree of gained fruit juice are low, can obtain good economic benefit.
Another object of the present invention is to provide the application of aforesaid method.
Purpose of the present invention is achieved through the following technical solutions: a kind of is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, may further comprise the steps:
(1) pineapple peel obtains pineapple bran and pineapple peel juice through cleaning, squeezing, solid-liquid separation;
(2) pineapple peel juice flows into macroporous resin column with the flow velocity of 0.5～2.0BV/h, and is saturated until macroporous resin adsorption; Collect the preceding effluent liquid of macroporous resin column absorption leakage point; Debris is collected separately in effluent liquid after the macroporous resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices; Add 1～4g/L powder activated carbon in all effluent liquid before the resin column leakage point that collection obtains and stir decolouring 30～60min, can get fruit juice after filtration;
(3) be 50～60% ethanolic soln with the pineapple bran of gained in the step (1) and volume percent by mass ratio 1: mix (5～20), smash to pieces, then in 60～80 ℃ of backflow lixiviate 120～180min, through solid-liquid separation, skin slag after the removal lixiviate obtains the polyphenol vat liquor;
(4) the polyphenol vat liquor is carried out vacuum concentration and reclaim ethanol, until the concentrated solution volume is 20～40% of former vat liquor, it is 0.1～0.2B é that the adding deionized water is diluted to the solution degree Beaume, with the flow velocity inflow macroporous resin column of diluent, reach the absorption saturation point again until macroporous resin column with 0.5～2.0BV/h; Effluent liquid before the resin column leak point can be collected as extracting technology water and recycle, and the effluent liquid between resin column leak point and the saturation point needs again upper prop to carry out adsorption treatment;
(5) with the saturated macroporous resin column of absorption in deionized water wash step (2) and the step (4), washing to the inclusion-free again, the ethanolic soln with 70～80% (v/v) carries out wash-out, the Fractional Collections elutriant; The elutriant (being high flow point) that elution peak is concentrated carries out vacuum concentration and reclaims ethanol, is 15～25% of former effluent volume until the concentrated solution volume, is the polyphenol concentrated solution; The elutriant in all the other stages is back to the lixiviate pineapple bran;
(6) reach 0.2～0.4B é with deionized water dilution polyphenol concentrated solution to the solution degree Beaume, the methylene dichloride that adds 1～2 times of volume extracts, water intaking layer, re-extract 2～4 times; The ethyl acetate that adds 1～2 times of volume to raffinate (being water layer) extracts, separates, repeatable operation 2～4 times, the combined ethyl acetate layer, add the deionized water that is equivalent to raffinate volume 2～4% again, vacuum concentration reclaims ethyl acetate then, reach 10～20B é until the concentrated solution degree Beaume,, obtain the pineapple polyphenol again with the concentrated solution drying.
Described macroporous resin is polar macroporous resin, low-pole macroporous resin and non-polar macroporous resin;
In order to realize the present invention better, the macroporous resin of described macroporous resin column can be selected XDA-5, S-8, AB-8, X-5, D-101, NKA-9 and SD300 etc. for use, and is not limited to mentioned resin model; These resins method (resin manufacturer provides) according to the rules carry out pre-treatment and regeneration;
Juice clarification described in the step (2) can be used for being processed as pineapple fruit juice beverage, pineapple wine and pineapple vinegar etc.;
Smash to pieces described in the step (3) and preferably place machinery to smash to pieces in the jar to smash to pieces;
Solid-liquid separation is preferably by centrifugation described in the step (3);
The vacuum degree control of vacuum concentration is at 0.06～0.1MPa described in step (4), step (5) and the step (6);
The speed of wash-out is 0.5～1.5BV/h described in the step (5);
Concentrated solution exsiccant method described in the step (6) is not limited to spraying drying or vacuum lyophilization etc.
Described is that raw material is united the method for producing pineapple polyphenol and fruit juice and is applied to the pineapple manufacture field with the pineapple peel.
