CN109912670A - A kind of method and device for extracting the anthocyanin containing selenium by purple potato - Google Patents
A kind of method and device for extracting the anthocyanin containing selenium by purple potato Download PDFInfo
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- CN109912670A CN109912670A CN201910266831.6A CN201910266831A CN109912670A CN 109912670 A CN109912670 A CN 109912670A CN 201910266831 A CN201910266831 A CN 201910266831A CN 109912670 A CN109912670 A CN 109912670A
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- purple potato
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- anthocyanin
- containing selenium
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- 239000004410 anthocyanin Substances 0.000 title claims abstract description 79
- 235000010208 anthocyanin Nutrition 0.000 title claims abstract description 79
- 229930002877 anthocyanin Natural products 0.000 title claims abstract description 79
- 150000004636 anthocyanins Chemical class 0.000 title claims abstract description 78
- 235000004976 Solanum vernei Nutrition 0.000 title claims abstract description 64
- 241000352057 Solanum vernei Species 0.000 title claims abstract description 64
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 30
- 239000011669 selenium Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000000605 extraction Methods 0.000 claims abstract description 41
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 claims abstract description 7
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 43
- 238000003860 storage Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 12
- 244000061456 Solanum tuberosum Species 0.000 claims description 8
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 210000002615 epidermis Anatomy 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 230000001360 synchronised effect Effects 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 abstract description 45
- 230000004044 response Effects 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006467 substitution reaction Methods 0.000 abstract description 5
- 235000019441 ethanol Nutrition 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 239000000243 solution Substances 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- 239000000284 extract Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000011260 aqueous acid Substances 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- 239000000049 pigment Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- -1 has petunia pigment Chemical compound 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- VEVZSMAEJFVWIL-UHFFFAOYSA-O cyanidin cation Chemical compound [O+]=1C2=CC(O)=CC(O)=C2C=C(O)C=1C1=CC=C(O)C(O)=C1 VEVZSMAEJFVWIL-UHFFFAOYSA-O 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009533 lab test Methods 0.000 description 2
- KZMACGJDUUWFCH-UHFFFAOYSA-O malvidin Chemical compound COC1=C(O)C(OC)=CC(C=2C(=CC=3C(O)=CC(O)=CC=3[O+]=2)O)=C1 KZMACGJDUUWFCH-UHFFFAOYSA-O 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
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- GCPYCNBGGPHOBD-UHFFFAOYSA-N Delphinidin Natural products OC1=Cc2c(O)cc(O)cc2OC1=C3C=C(O)C(=O)C(=C3)O GCPYCNBGGPHOBD-UHFFFAOYSA-N 0.000 description 1
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- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 244000170916 Paeonia officinalis Species 0.000 description 1
- 235000006484 Paeonia officinalis Nutrition 0.000 description 1
- 240000007377 Petunia x hybrida Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000010933 acylation Effects 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 229930014669 anthocyanidin Natural products 0.000 description 1
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- 235000007242 delphinidin Nutrition 0.000 description 1
- FFNDMZIBVDSQFI-UHFFFAOYSA-N delphinidin chloride Chemical compound [Cl-].[O+]=1C2=CC(O)=CC(O)=C2C=C(O)C=1C1=CC(O)=C(O)C(O)=C1 FFNDMZIBVDSQFI-UHFFFAOYSA-N 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
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- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical compound N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Landscapes
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention belongs to purple potatos to extract the technical field of anthocyanin containing selenium, and in particular to the method and device of the anthocyanin containing selenium is extracted by purple potato.Include the following steps: that step 1) is cleaned, stripping and slicing；Step 2, which immerses purple potato ball, to be added in extracting solution；The extracting solution is made of phosphatase 11-2%, water 98%-99%；Step 3) ultrasonic dissolution assisting；Ultrasonic dissolution assisting is carried out using the mixture that Ultrasound Instrument forms step 2;Step 4) filtering extraction filtrate is spare, repeats step 2-step 3), repeats 2-4 times；Step 5) purification；Filtrate described in step 4) is separated, anthocyanin containing selenium is extracted.The beneficial effects of the present invention are: water consumption substitution ethyl alcohol, it is at low cost with phosphoric acid substitution citric acid；Assisting ultrasonic device, extraction efficiency are high；Optimum ratio and ultrasonic time are chosen as response parameter, plays unexpected technical effect；High using automatic control equipment operation precision, labor intensity is low.
