CN109534944A - A kind of method and device preparing lycopene nano-powder - Google Patents
A kind of method and device preparing lycopene nano-powder Download PDFInfo
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- CN109534944A CN109534944A CN201811352781.5A CN201811352781A CN109534944A CN 109534944 A CN109534944 A CN 109534944A CN 201811352781 A CN201811352781 A CN 201811352781A CN 109534944 A CN109534944 A CN 109534944A
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- lycopene
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- carbon dioxide
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- OAIJSZIZWZSQBC-GYZMGTAESA-N lycopene Chemical compound CC(C)=CCC\C(C)=C\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C=C(/C)CCC=C(C)C OAIJSZIZWZSQBC-GYZMGTAESA-N 0.000 title claims abstract description 106
- 235000012661 lycopene Nutrition 0.000 title claims abstract description 103
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 title claims abstract description 99
- JEVVKJMRZMXFBT-XWDZUXABSA-N Lycophyll Natural products OC/C(=C/CC/C(=C\C=C\C(=C/C=C/C(=C\C=C\C=C(/C=C/C=C(\C=C\C=C(/CC/C=C(/CO)\C)\C)/C)\C)/C)\C)/C)/C JEVVKJMRZMXFBT-XWDZUXABSA-N 0.000 title claims abstract description 99
- 239000001751 lycopene Substances 0.000 title claims abstract description 99
- 229960004999 lycopene Drugs 0.000 title claims abstract description 99
- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011858 nanopowder Substances 0.000 title claims abstract description 28
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000002994 raw material Substances 0.000 claims abstract description 79
- 239000013078 crystal Substances 0.000 claims abstract description 70
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 49
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 49
- 238000004090 dissolution Methods 0.000 claims abstract description 49
- 238000002425 crystallisation Methods 0.000 claims abstract description 29
- 230000008025 crystallization Effects 0.000 claims abstract description 29
- 239000012530 fluid Substances 0.000 claims abstract description 21
- 239000000284 extract Substances 0.000 claims abstract description 17
- 235000013399 edible fruits Nutrition 0.000 claims description 13
- 230000008676 import Effects 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 8
- 241000235553 Blakeslea trispora Species 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 150000002664 lycopenes Chemical class 0.000 claims description 4
- 238000000855 fermentation Methods 0.000 claims description 2
- 230000004151 fermentation Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 14
- 239000002904 solvent Substances 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 240000003768 Solanum lycopersicum Species 0.000 description 7
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000000790 scattering method Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- OENHQHLEOONYIE-UKMVMLAPSA-N all-trans beta-carotene Natural products CC=1CCCC(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C OENHQHLEOONYIE-UKMVMLAPSA-N 0.000 description 2
- 235000013734 beta-carotene Nutrition 0.000 description 2
- 239000011648 beta-carotene Substances 0.000 description 2
- TUPZEYHYWIEDIH-WAIFQNFQSA-N beta-carotene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2=CCCCC2(C)C TUPZEYHYWIEDIH-WAIFQNFQSA-N 0.000 description 2
- 229960002747 betacarotene Drugs 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 description 2
- DYLIWHYUXAJDOJ-OWOJBTEDSA-N (e)-4-(6-aminopurin-9-yl)but-2-en-1-ol Chemical compound NC1=NC=NC2=C1N=CN2C\C=C\CO DYLIWHYUXAJDOJ-OWOJBTEDSA-N 0.000 description 1
- 206010004446 Benign prostatic hyperplasia Diseases 0.000 description 1
- 241000235548 Blakeslea Species 0.000 description 1
- 241001451058 Choanephoraceae Species 0.000 description 1
- 108010004103 Chylomicrons Proteins 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 241000235388 Mucorales Species 0.000 description 1
- 241000589516 Pseudomonas Species 0.000 description 1
- 235000002560 Solanum lycopersicum Nutrition 0.000 description 1
- 230000011759 adipose tissue development Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002634 lipophilic molecules Chemical group 0.000 description 1
- 108060004506 lycopene beta-cyclase Proteins 0.000 description 1
- 108060004507 lycopene cyclase Proteins 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000037353 metabolic pathway Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003924 oil dispersant Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Mycology (AREA)
- Botany (AREA)
- Polymers & Plastics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of device and method for preparing lycopene nano-powder.The device is made of dissolution of raw material device and crystal separator.This method comprises: using the lycopene in supercritical carbon dioxide fluid dissolution lycopene raw material；Dissolved with lycopene supercritical carbon dioxide fluid depressurized in crystal separator, cooling down forms subcritical state or gaseous state, crystal of lycopene therein is precipitated；By adjusting solution presasure, temperature and crystallization pressure, temperature difference of the lycopene in carbon dioxide solvent, the partial size of crystal of lycopene is controlled, nano-powder is made.Lycopene in lycopene raw material (content=1-99%, W/W) can be prepared into 10nm-2 μm of partial size of powder by device and method provided by the invention.Solvent used in this method is carbon dioxide, and Product safety is strong, safe operation, environmental-friendly, is applicable in various food-grade lycopene raw materials, such as: including biological source extract and synthetic.
