CN109874999A - Synchronous grape pip powder, preparation and the dedicated unit for extracting protein and dietary fiber - Google Patents

Synchronous grape pip powder, preparation and the dedicated unit for extracting protein and dietary fiber Download PDF

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Publication number
CN109874999A
CN109874999A CN201910223668.5A CN201910223668A CN109874999A CN 109874999 A CN109874999 A CN 109874999A CN 201910223668 A CN201910223668 A CN 201910223668A CN 109874999 A CN109874999 A CN 109874999A
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China
Prior art keywords
grape pip
dietary fiber
protein
powder
synchronous
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Inventor
孔令明
邹积赟
杨华峰
张爱琴
孙乾
薛雨菲
张玥
杨罡
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XINJIANG HAIRUISHENG BIO-ENGINEERING Co Ltd
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XINJIANG HAIRUISHENG BIO-ENGINEERING Co Ltd
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Publication of CN109874999A publication Critical patent/CN109874999A/en
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Abstract

The present invention is directed to disclose a kind of synchronous grape pip powder for extracting protein and dietary fiber, preparation and dedicated unit, using grouts of the by-product after using grape pip to extract oil after ungrease treatment as raw material, using dedicated equipment, pass through coarse crushing and ultramicro crushing treatment, double enzyme resolving tech are combined to digest smashed material using ultrasonic treatment, vacuum spray drying is carried out by the enzymolysis liquid of extraction, it is set to form the vacuum fine grained for being easier to dissolve and digest and assimilate again while possessing nutriment, it is edible convenient for the various ways of such nutriment, the grape pip powder rich in protein and dietary fiber of preparation, with homogeneous, mouthfeel silk is sliding, good smell, the advantages that dissolubility is good, and the recovery rate of protein and dietary fiber is greatly promoted, for having widely in fact using grape liquor-making byproduct field With property and Development volue.

Description

Synchronous grape pip powder, preparation and the dedicated unit for extracting protein and dietary fiber
Invention field
The present invention is to belong to be related to the technical field of dietary fiber extraction.Specifically, the present invention relates to a kind of synchronize to mention Take the technical field of the grape pip powder of protein and dietary fiber, preparation and dedicated unit.
Background technique
Grape is one of most ancient, the widest plant of distribution that originates from, wherein Europe, Asia are main grape producing country, Vintage accounts for the 42.2% and 30.1% of the whole world respectively.80% for making wine in Gross World Product, China's grape -growing areas 570,000 hectares are had evolved to.The ground such as Hebei therein, Shandong, Ningxia, Gansu, Xinjiang are the main producing region of grape wine, until 2013, vinifera cultivated area was up to 90,000 hectares, and vintage is up to 11,700,000 liters.And in grape wine and grape juice Production process in, a large amount of grape pip slag can be generated, grape pip accounts for about the 4-7% of fresh fruit weight, and annual output is already expired 50,000 tons.
From the point of view of current research achievement, the effective component in grape pip mainly has: unsaturated fatty acid content is higher Grape seed oil, the protein with anti-oxidant and Scavenging ability procyanidine and amino acid classes multiplicity.But China, the effective rate of utilization of grape liquor-making byproduct is then very low, and most of grape liquor-making byproduct is all by as trade waste Lose or be used as animal fodder after simple process, this not only causes environmental pollution to a certain extent, to resource and A kind of significant wastage.Therefore, deep processing is carried out to the by-product after grape wine brewing, develops high value-added product, sufficiently Using resource, reduce environmental pollution, turn waste into wealth, improve and improve people's health level, have far-reaching economic significance and Social benefit.
The extracting method of functional components is mainly the method for using step by step arithmetic.When being extracted to protein, often It is individually extracted using alkali solution technique and the molten method of salt;When extracting to dietary fiber, be broadly divided into 4 classes, i.e., chemical analysis, One enzyme combination partition method of chemical reagent, membrane separation process and fermentation method extract.These methods on the one hand there are recovery rates low, efficiency Low, easy the problems such as making albuminous degeneration, on the one hand all relatively it is suitable for effective extraction of separate constituent, and cannot be to a variety of effective nutrition Ingredient synchronizes extraction.Therefore, how efficiently, the synchronous methods extracted and obtain good function ingredient become as most Mainly, also problem most in the urgent need to address.
Currently, the research of albumen is started late in China's grape liquor-making byproduct, extracting method is relatively single, is only limited to alkali Molten method and the molten method of salt are individually extracted.It is more during the extraction process due to not considering further although recovery rate is relatively high Interference of the phenolic compound to protein extraction, the quality of gained protein product be not high.
Summary of the invention
For having no that from the grape pip dregs of rice protein and dietary fiber synchronize the state of the art of extraction at present.The present invention It is intended to provide a kind of synchronous grape pip powder, preparation and dedicated unit for extracting protein and dietary fiber, to use grape pip Grouts of the by-product after ungrease treatment after oil expression are raw material, using dedicated equipment, at coarse crushing and ultramicro grinding Reason combines double enzyme resolving tech to digest smashed material using ultrasonic treatment, is carried out by the enzymolysis liquid of extraction true Sky spray drying, makes it form the vacuum fine grained for being easier to dissolve and digest and assimilate again while possessing nutriment, just It is edible in the various ways of such nutriment.
What the invention is realized by the following technical scheme:
The present invention provides a kind of synchronous grape pip powder for extracting protein and dietary fiber, especially by following preparation method It obtains:
(1) it pre-processes: will be crushed after the grape pip dregs of rice degreaser drying after oil expression with Roughpulverizer, obtain Portugal after crossing 40 meshes Grape seed dregs of rice powder, it is spare.
(2) it pulverizes: the grape pip dregs of rice powder that step (1) obtains being mixed with zirconium oxide balls, is pulverized, it will Its crushing is the grape pip dregs of rice powder rich in protein and dietary fiber that partial size is 10 μm.