Description
Technical field
The invention belongs to purple potatos to extract the technical field of anthocyanin containing selenium, and in particular to extract pattern containing selenium by purple potato
The method and device of glycosides.
Background technique
Anthocyanidin be the flowers of many plants, leaf, fruit colors, not only have it is anti-oxidant, remove free radical, be anti-
Cancer, the anti-inflammatory and bioactivity such as antibacterial, and it is bright in colour, have no toxic side effect, be widely used in food, medicine and health care product
Industry.
Purple potato (Purple potato), epidermis and potato meat are atropurpureus, are the new varieties introduced in recent years, at me
State is planted experimentally in some places.98% is acylated anthocyanin in purple potato anthocyanin, and aglycon mainly has petunia pigment, Chinese herbaceous peony
Pigment, malvidin and delphinidin.Research about purple potato anthocyanin also rests on constituent analysis and anti-oxidant, clear
In terms of free radical activity.
The extracting method of anthocyanin mainly has extraction, ultrasonic wave added method, microwave assisting method etc..In order to increase anthocyanin
Stability, is often added certain density acid in Extraction solvent, but in order to avoid the hydrolysis of the anthocyanin of acylation, be typically chosen compared with
Weak acid such as citric acid.Citric acid is polynary middle strong acid, has preferable color-protecting function to anthocyanin, but on the high side, causes
The production cost of anthocyani pigment is higher.Phosphoric acid is also polyacid, and with citric acid similar temperament, but price is low.Therefore, herein
Investigate the technical parameter of anthocyanin in phosphoric acid ultrasound assisted extraction purple potato, it is intended to provide for its further research and development
Foundation.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of methods and dress that the anthocyanin containing selenium is extracted by purple potato
It sets, it being capable of low-intensity, low cost, high-precision, efficient extraction anthocyanin.
The invention discloses a kind of methods for extracting the anthocyanin containing selenium by purple potato, based on mass fraction, including it is as follows
Step:
Step 1) cleaning, stripping and slicing；Clean, the stripping and slicing after epidermis natural air drying by new light violet potato cleaning；
Step 2), which immerses purple potato ball, to be added in extracting solution；The extracting solution is by phosphatase 11-2%, water 98%-99%
Composition；
Step 3) ultrasonic dissolution assisting；Ultrasonic dissolution assisting is carried out using the mixture that Ultrasound Instrument forms step 2)；
Step 4) filtering extraction filtrate is spare, repeats step 2)-step 3), repeats 2-4 times；
Step 5) purification；Step 4) the filtrate is separated, anthocyanin containing selenium is extracted.
Preferably, based on mass fraction, the extracting solution has phosphatase 11 .5%, and water 98.5% forms.
Further, the solid-liquid ratio of the purple potato ball and the extracting solution is 1:3-1:8 (g/L).
Preferably, the solid-liquid ratio of the purple potato ball and the extracting solution is 1:5 (g/L).
Further, the step 3) ultrasonic time is 20min.
The invention also discloses a kind of devices that the anthocyanin containing selenium is extracted by purple potato, including extraction element, configuration dress
It sets, register；
The extraction element includes extractor, Vltrasonic device is provided on the extractor, when the Vltrasonic device is opened
Between according to setting automatically control；Be provided with feeding-in solid body mouth, liquid inlet opening, discharge port on the extractor, the solid into
Material mouth setting exists in the extractor top, the liquid inlet opening setting in the extractor top, the discharge port setting
The extractor lower part；Thermometer is set on the extractor, for measuring the extractor internal temperature；
The configuration device includes two storage tanks, preparing tanks；Two outlets are connected with the preparing tank respectively；
The preparing tank outlet is connected with the liquid inlet opening；It is provided with liquidometer on the storage tank, is arranged at the outlet
There is switch valve；Two storage tanks are respectively provided with phosphoric acid, water；The preparing tank exit is provided with metering valve, the metering valve
According to default inlet amount unlatching/closing；
Register is set on the extractor, and the register is using in collet, coil pipe, electric heater unit at least one
Kind, the collet, coil pipe are exchanged heat by internal heating agent with material in the extractor, the heat exchange include heat with/
Or cooling.