Description
Technical field
The invention belongs to Food Sciences and technical field, are related to a kind of method for preparing lycopene nutrient nano-powder
And device, and in particular to it is a kind of using supercritical carbon dioxide fluid as solvent prepare lycopene nano-powder device and
Method.
Background technique
Lycopene is a kind of nutrient often edible in people's daily life, has a variety of healthy functions (such as: antioxygen
Change, enhancing is immune, treats the healthy functions such as hyperplasia of prostate).Since there are multiple double bonds, lycopenes point in its molecular structure
Son has a variety of geometric isomers.Lycopene in nature with all trans isomer for main existence form, such as Formulas I institute
Show.
In the food of the mankind, tamato fruit is the most abundant source of lycopene.Tomato red is extracted from tamato fruit
The method of element includes: organic solvent (such as ethyl acetate) and supercritical carbon dioxide extraction method.Lycopene in extract
Content at 2-6% (W/W), can reach 75% or more after concentrated.
Supercritical fluid is a kind of state of the substance on critical pressure and critical-temperature.Supercritical carbon dioxide fluid
It is a kind of state of the carbon dioxide on its critical pressure (7.38MPa) and critical-temperature (31.2 DEG C), there is solvent property,
It can dissolve nonpolar small molecular organic compounds.
Summary of the invention
Tomato red is prepared as medium for this purpose, the purpose of the present invention is to provide a kind of application supercritical carbon dioxide fluids
The device of plain nano-powder, the device can prepare 10nm-2 μm of partial size of lycopene nano-powder, and structure is simple, operation side
Just.
It is above-mentioned to cooperate it is another object of the present invention to provide a kind of method for preparing lycopene nano-powder
The use of device.
To achieve the goals above, the present invention provides a kind of device for preparing lycopene nano-powder, by dissolution of raw material
Device and crystal separator composition；
Wherein, which is in cylindrical shape, and draw ratio 1:1-48:1, which is equipped with
Ingress pipe is used for introducing carbon dioxide and raw material；The ingress pipe is vertical with roof plane, which is equipped with the first valve,
For controlling the switch and flow velocity of carbon dioxide and raw material；The dissolution of raw material device is equipped with the first control temperature unit of temperature controllable；
The crystal separator top is in cylindrical shape, and lower part is in inverted cone mesa-shaped, and cylindrical portion draw ratio is 1:2-1:
4, rounding frustum Partial Height and upper bottom surface diameter ratio are 1:0.4-1:1, and upper bottom surface and bottom surface diameter ratio are 1:0.05-1:
0.1.The crystal separator roof center is equipped with carbon dioxide exhaust line, the carbon dioxide exhaust line and the crystal separator roof
Plane is vertical, which is equipped with the second valve, is used for control switch and flow velocity；The crystal separator bottom is set
There is crystallization collecting pipe, the crystallization collecting pipe is vertical with the crystal separator bottom plane；The crystallization collecting pipe is equipped with third valve
Door；The crystal separator is equipped with the second control temperature unit of temperature controllable；
Between the dissolution of raw material device and the crystal separator be equipped with connecting tube, the connecting tube both ends respectively with the dissolution of raw material
Side wall of the device with the crystal separator close to top is connect, and the side wall tangent line with the dissolution of raw material device and the crystal separator
Direction is vertical；The connecting tube is equipped with the 4th valve, is used for control switch and flow velocity；
The volumetric ratio of the dissolution of raw material device and the crystal separator is 1:3-1:20 (V/V).