(3) double enzymolysis is synchronous extracts: grape pip dregs of rice powder prepared by step (2) being placed in enzymatic vessel, to grape pip dregs of rice powder Middle addition deionized water adjusts pH value 7.0 with NaOH, is added by papain and cellulase the temperature was then adjusted to 40 DEG C Double enzyme preparations of composition, enzyme digestion reaction 1h, and using at dual-frequency ultrasonic wave in protein extraction process synchronous with dietary fiber Extracting solution is centrifuged 20min in 4500r/min after extraction, takes supernatant by reason;
(4) vacuum spray drying: 40% drying aid is added in the supernatant that step (3) are obtained, and controls inlet air temperature 160 DEG C, feed rate 400mL/h, atomizing pressure 160kPa enter the wind flow 0.60m3/min;Protein and dietary fiber mixing is made Dry powder;
(5) above-mentioned collection is pulverized, is filled in the synchronous extraction of double enzymolysis and vacuum spray drying technique using Special integrated It sets.
Preferably, in the present invention, grape pip dregs of rice powder is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: Portugal Grape seed dregs of rice powder=6:1
Preferably, in the present invention, the condition of ultramicro grinding is revolving speed 10000r/min, grinding time 30min.
Preferably, in the present invention, deionized water is added into grape pip dregs of rice powder, according to parts by weight, grape pip dregs of rice powder: goes Ionized water is 1:15.
Preferably, in the present invention, double enzyme preparations, according to parts by weight, and papain: cellulase=2:1, after mixing Obtain double enzyme preparations.
Preferably, in the present invention, by weight percentage, the additive amount of double enzyme preparations is 2%.
Preferably, in the present invention, dual-frequency ultrasonic wave treatment conditions are that double-frequency ultrasound combination frequency is 20kHz/50kHz, sound It is by force 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;
In the present invention, drying aid is maltodextrin.
Meanwhile a kind of collection that the present invention specifically provides pulverizes, the synchronous extraction of double enzymolysis and vacuum spray drying are dedicated Integrated device, including enzyme digestion reaction tank, micronizer, Roughpulverizer, solid-liquid separating machine, fluid reservoir and vacuum spray drying Micronizer is arranged in machine, enzyme digestion reaction tank side, and Roughpulverizer, Roughpulverizer and Ultramicro-powder is arranged in the micronizer other side Broken machine is connected by first pipe, and enzyme digestion reaction tank is connect with micronizer by screw elevator, below enzyme digestion reaction tank Solid-liquid separating machine is connected by second pipe, fluid reservoir is set by solid-liquid separating machine, and fluid reservoir is connected by water pump and pump tube Vacuum spray dehydrator is connect, the grape pip dregs of rice are by coarse crushing, ultramicro grinding, the synchronous extraction of double enzymolysis, vacuum spray drying Protein and dietary fiber mixed powder is made.
In the present invention, enzyme digestion reaction tank includes tank body, and tank body is in capsule shape type, and top of the tank is arranged motor, sets in tank body It sets stirring and stirs axis, agitating shaft is stirred bracing strut and is hung vertically in tank interior, and passes through shaft coupling with the motor of top of the tank It connects, paddle is set on agitating shaft, paddle is symmetric by axis of agitating shaft, and paddle is equipped with hydrophobic coating tank Control panel is arranged in external side.
In the present invention, material inlet tube is arranged in top of the tank, and material inlet pipe leads to tank interior.
In the present invention, tank body top two sides setting note deionized water interface and note enzymatic hydrolysis liquid interface infuse deionized water interface Lead to tank body, note enzymatic hydrolysis liquid interface connects the intracorporal spraying rack of tank.
In the present invention, feed opening is arranged in tank body upper side.
In the present invention, material taking mouth is arranged in tank body lower part side, and shut-off valve is arranged in material taking mouth.
In the present invention, liquid level sensor is arranged in tank body internal upper part, and liquid level sensor and control panel are electrically connected.
In the present invention, lower part setting temperature sensor and ultrasonic oscillator in tank body, temperature sensor and control panel are electric Property connection.
In the present invention, rack is set below tank body, double-frequency ultrasound wave producer, double-frequency ultrasound wave producer are set in rack It is electrically connected with ultrasonic oscillator.
In the present invention, material outlet pipe is arranged in tank base, and solenoid valve, solenoid valve and control plane is arranged in material outlet pipe Plate is electrically connected.
In the present invention, tank body side is provided with bar shaped observation window, and transparent glass is arranged in observation window, is equipped with and carves by observation window Spend line.
In the present invention, the tank body of enzyme digestion reaction tank is wrapped with temperature control layer, and temperature control layer two sides are provided with water filling port and water outlet Mouthful, water filling port level height is lower than water outlet level height.
A kind of synchronous grape pip powder and preparation for extracting protein and dietary fiber provided by the invention, using collection Ultramicro-powder Broken, the synchronous extraction of double enzymolysis and vacuum spray drying Special integrated device, the dual-frequency ultrasonic wave of use assist double enzyme enzymatic isolation methods Protein and dietary fiber, vacuum spray drying and the processing of corresponding superfine communication technique are extracted, the technology of specific matching is screened Parameter, sport technique segment has progressive, closely coupled feature, according to grape pip dregs of rice feature, sufficiently uses various technologies Means obtain, organic linking between each sport technique segment from test is repeated several times, whole inseparable, mating suitable collection ultra micro Crushing, the synchronous extraction of double enzymolysis and vacuum spray drying Special integrated device, can just obtain a kind of rich in protein and diet The grape pip powder of fiber, and have many advantages, such as that homogeneous, mouthfeel silk is sliding, good smell, and protein and dietary fiber mention Rate is taken greatly to be promoted.