Further, the extraction element further includes blender, and the whip switch switchs phase with the Vltrasonic device
It is chain, the synchronous unlatching/closing of the two.The blender is arranged on the extractor for promoting the extractor materials inside
It is uniformly mixed.
Further, the detection device further includes pH meter, and the pH meter is arranged on the extractor for measuring institute
State extractor internal pH-values.
Further, the extractor uses at least one of tube extractor, autoclave extractor.
Further, the liquidometer is connected lock with the switch valve opening.When liquidometer liquid level difference reaches preset value, institute
Switch valve is stated to be automatically closed.
Further, the device that the anthocyanin containing selenium is extracted by purple potato further includes feeding-in solid body device, further includes
Feeding-in solid body device, it includes solid that the feeding-in solid body device, which exports the feeding-in solid body device that is connected with the feeding-in solid body mouth,
Storage tank, solids feeder；The solids feeder import is connected with the solid outlet, solids feeder outlet with
The feeding-in solid body mouth is connected.
Further, the solid tank bottom is taper, and the solid outlet is arranged in taper bottommost.
Further, the solids feeder uses at least one of conveyer belt, screw-feeder.
Further, the thermometer switchs mutually chain with the register；
When the register uses collet and/or coil pipe, the thermometer is exported with the register and/or entrance
Valve opening is mutually chain, by automatically adjusting the valve opening A.T.C；
When the register uses electric heater unit, the thermometer and the heat-exchange device electric current are mutually chain, lead to
It crosses and automatically adjusts the size of current A.T.C.
Further, the device that the anthocyanin containing selenium is extracted by purple potato further includes alarm, the alarm with
The detection device is mutually chain, and when the numerical value of the detection device is more than preset value, the alarm is alarmed.The liquid level
The alarm is alarmed when meter liquid level is more than highest preset value and/or minimum predetermined value；The thermometer is more than preset value
When, the alarm is alarmed.
Further, the device that the anthocyanin containing selenium is extracted by purple potato further includes filter device, the filtering dress
It sets and is connected with the discharge port.For the filter device for the solid impurity particle in filtering product, filtrate is that product can be with
It is directly canned to sell outside.
In use, phosphoric acid, water is added into the storage tank respectively, purple potato ball is added in the solid storage tank, in advance
Allocation ratio (1-2%), the solid-liquid ratio (1:3-1:8 (g/L)) of phosphoric acid and water are set.Under the control of robot control system(RCS), according to such as
Lower step is automatically brought into operation:
Quantitatively from addition water, phosphoric acid, the formation extraction in the preparing tank into the extractor in the wet tank
Liquid；
It is quantitative by the preparing tank quantitatively from the solid feeding device to the extractor quantification purple potato ball
Extracting solution is added into the extractor and opens stirring, Vltrasonic device；Filtrate filtered out by filter after extraction stand-by, filter residue
It repeats to extract again, repeat 2-4 times.
The beneficial effects of the present invention are:
1, water consumption substitution ethyl alcohol, it is at low cost with phosphoric acid substitution citric acid；
2, assisting ultrasonic device, extraction efficiency are high；
3, optimum ratio and ultrasonic time are chosen as response parameter, plays unexpected technical effect；
4, high using automatic control equipment operation precision, labor intensity is low.