Principle of the present invention is: macroporous resin has stronger adsorptive power to polyphenol, pigment etc. than macromolecular substance, and to the adsorptive power of small-molecule substance a little less than, so select macroporous resin to be used for adsorbing materials such as pineapple peel juice, pineapple bran vat liquor polyphenol and pigment; In order further to remove polyphenol and pigment in the pineapple peel juice, adopt the small quantities of powder gac that it is carried out adsorption treatment again, can obtain the extremely low fruit juice of browning degree; Adopt ethanolic soln the adsorbed material of macroporous resin can be eluted, because that elutriant contains pigment impurity is more, and methylene dichloride is checked colors and is have very strong solubility, adopts dichloromethane extraction can remove most of pigment impurity; In order further to improve the purity of pineapple polyphenol, according to the very strong dissolution characteristics of ethyl acetate to polyphenol, again methylene dichloride raffinate layer (water layer) is carried out ethyl acetate extraction, can obtain highly purified polyphenol solution, through concentrated, dry, can obtain highly purified pineapple polyphenol product again.
The present invention has following advantage and effect with respect to prior art:
(1) the method for the invention comprises steps such as ethanol lixiviate, resin absorption, dichloromethane extraction, ethyl acetate extraction, helps obtaining highly purified pineapple polyphenol; The fruit juice preparation method has adopted resin and gac distribution absorption, helps removing polyphenol and pigment in the pineapple peel juice, and the juice browning degree is reduced significantly.By the juice clarification that the present invention makes, sugar and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching; The pineapple polyphenol purity that makes is more than 90%, and extraction yield can reach the extraction of per kilogram pineapple peel and obtain 2.5g pineapple polyphenol, and economic benefit is more remarkable.
(2) used extraction raw material is a depleted pineapple peel in the pineapple processing among the present invention, not only avoided the pollution of waste to environment, and opened up the new way of pineapple peel comprehensive utilization, and the method among the present invention can combination producing fruit juice and two products of polyphenol, to the added value that reduces production costs, promote byproduct in the pineapple secondary industry and promote that recycling economy development is all significant.
(3) the method for the invention embodies efficient, energy-conservation and environmental protection in the following aspects:
A, reach absorption in macroporous resin column and just begin wash-out, resin column service efficiency height after saturated;
The effluent liquid Fractional Collections of B, vat liquor upper prop, effluent liquid before the resin column leak point is back to the lixiviate pineapple bran, the elutriant Fractional Collections, the preceding flow point that polyphenol concentration is lower, back flow point all are back to the lixiviate pineapple bran, thereby form a round-robin operational path, help improving the polyphenol extraction yield and reduce discharge of wastewater;
C, vat liquor, the high flow point of elutriant, acetic acid ethyl acetate extract all reclaim organic solvent through vacuum concentration, both can reuse organic solvent, can avoid environmental pollution again.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) takes by weighing fresh pineapple skin 200kg,, get 140.6L pineapple peel juice and 55.6kg pineapple bran through cleaning, squeezing and centrifugation.
(2) pineapple peel juice is flowed into the XDA-5 resin column with the flow velocity of 1.0BV/h and carry out adsorbing polyphenols and pigment, it is saturated to reach absorption until resin column, collects the effluent liquid before the resin column absorption leakage point.Debris needs to collect separately in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices.Then, the 250g Powdered Activated Carbon is made an addition in the collection liquid (activated carbon dosage is 1.78g/L), stir decolouring 30min, obtain clarifying fruit juice after filtration, the sugar of fruit juice and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching.With the absorbancy (A value) of 1cm cuvette working sample under 420nm, the A value before and after the pineapple peel juice adsorption treatment is respectively 0.926 and 0.042, and normal temperature is stored after 18 months down, and the A value of pineapple peel fruit juice is 0.096, and browning degree is very slight.
(3) the 55.6kg pineapple bran is mixed with 60% (v/v) ethanolic soln of 600L, place machinery to smash to pieces and smash operation 30min in the jar to pieces, in 60 ℃ of backflow lixiviate 180min, obtain the polyphenol vat liquor then through centrifugation.
(4) be to carry out concentrating under reduced pressure under the 0.08MPa with the polyphenol vat liquor in vacuum tightness, get concentrated solution 150L, add 200L deionized water mixing, making its degree Beaume is 0.20B é, flow velocity inflow XDA-5 resin column with 0.5BV/h carries out adsorbing polyphenols, and it is saturated to reach absorption until resin column.Debris need be collected in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point until all diluents.