By implement technical solution of the present invention, can achieve it is following the utility model has the advantages that
(1) present invention provides a kind of synchronous grape pip powder, preparation and dedicated unit for extracting protein and dietary fiber, with Grouts after grape pip oil expression are raw material, and the extract equipment provided through the invention is pulverized, dual-frequency ultrasonic wave auxiliary pair Enzyme enzymatic isolation method extracts the processing means such as protein and dietary fiber, vacuum spray drying, and one kind of acquisition is rich in protein and meals The grape pip powder for eating fiber, has many advantages, such as homogeneous, mouthfeel silk cunning, good smell, and protein and dietary fiber mention Rate is taken greatly to be promoted.Grape pip dregs of rice added value of product is improved, it is extensive practical having using grape liquor-making byproduct field Property and Development volue.
(2) present invention provides that a kind of collection, which pulverizes, double enzymolysis is synchronous extracts and vacuum spray drying Special integrated dress It sets, just can ensure that obtaining the strong grape pip powder rich in protein and dietary fiber of high recovery rate, purity is high, functional characteristic produces The various functions characteristic of product, protein and dietary fiber has different degrees of improvement, and wherein the present invention is relatively not used in dissolubility Middle technology compared to improving 8% or more, jitter time is then compared with shortening 20% or more.
Detailed description of the invention
Fig. 1 is shown as the synchronous process flow chart for extracting protein and dietary fiber from the grape pip dregs of rice.
Fig. 2 is shown as the synchronous extraction of collection ultramicro grinding, double enzymolysis and vacuum spray drying Special integrated apparatus structure shows It is intended to.
Fig. 3 is shown as collection and pulverizes, digests in the synchronous extraction of double enzymolysis and vacuum spray drying Special integrated device The schematic diagram of reactor tank.
Fig. 4 is shown as collection and pulverizes, digests in the synchronous extraction of double enzymolysis and vacuum spray drying Special integrated device The cross-sectional view of reactor tank.
Fig. 5 is shown as collection and pulverizes, digests in the synchronous extraction of double enzymolysis and vacuum spray drying Special integrated device The stirring system figure of reactor tank.
Fig. 6 is shown as papain: cellulase ratio and grinding time reciprocal effect dietary cellulosic recovery rate Surface chart.
Fig. 7 is shown as the surface chart of double enzyme preparation additive amounts and grinding time reciprocal effect dietary cellulosic recovery rate.
Fig. 8 is shown as the surface chart of double-frequency ultrasound combination frequency Yu grinding time reciprocal effect dietary cellulosic recovery rate.
Fig. 9 is shown as papain: the curved surface of cellulase ratio and grinding time reciprocal effect extraction rate of protein Figure.
Figure 10 is shown as the surface chart of double-frequency ultrasound combination frequency Yu grinding time reciprocal effect extraction rate of protein.
Figure 11 is shown as papain: cellulase ratio and double enzyme preparation additive amount reciprocal effect extraction rate of protein Surface chart.
Figure 12 is shown as alkali carries albumen grape pip powder and multiplex-enzyme extraction rich in protein and dietary fiber grape pip powder Solubility influence diagram.
In Fig. 2-5,1- Roughpulverizer, 2- micronizer, 3- enzyme digestion reaction tank, 30- rack, 31- tank body, 32- motor, 33- shaft coupling, 34- agitating shaft, 35- paddle, 36- spraying rack, 37- temperature sensor, 38- liquid level sensor, 39- double frequency are super Sonic generator, 310- stirring bracing strut, 311- ultrasonic oscillator, 312- material inlet pipe, 313- material outlet pipe, 314- take Sample mouth, 315- feed opening, 316- note deionized water interface, 317- note enzymatic hydrolysis liquid interface, 318- temperature control layer, 319- water filling port, 320- water outlet, 321- control panel, 322- observation window, 323- shut-off valve, 324- solenoid valve, 40- second pipe, 4- solid-liquid point It disembarks, 5- vacuum spray dehydrator.
Specific embodiment
In the following, illustrating the present invention for embodiment, still, the present invention is not limited to following embodiments.
The raw material selected in the present invention: the defatted grape seed dregs of rice, the preferential defatted grape seed for utilizing grape liquor-making byproduct The dregs of rice.
Hydrophobic coating that the present invention uses, micronizer 2, tank body 31, motor 32, shaft coupling 33, stirs Roughpulverizer 1 Mix axis 34, paddle 35, spraying rack 36, temperature sensor 37, liquid level sensor 38, double-frequency ultrasound wave producer 39, ultrasonic wave Oscillator 311, temperature control layer 318, control panel 321, shut-off valve 323, solenoid valve 324, solid-liquid separating machine 4, fluid reservoir 41, water pump 42 It can buy or customize by public channel with pump tube 43.
All reagents and instrument selected in the present invention, equipment are all well known in the art selection, but do not limit the present invention Implementation, other some reagents well known in the art and equipment are applied both to the implementation of following implementation of the present invention.
Embodiment one: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The present invention provides a kind of preparation of synchronous grape pip powder for extracting protein and dietary fiber, specifically includes following step It is rapid:
(1) it pre-processes: will be crushed after the grape pip dregs of rice degreaser drying after oil expression with Roughpulverizer, obtain Portugal after crossing 40 meshes Grape seed dregs of rice powder, it is spare.
(2) it pulverizes: being mixed the grape pip dregs of rice powder that step (1) obtains with zirconium oxide balls with micronizer 2, into Row pulverizes, and is crushed into the grape pip dregs of rice powder rich in protein and dietary fiber that partial size is 10 μm.