Detailed description of the invention
Fig. 1 extracts aqueous acid to the influence diagram of purple potato anthocyanin extraction efficiency；
Purple potato anthocyanin content is with phosphoric acid concentration variation diagram in Fig. 2 extraction aqueous acid；
Purple potato anthocyanin content is with solid-liquid ratio variation diagram in Fig. 3 extraction aqueous acid；
Purple potato anthocyanin content is with ultrasonic time variation diagram in Fig. 4 extraction aqueous acid；
Fig. 5 phosphoric acid concentration and ultrasonic time interaction response plan view；
Fig. 6 phosphoric acid concentration and solid-liquid ratio interaction response plan view；
Fig. 7 ultrasonic time and solid-liquid ratio interaction response plan view；
Fig. 8 is attachment structure schematic diagram of the present invention；
Fig. 9 is reaction unit structural schematic diagram of the present invention；
Figure 10 is feeding-in solid body apparatus structure schematic diagram of the present invention.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment 1
The invention discloses a kind of methods for extracting the anthocyanin containing selenium by purple potato, based on mass fraction, including it is as follows
Step:
Step 1) cleaning, stripping and slicing；Clean, the stripping and slicing after epidermis natural air drying by new light violet potato cleaning；
Step 2), which immerses purple potato ball, to be added in extracting solution；The extracting solution is by phosphatase 11-2%, water 98%-99%
Composition；
Step 3) ultrasonic dissolution assisting；Ultrasonic dissolution assisting is carried out using the mixture that Ultrasound Instrument forms step 2)；
Step 4) filtering extraction filtrate is spare, repeats step 2)-step 3), repeats 2-4 times；
Step 5) purification；Step 4) the filtrate is separated, anthocyanin containing selenium is extracted.
Preferably, based on mass fraction, the extracting solution has phosphatase 11 .5%, and water 98.5% forms.
Described in the present embodiment, the solid-liquid ratio of the purple potato ball and the extracting solution is 1:3-1:8 (g/L).
Preferably, the solid-liquid ratio of the purple potato ball and the extracting solution is 1:5 (g/L).
Described in the present embodiment, the step 3) ultrasonic time is 20min.
The invention also discloses a kind of devices that the anthocyanin containing selenium is extracted by purple potato, including extraction element 1, configuration dress
Set 2, register 3；
The extraction element 1 includes extractor 11, is provided with Vltrasonic device 12, the Vltrasonic device on the extractor 11
12 opening times automatically controlled according to setting；It is provided with feeding-in solid body mouth 111 on the extractor 11, liquid inlet opening 112, goes out
Material mouth 113, the setting of feeding-in solid body mouth 111 are mentioned in 11 top of extractor, the setting of liquid inlet opening 112 described
11 top of device is taken, the discharge port 113 is arranged in 11 lower part of extractor；Thermometer 114 is set on the extractor 11, is used
In measurement 11 internal temperature of extractor；
The configuration device 2 includes two storage tanks 21, preparing tank 22；Two storage tanks 21 outlets respectively with the preparation
Tank 22 is connected；The outlet of preparing tank 22 is connected with the liquid inlet opening 112；It is provided with liquidometer 211 on the storage tank 21,
21 exit of storage tank is provided with switch valve；Two storage tanks 21 are respectively provided with phosphoric acid, water；22 exit of preparing tank
It is provided with metering valve 221, the metering valve 221 is according to default inlet amount unlatching/closing；
Register 3 is set on the extractor 11, the register 3 using in collet, coil pipe, electric heater unit extremely
One kind less, the collet, coil pipe are exchanged heat by internal heating agent with material in the extractor 11, and the heat exchange includes adding
Heat and/or cooling.
Described in the present embodiment, the extraction element 1 further includes blender, the whip switch and the Vltrasonic device
12 switches are mutually chain, the synchronous unlatching/closing of the two.The blender is arranged on the extractor 11 for promoting the extraction
11 materials inside of device is uniformly mixed.
Described in the present embodiment, the detection device further includes pH meter, and the pH meter setting is used on the extractor 11
In measurement 11 internal pH-values of extractor.
Described in the present embodiment, the extractor 11 uses at least one of tube extractor 11, autoclave extractor 11.
Described in the present embodiment, the liquidometer 211 is connected lock with the switch valve opening.211 liquid level difference of liquidometer reaches
When to preset value, the switch valve is automatically closed.
Described in the present embodiment, the device that the anthocyanin containing selenium is extracted by purple potato further includes feeding-in solid body device,
The feeding-in solid body device includes solid storage tank, solids feeder；The solids feeder import and the solid outlet
It is connected, the solids feeder outlet is connected with the feeding-in solid body mouth 111.