(5) with the saturated XDA-5 resin column of absorption in deionized water thorough washing step (2) and the step (4), use 80% (v/v) ethanolic soln to carry out wash-out again, elution flow rate is 0.5BV/h, collects the elutriant 72L that elution peak is concentrated relatively.Elutriant is to be concentrated into 12L under the 0.08MPa in vacuum tightness, is the polyphenol concentrated solution.
(6) add the 228L deionized water in the polyphenol concentrated solution, making its degree Beaume is 0.20B é, places in the column extractor, adds the 240L methylene dichloride and extracts, and raffinate (water layer) is got in repetitive operation 3 times.In raffinate, add the 240L ethyl acetate and extract, repetitive operation 3 times, the combined ethyl acetate layer adds the 7L deionized water, is to be concentrated into 3.8L (degree Beaume is 10B é) under the 0.08MPa in vacuum tightness.The gained concentrated solution is spray-dried, obtains 558.3g pineapple polyphenol, and extraction yield extracts for the per kilogram pineapple peel and obtains 2.8g pineapple polyphenol.Adopting the Folin-Ciocalte colorimetry to record polyphenols content is 93.8%, utilizes high performance liquid chromatography (HPLC) analysis, and wherein catechin content is 8.6%, and l-Epicatechol content is 11.8%, and gallic acid content is 7.4%.
Embodiment 2
(1) takes by weighing fresh pineapple skin 150kg,, get 100.2L pineapple peel juice and 45.4kg pineapple bran through cleaning, squeezing and centrifugation.
(2) pineapple peel juice is flowed into the AB-8 resin column with the flow velocity of 1.5BV/h and carry out adsorbing polyphenols and pigment, it is saturated to reach absorption until resin column, collects the effluent liquid before the resin column absorption leakage point.Debris needs to collect separately in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices.Then, the 280g Powdered Activated Carbon is made an addition in the collection liquid (activated carbon dosage is 2.80g/L), stir decolouring 45min, obtain clarifying fruit juice after filtration, the sugar of fruit juice and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching.With the absorbancy (A value) of 1cm cuvette working sample under 420nm, the A value before and after the pineapple peel juice adsorption treatment is respectively 0.965 and 0.057, and normal temperature is stored after 18 months down, and the A value of pineapple peel fruit juice is 0.104, and browning degree is very slight.
(3) the 45.4kg pineapple bran is mixed with 50% (v/v) ethanolic soln of 600L, place machinery to smash to pieces and smash operation 30min in the jar to pieces, in 70 ℃ of backflow lixiviate 150min, obtain the polyphenol vat liquor then through centrifugation.
(4) be to carry out concentrating under reduced pressure under the 0.07MPa with the polyphenol vat liquor in vacuum tightness, get concentrated solution 200L, add 320L deionized water mixing, making its degree Beaume is 0.10B é, flow velocity inflow AB-8 resin column with 2.0BV/h carries out adsorbing polyphenols, and it is saturated to reach absorption until resin column.Debris need be collected in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point until all diluents.
(5) with the saturated AB-8 resin column of absorption in deionized water thorough washing step (2) and the step (4), use 75% (v/v) ethanolic soln to carry out wash-out again, elution flow rate is 0.8BV/h, collects the elutriant 67.4L that elution peak is concentrated relatively.Elutriant is to be concentrated into 16L under the 0.07MPa in vacuum tightness, is the polyphenol concentrated solution.
(6) add the 84L deionized water in the polyphenol concentrated solution, making its degree Beaume is 0.40B é, places in the column extractor, adds the 200L methylene dichloride and extracts, and raffinate (water layer) is got in repetitive operation 4 times.In raffinate, add the 200L ethyl acetate and extract, repetitive operation 2 times, the combined ethyl acetate layer adds the 4L deionized water, is to be concentrated into 1.4L (degree Beaume is 20B é) under the 0.08MPa in vacuum tightness.The gained concentrated solution is spray-dried, gets 411.5g pineapple polyphenol, and extraction yield extracts for the per kilogram pineapple peel and obtains 2.7g pineapple polyphenol.Adopting the Folin-Ciocalte colorimetry to record polyphenols content is 92.5%, utilizes high performance liquid chromatography (HPLC) analysis, and wherein catechin content is 8.4%, and l-Epicatechol content is 11.9%, and gallic acid content is 7.5%.
Embodiment 3
(1) takes by weighing fresh pineapple skin 150kg,, get 100.5L pineapple peel juice and 44.8kg pineapple bran through cleaning, squeezing and centrifugation.