(3) double enzymolysis is synchronous extracts: grape pip dregs of rice powder prepared by step (2) being placed in enzyme digestion reaction tank 3, is gone by note Deionized water is added into tank body 31 and mixes with grape pip dregs of rice powder for ionized water interface 316, starts motor by control panel 321 32, motor 32 drives shaft coupling 33 and agitating shaft 34 and paddle 35 to start to stir, and passes through the temperature sensor 37 in can 31 Monitor the temperature in pipe, using on temperature control layer 318 water filling port 319 and water outlet 320 temperature in tank body 31 is adjusted to 40 DEG C, the shut-off valve 323 for opening sample tap 314 samples, and detects sample pH value, pH value 7.0 is adjusted by the NaOH of feed opening 315, The double enzyme preparations being made of papain and cellulase are added into tank body 31 by note enzymatic hydrolysis liquid interface 317, enzymatic hydrolysis is anti- 1h is answered, and in protein extraction process synchronous with dietary fiber, double-frequency ultrasound wave producer is opened by control panel 321 39, dual-frequency ultrasonic wave processing is carried out to the mixture in tank body 31 simultaneously using ultrasonic oscillator 311, will be extracted after extraction Liquid is centrifuged 20min by solid-liquid separating machine 44500r/min, takes supernatant;
(4) vacuum spray drying: 40% drying aid is added in the supernatant that step (3) are obtained, and passes through water pump 42 and water pump Pipeline 43, which injects, controls 160 DEG C of inlet air temperature, feed rate 400mL/h, atomizing pressure 160kPa in vacuum spray dehydrator 5, Enter the wind flow 0.60m3/min;Protein and dietary fiber mixed powder is made.
Preferably, in the present invention, grape pip dregs of rice powder is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: Portugal Grape seed dregs of rice powder=6:1.
Preferably, in the present invention, the condition of ultramicro grinding is revolving speed 10000r/min, grinding time 30min.
Preferably, in the present invention, deionized water is added into grape pip dregs of rice powder, according to parts by weight, grape pip dregs of rice powder: goes Ionized water is 1:15.
Preferably, in the present invention, double enzyme preparations, according to parts by weight, and papain: cellulase=2:1, after mixing Obtain double enzyme preparations.
Preferably, in the present invention, according to parts by weight, the additive amount of double enzyme preparations is 2%.
Preferably, in the present invention, dual-frequency ultrasonic wave treatment conditions are that double-frequency ultrasound combination frequency is 20kHz/50kHz, sound It is by force 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;
In the present invention, drying aid is maltodextrin.
Embodiment two: collection pulverizes, double enzymolysis synchronizes extraction and vacuum spray drying Special integrated device
Referring to shown in attached drawing 2-5, the present invention provide it is a kind of protein and food fibre powder are prepared from the grape pip dregs of rice be System, including enzyme digestion reaction tank 3, pulverizer 1, micronizer 2, solid-liquid separating machine 4 and vacuum spray dehydrator 5, enzyme digestion reaction Micronizer 2 is arranged in 3 side of tank, and pulverizer 1 is arranged in 2 other side of micronizer, and pulverizer 1 passes through with micronizer 2 First pipe 11 connects, and enzyme digestion reaction tank 3 connect 21 by screw elevator with micronizer 2, the lower section of enzyme digestion reaction tank 3 Connect solid-liquid separating machine 4 by second pipe 40, fluid reservoir 41 be set by solid-liquid separating machine 4, fluid reservoir 41 by water pump 42 and Pump tube 43 connects vacuum spray dehydrator 5.
In the present invention, enzyme digestion reaction tank includes tank body 31, and tank body 31 is in capsule-type, and motor 32, tank is arranged at the top of tank body 31 Agitating shaft 34 is set in body 31, and agitating shaft 34 is hung vertically in inside tank body 31 by stirring bracing strut 310, agitating shaft 34 and electricity Machine 32 is connected by shaft coupling 33, and paddle 35 is arranged on agitating shaft 34, and paddle 35 is axis in symmetrical point with agitating shaft 34 Cloth setting, paddle 35 are equipped with hydrophobic coating, control panel 321 are arranged on the outside of tank body 31.
In the present invention, material inlet tube 312 is set, material inlet pipe 312 leads to inside tank body 31 at the top of tank body 31.
In the present invention, 31 top two sides of tank body setting note deionized water interface 316 and note enzymatic hydrolysis liquid interface 317, note go from Sub- water interface 316 leads to tank body 31, and note enzymatic hydrolysis liquid interface 317 connects the spraying rack 36 in tank body 31.
In the present invention, feed opening 315 is arranged in 31 upper side of tank body.
In the present invention, material taking mouth is arranged in 31 lower side of tank body, and shut-off valve 323 is arranged in material taking mouth.
In the present invention, liquid level sensor 38 is arranged in 31 internal upper part of tank body, and liquid level sensor 38 electrically connects with control panel 321 It connects.
In the present invention, temperature sensor 37 and ultrasonic oscillator 311, temperature sensor 37 and control is arranged in lower part in tank body 31 Panel 321 processed is electrically connected.
In the present invention, rack 30 is set below tank body 31, double-frequency ultrasound wave producer 39, double-frequency ultrasound are set in rack 30 Wave producer 39 and ultrasonic oscillator 311 are electrically connected.
In the present invention, material outlet pipe 313 is arranged in 31 bottom of tank body, and solenoid valve 324, electricity are arranged in material outlet pipe 313 Magnet valve 324 and control panel 321 are electrically connected.
In the present invention, 31 side of tank body is provided with bar shaped observation window 322, and transparent glass, observation window are arranged in observation window 322 322 sides are equipped with graduation mark.
In the present invention, the tank body 31 of enzyme digestion reaction tank 3 is wrapped with temperature control layer 318, and 318 two sides of temperature control layer are provided with water filling Mouth 319 and water outlet 316,319 level height of water filling port are lower than 316 level height of water outlet.