Described in the present embodiment, the solid tank bottom is taper, and the solid outlet is arranged at taper most bottom
Portion.
Described in the present embodiment, the solids feeder uses at least one of conveyer belt, screw-feeder.
Described in the present embodiment, the thermometer 114 switchs mutually chain with the register 3；
When the register 3 is using collet and/or coil pipe, the thermometer 114 exported with the register 3 and/
Or inlet valve aperture is mutually chain, by automatically adjusting the valve opening A.T.C；
When the register 3 is using electric heater unit, the thermometer 114 is connected with the heat-exchange device electric current
Lock, by automatically adjusting the size of current A.T.C.
Described in the present embodiment, the device that the anthocyanin containing selenium is extracted by purple potato further includes alarm, the report
Alert device and the detection device are mutually chain, and when the numerical value of the detection device is more than preset value, the alarm is alarmed.Institute
The alarm is alarmed when stating 211 liquid level of liquidometer more than highest preset value and/or minimum predetermined value；The thermometer
114 be more than preset value when, the alarm is alarmed.
Described in the present embodiment, the device that the anthocyanin containing selenium is extracted by purple potato further includes filter device, described
Filter device is connected with the discharge port 113.The filter device is used for the solid impurity particle in filtering product, and filtrate is
Product directly canned can be sold outside.
In use, phosphoric acid, water is added into the storage tank 21 respectively, purple potato ball is added in the solid storage tank, in advance
Allocation ratio (1-2%), the solid-liquid ratio (1:3-1:8 (g/L)) of phosphoric acid and water are first set.Under the control of robot control system(RCS), according to
Following steps are automatically brought into operation:
It is quantitative from adding water, phosphoric acid, the shape in the preparing tank 22 into the extractor 11 in the wet tank 21
At extracting solution；
It is quantitative by the preparing tank quantitatively from the solid feeding device to the 11 quantification purple potato ball of extractor
Extracting solution is added in 22 into the extractor 11 and opens stirring, Vltrasonic device 12；Filtrate is filtered out by filter after extraction
For use, filter residue repeats to extract again, repeats 2-4 times.
The determination of response parameter:
In order to determine that preferred response parameter spy has done following experiment:
1 materials and methods
1.1 materials and reagent
1.1.1 material and reagent
Purple potato, purchase cultivate plantation farm in Dingxi, Gansu potato.Phosphoric acid, acetic acid, citric acid, hydrochloric acid are anhydrous
Ethyl alcohol is Sinopharm Chemical Reagent Co., Ltd..
2.1.2 instrument and equipment
SB25-12DTN supersonic wave cleaning machine, NingBo XinZhi Biology Science Co., Ltd；RE52AA rotary evaporator,
Shanghai Yarong Biochemical Instrument Plant；UNICO2000 visible spectrophotometer, the Shanghai You Nike Co., Ltd；AX-200 type ten thousand/
One electronic balance, Japanese Shimadzu Philippines company.
1.2 experimental method
1.2.1 anthocyanin content is analyzed
Show poor method analysis anthocyanin content with pH.Appropriate extracting solution is taken to use the buffer solution of pH=1.0, pH=4.5 respectively
Constant volume 10mL surveys light absorption value under 520,700nm wavelength, anthocyanin yield is calculated as follows.
Anthocyanin yield (mg/g)=AMWDFV/ ε Lm
In formula: A=(A520-A700) PH=1-(A520–A700)PH=4.5；MW, anthocyanin are 3- galactolipin cornflowerblue
The molal weight meter (449.2g/moL) of element；Molar extinction coefficient (the 26900L/mol of ε, 3- galactolipin cyanidin
cm)；V, liquor capacity (mL)；L, cuvette thickness (1cm)；DF, extension rate；M, the quality (g) of purple potato.