(2) pineapple peel juice is flowed into the X-5 resin column with the flow velocity of 2.0BV/h and carry out adsorbing polyphenols and pigment, it is saturated to reach absorption until resin column, collects the effluent liquid before the resin column absorption leakage point.Debris needs to collect separately in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices.Then, the 400g Powdered Activated Carbon is made an addition in the collection liquid (activated carbon dosage is 3.98g/L), stir decolouring 30min, can get clarifying fruit juice after filtration, the sugar of fruit juice and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching.With the absorbancy (A value) of lcm cuvette working sample under 420nm, the A value before and after the pineapple peel juice adsorption treatment is respectively 0.913 and 0.040, and normal temperature is stored after 18 months down, and the A value of pineapple peel fruit juice is 0.089, and browning degree is very slight.
(3) the 44.8kg pineapple bran is mixed with 60% (v/v) ethanolic soln of 224L, place machinery to smash to pieces and smash operation 45min in the jar to pieces, in 80 ℃ of backflow lixiviate 120min, obtain the polyphenol vat liquor then through centrifugation.
(4) be to carry out concentrating under reduced pressure under the 0.06MPa with the polyphenol vat liquor in vacuum tightness, get concentrated solution 89.6L, add 240L deionized water mixing, making its degree Beaume is 0.15B é, flow velocity inflow X-5 resin column with 1.0BV/h carries out adsorbing polyphenols, and it is saturated to reach absorption until resin column.Debris need be collected in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point until all diluents.
(5) with the saturated X-5 resin column of absorption in deionized water thorough washing step (2) and the step (4), use 70% (v/v) ethanolic soln to carry out wash-out again, elution flow rate is 1.5BV/h, collects the elutriant 80.8L that elution peak is concentrated relatively.Elutriant is to be concentrated into 20.2L under the 0.1MPa in vacuum tightness, is the polyphenol concentrated solution.
(6) add the 129.8L deionized water in the polyphenol concentrated solution, making its degree Beaume is 0.25B é, places in the column extractor, adds the 300L methylene dichloride and extracts, and raffinate (water layer) is got in repetitive operation 2 times.In raffinate, add the 150L ethyl acetate and extract, repetitive operation 4 times, the combined ethyl acetate layer adds the 3L deionized water, is to be concentrated into 2L (degree Beaume is 15B é) under the 0.1MPa in vacuum tightness.The gained concentrated solution is spray-dried, gets 410.2g pineapple polyphenol, and extraction yield extracts for the per kilogram pineapple peel and obtains 2.7g pineapple polyphenol.Adopting the Folin-Ciocalte colorimetry to record polyphenols content is 93.0%, utilizes high performance liquid chromatography (HPLC) analysis, and wherein catechin content is 8.8%, and l-Epicatechol content is 11.6%, and gallic acid content is 7.4%.
Embodiment 4
(1) takes by weighing fresh pineapple skin 150kg,, get 99.5L pineapple peel juice and 45kg pineapple bran through cleaning, squeezing and centrifugation.
(2) pineapple peel juice is flowed into the NKA-9 resin column with the flow velocity of 0.5BV/h and carry out adsorbing polyphenols and pigment, it is saturated to reach absorption until resin column, collects the effluent liquid before the resin column absorption leakage point.Debris needs to collect separately in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices.Then, the 100g Powdered Activated Carbon is made an addition in the collection liquid (activated carbon dosage is 1.0g/L), stir decolouring 30min, can get clarifying fruit juice after filtration, the sugar of fruit juice and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching.With the absorbancy (A value) of 1cm cuvette working sample under 420nm, the A value before and after the pineapple peel juice adsorption treatment is respectively 0.915 and 0.052, and normal temperature is stored after 18 months down, and the A value of pineapple peel fruit juice is 0.096, and browning degree is very slight.
(3) the 45kg pineapple bran is mixed with 50% (v/v) ethanolic soln of 900L, place machinery to smash to pieces and smash operation 45min in the jar to pieces, in 80 ℃ of backflow lixiviate 120min, obtain the polyphenol vat liquor then through centrifugation.