Embodiment three: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The preparation of the synchronous grape pip powder for extracting protein and dietary fiber, specifically includes the following steps: by after oil expression It is crushed after grape pip dregs of rice degreaser drying with Roughpulverizer, grape pip dregs of rice powder is obtained after crossing 40 meshes, by the grape pip dregs of rice powder of acquisition It is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1 is pulverized after mixing, Grape pip dregs of rice powder is placed in enzymatic vessel by revolving speed 10000r/min, grinding time 20min, deionized water is added, in parts by weight Meter, grape pip dregs of rice powder: deionized water 1:15 adjusts pH value 7.0 with NaOH the temperature was then adjusted to 40 DEG C, according to parts by weight, Papain: cellulase=1:2 obtains double enzyme preparations after mixing, is added 1% double enzyme preparations, enzyme digestion reaction 1h, and It is handled in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave, double-frequency ultrasound combination frequency is 20kHz/ 60kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;Extraction terminates Extracting solution is centrifuged 20min in 4500r/min afterwards, takes supernatant;40% drying aid is added in supernatant, controls inlet air temperature 140 DEG C, feed rate 400mL/h, atomizing pressure 180kPa, enter the wind flow 0.80m3Albumen is made in/min, vacuum spray drying Matter and dietary fiber mixed powder.
Example IV: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The preparation of the synchronous grape pip powder for extracting protein and dietary fiber, specifically includes the following steps: by after oil expression It is crushed after grape pip dregs of rice degreaser drying with Roughpulverizer, grape pip dregs of rice powder is obtained after crossing 40 meshes, by the grape pip dregs of rice powder of acquisition It is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1 is pulverized after mixing, Grape pip dregs of rice powder is placed in enzymatic vessel by revolving speed 10000r/min, grinding time 25min, deionized water is added, in parts by weight Meter, grape pip dregs of rice powder: deionized water 1:15 adjusts pH value 7.0 with NaOH the temperature was then adjusted to 40 DEG C, according to parts by weight, Papain: cellulase=2:2 obtains double enzyme preparations after mixing, is added 1.5% double enzyme preparations, enzyme digestion reaction 1h, and It is handled in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave, double-frequency ultrasound combination frequency is 20kHz/ 40kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;Extraction terminates Extracting solution is centrifuged 20min in 4500r/min afterwards, takes supernatant;40% drying aid is added in supernatant, controls inlet air temperature 150 DEG C, feed rate 400mL/h, atomizing pressure 170kPa, enter the wind flow 0.70m3Albumen is made in/min, vacuum spray drying Matter and dietary fiber mixed powder.
Embodiment five: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The preparation of the synchronous grape pip powder for extracting protein and dietary fiber, specifically includes the following steps: by after oil expression It is crushed after grape pip dregs of rice degreaser drying with Roughpulverizer, grape pip dregs of rice powder is obtained after crossing 40 meshes, by the grape pip dregs of rice powder of acquisition It is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1 is pulverized after mixing, Grape pip dregs of rice powder is placed in enzymatic vessel by revolving speed 10000r/min, grinding time 30min, deionized water is added, in parts by weight Meter, grape pip dregs of rice powder: deionized water 1:15 adjusts pH value 7.0 with NaOH the temperature was then adjusted to 40 DEG C, according to parts by weight, Papain: cellulase=2:1 obtains double enzyme preparations after mixing, is added 2% double enzyme preparations, enzyme digestion reaction 1h, and It is handled in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave, double-frequency ultrasound combination frequency is 20kHz/ 50kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;Extraction terminates Extracting solution is centrifuged 20min in 4500r/min afterwards, takes supernatant;40% drying aid is added in supernatant, controls inlet air temperature 160 DEG C, feed rate 400mL/h, atomizing pressure 160kPa, enter the wind flow 0.60m3Albumen is made in/min, vacuum spray drying Matter and dietary fiber mixed powder.
Embodiment six: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The preparation of the synchronous grape pip powder for extracting protein and dietary fiber, specifically includes the following steps: by after oil expression It is crushed after grape pip dregs of rice degreaser drying with Roughpulverizer, grape pip dregs of rice powder is obtained after crossing 40 meshes, by the grape pip dregs of rice powder of acquisition It is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1 is pulverized after mixing, Grape pip dregs of rice powder is placed in enzymatic vessel by revolving speed 10000r/min, grinding time 35min, deionized water is added, in parts by weight Meter, grape pip dregs of rice powder: deionized water 1:15 adjusts pH value 7.0 with NaOH the temperature was then adjusted to 40 DEG C, according to parts by weight, Papain: cellulase=2:3 obtains double enzyme preparations after mixing, is added 2.5% double enzyme preparations, enzyme digestion reaction 1h, and It is handled in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave, double-frequency ultrasound combination frequency is 30kHz/ 60kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;Extraction terminates Extracting solution is centrifuged 20min in 4500r/min afterwards, takes supernatant;40% drying aid is added in supernatant, controls inlet air temperature 170 DEG C, feed rate 400mL/h, atomizing pressure 150kPa, enter the wind flow 0.50m3Albumen is made in/min, vacuum spray drying Matter and dietary fiber mixed powder.
Embodiment seven: the preparation of the synchronous grape pip powder for extracting protein and dietary fiber
The preparation of the synchronous grape pip powder for extracting protein and dietary fiber, specifically includes the following steps: by after oil expression It is crushed after grape pip dregs of rice degreaser drying with Roughpulverizer, grape pip dregs of rice powder is obtained after crossing 40 meshes, by the grape pip dregs of rice powder of acquisition It is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1 is pulverized after mixing, Grape pip dregs of rice powder is placed in enzymatic vessel by revolving speed 10000r/min, grinding time 40min, deionized water is added, in parts by weight Meter, grape pip dregs of rice powder: deionized water 1:15 adjusts pH value 7.0 with NaOH the temperature was then adjusted to 40 DEG C, according to parts by weight, Papain: cellulase=3:1 obtains double enzyme preparations after mixing, is added 3% double enzyme preparations, enzyme digestion reaction 1h, and It is handled in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave, double-frequency ultrasound combination frequency is 30kHz/ 50kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min;Extraction terminates Extracting solution is centrifuged 20min in 4500r/min afterwards, takes supernatant;40% drying aid is added in supernatant, controls inlet air temperature 180 DEG C, feed rate 400mL/h, atomizing pressure 140kPa, enter the wind flow 0.40m3Albumen is made in/min, vacuum spray drying Matter and dietary fiber mixed powder.