1.2.2 the screening of Extraction solvent
Fresh potato is eluted with water, and 2mm graininess is cut into after epidermis natural air drying.Weigh 8 parts of (every part of 1g) purple Ma Ling
Potato particle is put into conical flask, be separately added into 0.25% hydrochloric acid of 10mL, 0.50% hydrochloric acid, 0.75% phosphoric acid, 1.50% phosphoric acid,
2.0% citric acid, 3.0% citric acid, 3.0% acetic acid, 4.0% acetic acid, room temperature ultrasonic extract 20min.Filter is collected in filtering
Liquid measures anthocyanin content, calculated yield.
1.2.3 experiment of single factor
Investigate phosphoric acid concentration (0.25,0.5,0.75,1.0,1.25,1.5%), ultrasonic time (5,7.5,10,15,2.,
25,30min), solid-liquid ratio (1:2,1:3,1:4,1:5,1:6,1:7,1:8g/mL) is to the shadow for extracting anthocyanin in purple potato
It rings.
1.2.4 response surface optimization
According to experiment of single factor as a result, phosphoric acid concentration (A), three ultrasonic time (B), solid-liquid ratio (C) factors are determined, with flower
Color glycosides yield is response, using Box-Behnken method design experiment in Design-Expert 8.0.6 software.Experiment is set
The factor level and coding such as table 1 of meter.
1 response surface design factor of table is horizontal and encodes
1.2.5 confirmatory experiment
According to response phase method optimal conditions, three parallel laboratory tests that purple potato anthocyanin is extracted are carried out.
2 results and analysis
2.1 experiment of single factor
2.1.1 the screening of Extraction solvent
Inventor primarily looks at Extraction solvent hydrochloric acid (quality point on the basis of existing anthocyanins pigment from purple sweet potato extractive technique
Number 0.25%, 0.50%), phosphoric acid (0.75%, 1.50%), citric acid (2.0%, 3.0%), acetic acid (3.0%, 4.0%) it is several
Kind acidic aqueous solution, extraction under conditions of solid-liquid ratio is 1:10, ultrasonic time is 20min, to anthocyanin in purple potato
Effect, as a result as shown in Figure 1.Extract influence (HCA1,0.25% salt of the aqueous acid to purple potato anthocyanin extraction efficiency
Acid；HCA1,0.50% hydrochloric acid；PHA1,0.75% phosphoric acid；PHA2,1.50% phosphoric acid；CA1,2.0% citric acid；CA2,3.0%
Citric acid；AA1,3.0% acetic acid；AA2,4.0% acetic acid).
As shown in Figure 1, hydrochloric acid can reach preferable effect to the extraction of purple potato anthocyanin under lower concentration, but
In view of the volatility of hydrochloric acid, industrial production is not suitable for.Acetic acid is needed to can be only achieved preferable extract using high concentration and imitated
Fruit.Industrially common 3.0% aqueous citric acid solution extracts anthocyanin, although effect is preferable, production cost is higher.And 1.50%
It is preferably close that phosphoric acid and 3.0% aqueous citric acid solution extraction anthocyanin obtain effect.In addition, acidity (the ka of phosphoric acid1=7.11 × 10-3,ka2=6.23 × 10-8,ka3=4.50 × 10-13) and citric acid (ka1=7.44 × 10-4,ka2=1.73 × 10-5,ka3=
4.02×10-7) close, and both there is preferable complexing power.Therefore, phosphoric acid is selected to extract.
2.1.2 phosphate aqueous solution extracts the influence factor of anthocyanin
In order to primarily determine the extraction conditions range of response surface optimization, experiment of single factor has been carried out first, experimental result is such as
Shown in Fig. 2-4.The result shows that: under the conditions of solid-liquid ratio 1:10, extraction time 20min, with phosphoric acid concentration (0.25,0.5,
0.75,1.0,1.25,1.5%) increase, the content of anthocyanin is presented in extracting solution first rise after downward trend, in phosphoric acid
Anthocyanin yield reaches maximum value when concentration is 1%.Then, right under conditions of phosphoric acid concentration 1%, ultrasonic time are 20min
Solid-liquid ratio is that 1:2,1:3,1:4,1:5,1:6,1:7,1:8g/mL are tested, and as a result when solid-liquid ratio is 1:5, anthocyanin is mentioned
Yield is taken to reach maximum value.Finally, investigating ultrasonic time to purple Ma Ling under the conditions of phosphoric acid concentration is 1%, solid-liquid ratio is 1:5
The influence of the extraction effect of anthocyanin in potato, as the result is shown: with the increasing of ultrasonic time (5,7.5,10,15,2., 25,30min)
Add the yield of anthocyanin to present first to rise and then ease up.When ultrasonic time is 20min, the extract yield of anthocyanin in purple potato
Reach preferable level.