(4) be to carry out concentrating under reduced pressure under the 0.1MPa with the polyphenol vat liquor in vacuum tightness, get concentrated solution 360L, add 40L deionized water mixing, making its degree Beaume is 0.12B é, flow velocity inflow X-5 resin column with 1.5BV/h carries out adsorbing polyphenols, and it is saturated to reach absorption until resin column.Debris need be collected in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point until all diluents.
(5) with the saturated X-5 resin column of absorption in deionized water thorough washing step (2) and the step (4), use 80% (v/v) ethanolic soln to carry out wash-out again, elution flow rate is 1.0BV/h, collects the elutriant 70.0L that elution peak is concentrated relatively.Elutriant is to be concentrated into 10.5L under the 0.1MPa in vacuum tightness, is the polyphenol concentrated solution.
(6) add the 99.5L deionized water in the polyphenol concentrated solution, making its degree Beaume is 0.33B é, places in the column extractor, adds the 165L methylene dichloride and extracts, and raffinate (water layer) is got in repetitive operation 3 times.In raffinate, add the 165L ethyl acetate and extract, repetitive operation 3 times, the combined ethyl acetate layer adds the 4L deionized water, is to be concentrated into 2.2L (degree Beaume is 13B é) under the 0.1MPa in vacuum tightness.The gained concentrated solution is spray-dried, gets 408.6g pineapple polyphenol, and extraction yield extracts for the per kilogram pineapple peel and obtains 2.7g pineapple polyphenol.Adopting the Folin-Ciocalte colorimetry to record polyphenols content is 92.8%, utilizes high performance liquid chromatography (HPLC) analysis, and wherein catechin content is 8.5%, and l-Epicatechol content is 11.3%, and gallic acid content is 7.5%.
Embodiment 5
(1) takes by weighing fresh pineapple skin 120kg,, get 83.4L pineapple peel juice and 33.1kg pineapple bran through cleaning, squeezing and centrifugation.
(2) pineapple peel juice is flowed into the X-5 resin column with the flow velocity of 1.5BV/h and carry out adsorbing polyphenols and pigment, it is saturated to reach absorption until resin column, collects the effluent liquid before the resin column absorption leakage point.Debris needs to collect separately in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point and is collected until all pineapple peel juices.Then, the 220g Powdered Activated Carbon is made an addition in the collection liquid (activated carbon dosage is 2.64g/L), stir decolouring 30min, can get clarifying fruit juice after filtration, the sugar of fruit juice and ascorbic loss are all less than 8%, and local flavor and pineapple pulp juice are very approaching.With the absorbancy (A value) of 1cm cuvette working sample under 420nm, the A value before and after the pineapple peel juice adsorption treatment is respectively 0.905 and 0.038, and normal temperature is stored after 18 months down, and the A value of pineapple peel fruit juice is 0.095, and browning degree is very slight.
(3) the 33.1kg pineapple bran is mixed with 60% (v/v) edible ethanol solution of 600L, place machinery to smash to pieces and smash operation 45min in the jar to pieces, in 60 ℃ of backflow lixiviate 180min, obtain the polyphenol vat liquor then through centrifugation.
(4) be to carry out concentrating under reduced pressure under the 0.08MPa with the polyphenol vat liquor in vacuum tightness, get concentrated solution 210L, add 30L deionized water mixing, making its degree Beaume is 0.13B é, flow velocity inflow X-5 resin column with 1.0BV/h carries out adsorbing polyphenols, and it is saturated to reach absorption until resin column.Debris need be collected in effluent liquid after the resin column absorption leakage point and the resin column, and upper prop carries out adsorption treatment again, flows out before the resin column leakage point until all diluents.
(5) with the saturated X-5 resin column of absorption in deionized water thorough washing step (2) and the step (4), use 70% (v/v) edible ethanol solution to carry out wash-out again, elution flow rate is 1.0BV/h, collects the elutriant 50.5L that elution peak is concentrated relatively.Elutriant is to be concentrated into 10L under the 0.08MPa in vacuum tightness, is the polyphenol concentrated solution.