Embodiment eight: the optimization preparation of the synchronous grape pip powder for extracting protein and dietary fiber
Prepare the grape pip powder rich in protein and dietary fiber respectively according to method described in embodiment one:
Scheme 1: grinding time 20min, papain: cellulase=1:2,1% double enzyme preparation additive amounts, double frequency ULTRASONIC COMPLEX frequency is 20kHz/60kHz, 140 DEG C of inlet air temperature, atomizing pressure 180kPa, enters the wind flow 0.80m3/min。
Scheme 2: grinding time 25min, papain: cellulase=2:2,1.5% double enzyme preparation additive amounts are double Frequency ULTRASONIC COMPLEX frequency is 20kHz/40kHz, 150 DEG C of inlet air temperature, atomizing pressure 170kPa, enters the wind flow 0.70m3/min。
Scheme 3: grinding time 30min, papain: cellulase=2:1,2% double enzyme preparation additive amounts, double frequency ULTRASONIC COMPLEX frequency is 20kHz/50kHz, 160 DEG C of inlet air temperature, atomizing pressure 160kPa, enters the wind flow 0.60m3/min。
Scheme 4: grinding time 35min, papain: cellulase=1:3,2.5% double enzyme preparation additive amounts are double Frequency ULTRASONIC COMPLEX frequency is 30kHz/60kHz, 170 DEG C of inlet air temperature, atomizing pressure 150kPa, enters the wind flow 0.50m3/min。
Scheme 5: grinding time 40min, papain: cellulase=3:1,3% double enzyme preparation additive amounts, double frequency ULTRASONIC COMPLEX frequency is 30kHz/50kHz, 180 DEG C of inlet air temperature, atomizing pressure 140kPa, enters the wind flow 0.40m3/min。
The grape pip powder rich in protein and dietary fiber prepared on above-mentioned experiment basis carries out extraction rate of protein With the evaluation of dietary fiber recovery rate.
1. measuring method
(1) protein Coomassie brilliant G-250 in protein content determination measurement grape pip powder.Calculation formula are as follows:
(2) measurement and calculating of dietary fiber are referring to national standard: GB 5009.88-2014 is measured.Calculation formula Are as follows:
2. the grape pip powder manufacture craft that response surface is rich in protein and dietary fiber
Experiment of single factor is designed, is probed into the grape pip powder preparation method rich in protein and dietary fiber respectively when crushing Between, papain: the ratio of cellulase, double enzyme preparation additive amounts and double-frequency ultrasound combination frequency to extraction rate of protein and The influence of dietary fiber recovery rate.The experiment of four factors, three horizontal respone face, response interview are carried out on the basis of experiment of single factor It tests factor and water-glass is shown in Table 1.
Table 1: response surface experiments factor and water-glass
The response surface optimization that ferments is analyzed: comprehensive single factor experiment is as a result, using Box-Behnken Responds Surface Methodology to it It optimizes.Response surface experiments design and response the results are shown in Table 2.
Table 2: response surface optimization test result
Multiple regression equation fitting is carried out by 2 test data of table, can be established with extraction rate of protein (Y1) and dietary fiber Yield (Y2) respectively to grinding time (A), papain: the ratio (B) of cellulase, double enzyme preparation additive amounts (C) and double The fit equation of frequency ULTRASONIC COMPLEX frequency (D) are as follows:
Y1=82.92+3.19A+2.39B+1.02C+0.072D-5.78AB-2.67AC-0.76AD-3.44 BC+ 0.085BD+2.0CD-17.67A2-9.24B2-5.06C2-3.57D2
Y2=36.36-0.40A-0.34B-0.21C+0.19D-2.26AB-1.39AC-0.033AD-1.7B C-0.41BD+ 0.24CD-9.54A2-4.92B2-3.34C2-3.39D2
Table 3: extraction rate of protein response surface experiments result and variance analysis
Note: " * " indicates significant (0.01 < p < 0.05);" * * " indicates extremely significant (p < 0.01).
Table 4: dietary fiber yield response surface experiments result and variance analysis
Note: " * " indicates significant (0.01 < p < 0.05);" * * " indicates extremely significant (p < 0.01).
The conspicuousness that each variable influences index (response) in regression equation is determined, the value of probability P is got over by F inspection Small, then the significance degree of relevant variable is higher.By table 3, table 4 it is found that when model F value is respectively F=29.77, F=35.28, P < 0.0001, illustrate that model is extremely significant.When the quasi- item of the mistake of extraction rate of protein and dietary fiber yield is respectively F=1.22, P =0.4587 > 0.05, F=5.66, it is not significant that P=0.0547 > 0.05 illustrates that model loses quasi- item.The coefficient of determination is respectively R2= 0.9675, R2=0.9728, correction coefficient is respectively R2 Adj=0.9350, R2 Adj=0.9457 show measured value and predicted value it Between have good degree of fitting.It is possible thereby to which the foundation for illustrating model illustrates that the fitting degree of this model is preferable in conspicuousness, try It tests that operation is accurate credible, therefore can use this model to the manufacture craft mistake rich in protein and the grape pip powder of dietary fiber Journey is analyzed and predicted.
It is fixed not in other factors in order to investigate influence of each interactive item to extraction rate of protein and dietary fiber yield In the case where change, operation is carried out to regression equation using 8.05 software of Design-Expert, makes the response surface figure of interactive item Referring to shown in attached drawing 6 to attached drawing 11.