The anthocyanin in purple potato is extracted in 2.2Box-Behnken optimization
2.2.1 response phase method optimizes experimental result
On the basis of experiment of single factor result, with phosphoric acid concentration (A), ultrasonic time (B), solid-liquid ratio (C) for independent variable,
Anthocyanin yield (Y) is response, and with the experimental design of Box-Behnken method optimization and the results are shown in Table 2.
2 Box-Behnken test result of table
2.2.2 response-surface model and variance analysis
With Design-Expert software to 1 experimental data of table carry out regression fit, obtain be with anthocyanin yield (Y)
The regression equation of response.
=-0.69815+0.88719A+0.12749B+0.038174C+3.09375 × 10 Y (mg/g)-3AB+3.29375
×10-3AC+1.01125×10-3BC-0.49486A2-0.015094B2-1.22578×10-3C2
The variance analysis of regression model is shown in Table 3.
3 response-surface model variance analysis of table
Note: * indicates significant (p < 0.05) that * * indicates extremely significant (p < 0.01).
As shown in Table 3, regression model p < 0.0001, shows regression model highly significant；The quasi- item P=0.2559 of mistake >
0.05, it is not significant that model loses quasi- item.Model coefficient R 2=0.9948 illustrates that the model can explain 99.48% variation,
The model and test fitting degree are preferable, therefore the model analysis can be used and predict the extraction work of anthocyanin in purple potato
Skill.In conjunction with by the F value size of each factor it can be concluded that, the influence size that anthocyanin in purple potato is extracted in three factors
Are as follows: ultrasonic time > phosphoric acid concentration > solid-liquid ratio.
2.2.3 factor interactive analysis
The factor for extracting anthocyanin in purple potato to ultrasonic phosphate aqueous solution interacts analysis, as a result such as Fig. 5-
Shown in 7.Show that three factors act on the reciprocal effect that anthocyanin in purple potato is extracted.As shown in Figure 5, time curved surface becomes
Change is steeper, illustrates that influence of the ultrasonic time to anthocyanin yield is more significant than the influence of phosphoric acid concentration.In one timing of solid-liquid ratio, surpass
There is maximum in the sound time in 15-20min, phosphoric acid concentration 0.85-1.15%, anthocyanin yield.It will be appreciated from fig. 6 that when control ultrasound
Between it is constant in the case where, phosphoric acid concentration on anthocyanin yield influence it is more significant than solid-liquid ratio, when solid-liquid ratio is in 1:3-1:7g/ml, phosphorus
When the dense 0.85-1.15% of acid, anthocyanin yield has maximum.As shown in Figure 7, control solid-liquid ratio is constant, when phosphoric acid concentration exists
0.85-1.15%, ultrasonic time anthocyanin yield in 15-25min have maximum.
2.2.4 verification test
Obtained the optimum extraction process parameter of anthocyanin in purple potato by response surface optimization: phosphoric acid concentration is
0.98%, solid-liquid ratio 4.96, extraction time 18.92min.Actual experiment adjustment are as follows: extraction time 19min, solid-liquid ratio
5, phosphoric acid concentration 1.0%.Carried out 3 parallel laboratory tests by this condition, obtain anthocyanin yield average value be 0.409 ±
0.010mg/g (RSD=2.51%, n=3), compared with model predication value 0.411mg/g, difference is little, and illustrate the equation has
Effect property.