(6) add the 110L deionized water in the polyphenol concentrated solution, making its degree Beaume is 0.25B é, places in the column extractor, adds the 240L methylene dichloride and extracts, and raffinate (water layer) is got in repetitive operation 2 times.In raffinate, add the 240L ethyl acetate and extract, repetitive operation 2 times, the combined ethyl acetate layer adds the 4.8L deionized water, is to be concentrated into 2L (degree Beaume is 11.9B é) under the 0.08MPa in vacuum tightness.The gained concentrated solution is spray-dried, gets 340.2g pineapple polyphenol, and extraction yield extracts for the per kilogram pineapple peel and obtains 2.7g pineapple polyphenol.Adopting the Folin-Ciocalte colorimetry to record polyphenols content is 93.2%, utilizes high performance liquid chromatography (HPLC) analysis, and wherein catechin content is 8.8%, and l-Epicatechol content is 10.9%, and gallic acid content is 7.2%.
The foregoing description is a preferred implementation 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 the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1, a kind of is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, it is characterized in that, may further comprise the steps:
(1) pineapple peel obtains pineapple bran and pineapple peel juice through cleaning, squeezing, solid-liquid separation;
(2) pineapple peel juice flows into macroporous resin column with the flow velocity of 0.5～2.0BV/h, and is saturated until macroporous resin adsorption, collects the preceding effluent liquid of macroporous resin column absorption leakage point; Collect debris in effluent liquid after the macroporous resin column absorption leakage point and the resin column separately, and upper prop carries out adsorption treatment again, before the resin column leakage point, flow out and be collected until all pineapple peel juices; Add 1～4g/L powder activated carbon in all effluent liquid before the resin column leakage point that collection obtains and stir decolouring 30～60min, filter and obtain fruit juice;
(3) be 50～60% ethanolic soln with the pineapple bran of gained in the step (1) and volume percent by mass ratio 1: mix (5～20), smashs to pieces, in 60～80 ℃ of backflow lixiviate 120～180min, through solid-liquid separation, obtains the polyphenol vat liquor then;
(4) the polyphenol vat liquor is carried out vacuum concentration and reclaim ethanol, until the concentrated solution volume is 20～40% of former vat liquor volume, it is 0.1～0.2B é that the adding deionized water is diluted to the solution degree Beaume, with the flow velocity inflow macroporous resin column of diluent, reach the absorption saturation point again until macroporous resin column with 0.5～2.0BV/h; Effluent liquid before the resin column leak point can be collected as extracting technology water and recycle, and the effluent liquid between resin column leak point and the saturation point needs again upper prop to carry out adsorption treatment;
(5) with the saturated macroporous resin column of absorption in deionized water wash step (2) and the step (4), washing to the inclusion-free with volume percent is that 70～80% ethanolic soln carries out wash-out, the Fractional Collections elutriant again; The elutriant that elution peak is concentrated carries out vacuum concentration and reclaims ethanol, is 15～25% of former effluent volume until the concentrated solution volume, is the polyphenol concentrated solution; The elutriant in all the other stages is back to the lixiviate pineapple bran;
(6) reach 0.2～0.4B é with deionized water dilution polyphenol concentrated solution to the solution degree Beaume, the methylene dichloride that adds 1～2 times of volume extracts, water intaking layer, re-extract 2～4 times; The ethyl acetate that adds 1～2 times of volume to raffinate extracts, separates, repeatable operation 2～4 times, the combined ethyl acetate layer, add the deionized water that is equivalent to raffinate volume 2～4% again, vacuum concentration reclaims ethyl acetate then, reach 10～20B é until the concentrated solution degree Beaume,, obtain the pineapple polyphenol again with the concentrated solution drying.
2, according to claim 1 is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, it is characterized in that: the macroporous resin of described macroporous resin column is a kind of among XDA-5, S-8, AB-8, X-5, D-101, NKA-9 or the SD300;
3, according to claim 1 is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, and it is characterized in that: the vacuum tightness of described vacuum concentration is 0.06～0.1MPa.
4, according to claim 1 is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, and it is characterized in that: the solid-liquid separation described in the step (3) is for to be undertaken by centrifugation.
5, according to claim 1 is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, and it is characterized in that: the speed of wash-out is 0.5～1.5BV/h described in the step (5).
6, according to claim 1 is that raw material is united the method for producing pineapple polyphenol and fruit juice with the pineapple peel, it is characterized in that: dry spraying drying mode or the vacuum lyophilization mode of adopting of the concentrated solution described in the step (6).
7, claim 1～6 each described be that raw material is united the method for producing pineapple polyphenol and fruit juice and is applied to the pineapple manufacture field with the pineapple peel.
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