It is analyzed by software Design-Expert 8.05 and considers that practical operation is convenient, choose grinding time 30min, pawpaw Protease: ratio=2:1 of cellulase, double enzyme preparation additive amounts are 2% and double-frequency ultrasound combination frequency is 20kHz/ 50kHz carries out 3 parallel tests, and extraction rate of protein average value is 85.21% and dietary fiber yield average value is 36.54%, the mathematical model to optimization the compoiste fermented drink technological condition for fermentation of grape pip chick-pea be it is feasible, have it is practical Value.
3. the grape pip powder manufacture craft that orthogonal optimization is rich in protein and dietary fiber
Experiment of single factor is designed, probes into enter the wind temperature in the grape pip powder preparation method rich in protein and dietary fiber respectively The influence of degree, atomizing pressure and air inlet flow to extraction rate of protein and dietary fiber recovery rate.On the basis of experiment of single factor Upper progress Three factors-levels orthogonal experiment, orthogonal test factor and water-glass are shown in Table 5.
Table 5: orthogonal test factor and water-glass
Grape pip powder manufacture craft test result and analysis of the orthogonal optimization rich in protein and dietary fiber are shown in Table 6 and table 7。
Table 6: orthogonal experiments and analysis
Table 7: orthogonal experiments and analysis
From table 6 and table 7 as can be seen that in the range of experimental design, influence of the inlet air temperature to extraction rate of protein is most Greatly, influence of the atomizing pressure to cellulose recovery rate is maximum.Obtaining optimum optimizing condition in conjunction with table 6 and table 7 is A2B2C2, i.e., into Air temperature be 160 DEG C, atomizing pressure 160kPa and air inlet flow 0.6m3When/min, extraction rate of protein and dietary fiber are extracted Rate highest.
Obtained using response surface software and orthogonal test, using extract equipment provided by the invention production rich in protein and The best conditions of preparation pr ocess of the grape pip powder of dietary fiber is respectively as follows: grinding time 30min, papain: cellulase Ratio=2:1, double enzyme preparation additive amounts be 2% and double-frequency ultrasound combination frequency be 20kHz/50kHz, inlet air temperature 160 DEG C, atomizing pressure 160kPa and air inlet flow 0.6m3When/min, extraction rate of protein and dietary fiber recovery rate highest.
Embodiment eight: the grape pip powder physical and chemical index rich in protein and dietary fiber
(1) protein solubility
The dissolubility of protein is the most important functional character of phytoprotein, and other properties of protein are as blistered Property, emulsibility etc. all rely on the dissolubility of protein, influence protein solubility factor include processing conditions, temperature, pH, Ionic strength etc..The dissolubility for grasping albumen under different pH value is conducive to instruct its application in different food products system.Pass through Under different pH environments, the multiplex-enzyme extraction obtained to conventional base leach protein grape pip powder and this programme is rich in protein and meals The influence for eating the solubility of the grape pip powder of fiber, as a result referring to attached drawing 12, as seen from the figure, alkali carries albumen grape pip powder and compound Enzyme extracts that the grape pip powder rich in protein and dietary fiber is minimum in pH 4.0 and pH3.0 solubility respectively, hereafter albumen Solubility increases with the increase of pH.The dissolubility of grape pip powder of the multiplex-enzyme extraction rich in protein and dietary fiber is obvious Better than alkali carries albumen grape pip powder, in pH7, solubility reaches grape pip powder of the multiplex-enzyme extraction rich in protein and dietary fiber To 36.04%.Dissolubility is relatively not used comparing for technology in the present invention and improves 8% or more.This is because the hydrolysis of protease Effect, protein structure are changed, and polypeptide chain fracture is exposed the carboxyl of ionization therein and amino, the polarity of molecule Increase, hydrophilic interaction enhancing between protein-protein, the multiplex-enzyme extraction for being is rich in the grape pip of protein and dietary fiber The dissolubility of powder improves.
(2) jitter time
Table 8: when the dispersion rich in protein and dietary fiber grape pip powder of alkali carries albumen grape pip powder and multiplex-enzyme extraction Between compare
Alkali carries albumen grape pip powder Multiplex-enzyme extraction is rich in the grape pip powder of protein and dietary fiber
Jitter time/s 52.38±1.67 39.29±2.12
Pass through point of the grape pip powder to alkali carries albumen grape pip powder and multiplex-enzyme extraction rich in protein and dietary fiber The scattered time is tested, and test result ginseng is shown in Table 8, and the jitter time of the two has significant difference, and multiplex-enzyme extraction is rich in egg The jitter time of white matter and the grape pip powder of dietary fiber is 39.29 ± 2.12s, and the jitter time of alkali carries albumen grape pip powder For 52.38 ± 1.67s, then compared with shortening 25% or more.
A kind of grape pip powder and preparation method thereof rich in protein and dietary fiber provided by this method, according to Portugal Grape seed dregs of rice feature, the dual-frequency ultrasonic wave of use assist double enzyme enzymatic isolation methods extract protein and dietary fiber, vacuum spray drying and The sport technique segments such as corresponding superfine communication technique processing have it is progressive, it is closely coupled.The present invention is squeezed for from grape pip Grouts after oil are raw material, and preparation is rich in the grape pip powder of protein and dietary fiber, are obtained, are used by the way that test is repeated several times Dual-frequency ultrasonic wave assists double enzyme enzymatic isolation methods to extract protein and dietary fiber, vacuum spray drying and corresponding superfine communication technique Mutually auxiliary interdependent, organic linking between each sport technique segment is handled, it is whole inseparable, it can just obtain method of the invention and produce to obtain Protein and dietary fiber mixed powder compared with the product that common enzyme process and single-frequency ultrasonic extraction produces both at home and abroad, tool The advantages that textured uniform, mouthfeel silk is sliding, good smell, while microorganism and other sanitary indexs meet relevant criterion.And The recovery rate of protein and dietary fiber largely has biggish promotion, and wherein dissolubility is relatively not used in the present invention Technology compared to improving 8% or more, jitter time then compared with shortening 25% or more.Grape pip dregs of rice added value of product is improved, There is wide applicability and Development volue using grape liquor-making byproduct field.