3 conclusions
The extraction process of anthocyanin in purple potato: choosing phosphoric acid concentration is 0.98%, solid-liquid ratio 4.96, ultrasonic time
18.92min.Verification test result and the identical property of model prediction are good.Anthocyanin is extracted with phosphoric acid substitution citric acid, also there is acid
The low feature of concentration, advantageously reduces production cost.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (9)
1. a kind of method for extracting the anthocyanin containing selenium by purple potato, which is characterized in that based on mass fraction, including walk as follows
It is rapid:
Step 1) cleaning, stripping and slicing；Clean, the stripping and slicing after epidermis natural air drying by new light violet potato cleaning；
Step 2 immerses purple potato ball in extracting solution；The extracting solution is made of phosphatase 11-2%, water 98%-99%；
Step 3) ultrasonic dissolution assisting；Ultrasonic dissolution assisting is carried out using the mixture that Ultrasound Instrument forms step 2;
Step 4) filtering extraction filtrate is spare, repeats step 2-step 3), repeats 2-4 times；
Step 5) purification；Filtrate described in step 4) is separated, anthocyanin containing selenium is extracted.
2. the method for extracting the anthocyanin containing selenium by purple potato as described in claim 1, which is characterized in that the purple potato
The solid-liquid ratio of block and the extracting solution is 1:3-1:8 (g/L).
3. the method for extracting the anthocyanin containing selenium by purple potato as described in claim 1, which is characterized in that the purple potato
The solid-liquid ratio of block and the extracting solution is 1:5 (g/L).
4. the method for extracting the anthocyanin containing selenium by purple potato as described in claim 1, which is characterized in that with mass fraction
Meter, the extracting solution are made of phosphatase 11 .5%, water 98.5%.
5. a kind of device for extracting the anthocyanin containing selenium by purple potato, which is characterized in that including extraction element (1), configuration device
(2)；The extraction element (1) includes extractor (11), is provided with Vltrasonic device (12), the ultrasound on the extractor (11)
Device (12) opening time automatically controls according to setting；Be provided on the extractor (11) feeding-in solid body mouth (111), liquid into
Material mouth (112), discharge port (113), the feeding-in solid body mouth (111) setting on the extractor (11) top, the liquid into
Material mouth (112) setting is arranged in the extractor (11) top, the discharge port (113) in the extractor (11) lower part；Institute
Setting thermometer (114) on extractor (11) is stated, for measuring the extractor (11) internal temperature；The configuration device (2)
Including two storage tanks (21), preparing tank (22)；Two storage tank (21) outlets are connected with the preparing tank (22) respectively；It is described
Preparing tank (22) outlet is connected with the liquid inlet opening (112)；It is provided with liquidometer (211) on the storage tank (21), it is described
Storage tank (21) exit is provided with switch valve；Two storage tanks (21) are respectively provided with phosphoric acid, water；Preparing tank (22) outlet
Place is provided with metering valve (221), and the metering valve (221) is according to default inlet amount unlatching/closing；
Register (3) are set on the extractor (11), the register (3) is using in collet, coil pipe, electric heater unit
At least one, the collet, coil pipe are exchanged heat by internal heating agent with the extractor (11) interior material, the heat exchange packet
Include heating and/or cooling.
6. the device of the anthocyanin containing selenium is extracted by purple potato as claimed in claim 5, which is characterized in that the extraction element
It (1) further include blender, the whip switch switchs mutually chain, the synchronous unlatching/closing of the two with the Vltrasonic device (12).
7. the device of the anthocyanin containing selenium is extracted by purple potato as claimed in claim 5, which is characterized in that further include solid into
Expect device (4), feeding-in solid body device (4) outlet is connected with the feeding-in solid body mouth (111), the feeding-in solid body device
It (4) include solid storage tank (41), solids feeder (42)；Solids feeder (42) import and the solid storage tank (41) go out
Mouth is connected, and solids feeder (42) outlet is connected with the feeding-in solid body mouth (111).
8. the device of the anthocyanin containing selenium is extracted by purple potato as claimed in claim 5, which is characterized in that the solid storage tank
(41) bottom is taper, and solid storage tank (41) outlet is arranged in taper bottommost.
9. the device of the anthocyanin containing selenium is extracted by purple potato as claimed in claim 5, which is characterized in that the feeding-in solid body
Device uses at least one of conveyer belt, screw-feeder.
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