As described above, the present invention can be realized preferably, the above embodiments are only to preferred implementation side of the invention Formula is described, and is not intended to limit the scope of the present invention, and without departing from the spirit of the design of the present invention, this field is general The various changes and improvement that logical technical staff makes technical solution of the present invention, should all fall into present invention determine that protection scope It is interior.

Claims (10)

1. a kind of synchronous grape pip powder for extracting protein and dietary fiber, which is characterized in that pass through preparation side in detail below Method prepares, specific preparation method the following steps are included:
(1) it pre-processes: will be crushed after the grape pip dregs of rice degreaser drying after oil expression with Roughpulverizer, obtain grape pip after crossing 40 meshes Dregs of rice powder, it is spare;
(2) it pulverizes: the grape pip dregs of rice powder that step (1) obtains being mixed with zirconium oxide balls, is pulverized, by its powder Broken is the grape pip dregs of rice powder rich in protein and dietary fiber that partial size is 10 μm;
(3) double enzymolysis is synchronous extracts: grape pip dregs of rice powder prepared by step (2) being placed in enzymatic vessel, is added into grape pip dregs of rice powder Enter deionized water, the temperature was then adjusted to 40 DEG C, adjusts pH value 7.0 with NaOH, addition is made of papain and cellulase Double enzyme preparations, enzyme digestion reaction 1h, and in protein extraction process synchronous with dietary fiber using dual-frequency ultrasonic wave handle, mention Extracting solution is centrifuged 20min in 4500r/min after taking, takes supernatant;
(4) vacuum spray drying: 40% drying aid is added in the supernatant that step (3) are obtained, and controls 160 DEG C of inlet air temperature, into Stream amount 400mL/h, atomizing pressure 160kPa enter the wind flow 0.60m3/min;Protein and dietary fiber mixed powder is made;
(5) Special integrated device is used in the synchronous extraction of above-mentioned ultramicro grinding, double enzymolysis and vacuum spray drying technique.
2. a kind of synchronous grape pip powder for extracting protein and dietary fiber as described in claim 1, which is characterized in that described Grape pip dregs of rice powder is mixed with zirconium oxide balls, according to parts by weight, zirconium oxide balls: grape pip dregs of rice powder=6:1.
3. a kind of synchronous grape pip powder for extracting protein and dietary fiber as described in claim 1, which is characterized in that described The condition of ultramicro grinding is revolving speed 10000r/min, grinding time 30min.
4. a kind of synchronous grape pip powder for extracting protein and dietary fiber as described in claim 1, which is characterized in that described According to parts by weight, papain: cellulase=2:1 obtains double enzyme preparations to double enzyme preparations after mixing.
5. a kind of synchronous grape pip powder for extracting protein and dietary fiber as described in claim 1, which is characterized in that described The additive amount of double enzyme preparations is 2%.
6. a kind of synchronous grape pip powder for extracting protein and dietary fiber as described in claim 1, which is characterized in that described Dual-frequency ultrasonic wave treatment conditions are that double-frequency ultrasound combination frequency is 20kHz/50kHz, sound intensity 0.4W/cm2, action time 20s, intermittent time 30s are stirred by conditions above and are extracted 60min.
7. a kind of collection pulverizes, double enzymolysis synchronizes extraction and vacuum spray drying Special integrated device, including enzyme digestion reaction Tank, micronizer, Roughpulverizer, solid-liquid separating machine, fluid reservoir and vacuum spray dehydrator, which is characterized in that the enzyme It solves reactor tank side and micronizer is set, Roughpulverizer, Roughpulverizer and micronizer is arranged in the micronizer other side It is connected by first pipe, enzyme digestion reaction tank is connect with micronizer by screw elevator, is passed through below enzyme digestion reaction tank Second pipe connects solid-liquid separating machine, and fluid reservoir is arranged by solid-liquid separating machine, and fluid reservoir is true by water pump and pump tube connection Empty spray dryer, the grape pip dregs of rice can be made by coarse crushing, ultramicro grinding, the synchronous extraction of double enzymolysis, vacuum spray drying Protein and dietary fiber mixed powder.
8. integrated device as claimed in claim 7, which is characterized in that the enzyme digestion reaction tank includes tank body, and tank body is in Motor is arranged in capsule shape type, top of the tank, and axis is stirred in setting in tank body, and agitating shaft is stirred bracing strut and is hung vertically in tank body Inside, and connect with the motor of top of the tank by shaft coupling, paddle is set on agitating shaft, and paddle is using agitating shaft as axis It is symmetric, paddle, which is equipped on the outside of hydrophobic coating tank body, is arranged control panel.
9. integrated device as claimed in claim 7, which is characterized in that the enzyme digestion reaction tank top two sides setting Deionized water interface and note enzymatic hydrolysis liquid interface are infused, note deionized water interface leads to tank body, and note enzymatic hydrolysis liquid interface connects tank body Interior spraying rack.
10. integrated device as claimed in claim 7, which is characterized in that machine is arranged below the enzyme digestion reaction tank Frame, double-frequency ultrasound wave producer is arranged in rack, and double-frequency ultrasound wave producer and ultrasonic oscillator are electrically connected.
CN201910223668.5A 2019-03-22 2019-03-22 Synchronous grape pip powder, preparation and the dedicated unit for extracting protein and dietary fiber Pending CN109874999A (en)

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EP4256968A3 (en) * 2021-07-16 2024-01-10 Voyage Foods, Inc. Chocolate replicas produced from individual components

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