The present invention also provides a kind of methods for preparing lycopene nano-powder, include the following steps:
1) it charges
The first valve, the second valve, the 4th valve in the above-mentioned device for preparing lycopene nano-powder is open,
Third valve is closed, from carbon dioxide exhaust line access -0.06MPa negative pressure source, so that lycopene raw material is imported from ingress pipe,
Lycopene raw material import volume is the 1/4-1/8 of raw material dissolvers volume in the device for prepare lycopene nano-powder, control
The temperature of dissolution of raw material device is 50-55 DEG C；
2) device empties
Open first valve, the second valve, third valve, close the 4th valve, import 1 atmosphere of pressure > from ingress pipe
The carbon dioxide gas of pressure empties air in system；
3) dissolution of raw material
Open first valve, closes the second valve, third valve, the 4th valve, imports overcritical titanium dioxide from ingress pipe
Carbon flow body makes after pressure reaches 7.2-60MPa, temperature reaches 32-65 DEG C in dissolution of raw material device, closes the first valve, stands 30-
300min makes solubility of the lycopene in the supercritical carbon dioxide fluid in dissolution of raw material device in lycopene raw material
Reach saturation；
4) it crystallizes
The second valve is opened, the 4th valve is slowly opened.The second valve and the 4th valve are adjusted, is made in crystal separator
Pressure is maintained at 0.1-7.2MPa, and temperature is maintained at 4-32 DEG C.Crystallization point is transferred to all lycopenes in dissolution of raw material device
After device, the first valve is closed, stops input supercritical carbon dioxide fluid；
5) crystallization is collected
After device internal pressure will be for 1 atmospheric pressure, temperature control opens third at 70-90 DEG C in crystal separator
Valve collects crystal of lycopene.
Crystal particle diameter range: 10nm-2 μm；
Wherein, the lycopene raw material are as follows: (1) lycopene synthetic, purity is by weight >=96%；(2)
Lycopene tunning extract, purity 6-99% by weight；Or, (3) tamato fruit extract, purity 6- by weight
20%.
Wherein, the lycopene tunning extract is three spore cloth Laplaces mould (Blakeslea trispora) fermentation
Product is obtained through organic solvent or supercritical carbon dioxide extraction.
Wherein, the tamato fruit extract using organic solvent extraction or supercritical carbon dioxide extraction method from
It is obtained by extraction in tamato fruit (Lycopersicon esculentum Mill.).
Wherein, the crystal particle diameter range of the crystal of lycopene is 10nm-2 μm.
Lycopene has good saturation solubility in supercritical carbon dioxide fluid.Meanwhile overcritical titanium dioxide
Phase conversion time between carbon flow body phase and gas phase is very short.It can be by controlling pressure phase transition in the phase transition process of solvent
Difference, temperature difference and transformation time realize the control to solute (such as lycopene) crystallization particle diameter.Compared with organic solvent, using super
The crystallization particle diameter that critical carbon dioxide fluid controls solute as solvent in phase transition process has easy, easy etc. apparent excellent
Point.
Lycopene is lipophilic molecule, enter alimentary canal after first with Adipogenesis true solution, and after through emulsify shape
At the chylomicrons of lycopene fatty solution.Lycopene powder partial size is smaller, forms the efficiency of lycopene fatty solution
It is higher.
The beneficial effects of the present invention are:
1) present invention uses physical method, can prepare 10nm-2 μm of partial size of lycopene nano-powder, not influence product
Food substance basis, improve the bioavilability of lycopene.
2) medium used in the present invention is carbon dioxide, and foodsafety is strong, safe operation, environmental-friendly.
3) method therefor of the present invention is simple and easy, easy to operate.
4) applicable raw materials of the present invention are in extensive range, and various food-grade lycopene raw materials can be used directly as raw material.
Detailed description of the invention
Fig. 1 is the schematic diagram of lycopene nano powder preparing device provided by the present invention.
Fig. 2 is pressure in pressure in raw material dissolvers in embodiment 1 provided by the present invention and crystal separator to tomato red
The influence schematic diagram of plain crystallization particle diameter.
Fig. 3 is the grain size distribution for detecting crystal of lycopene in the embodiment of the present invention 1 using laser refraction scattering method.
Fig. 4 is the grain size distribution for detecting crystal of lycopene in the embodiment of the present invention 2 using laser refraction scattering method.
Appended drawing reference
T-1: dissolution of raw material device；T-2: crystal separator；P-1: ingress pipe；P-2: connecting tube；P-3: carbon dioxide discharge
Pipe；P-4: crystallization collecting pipe；V-1: the first valve；V-2: the second valve；V-3: third valve；V-4: the four valve.
Specific embodiment
As shown in Figure 1, be the device provided by the present invention for preparing lycopene nano-powder, by dissolution of raw material device T-1 and
Crystal separator T-2 composition；Wherein, which is in cylindrical shape, draw ratio 1:1-48:1, the dissolution of raw material
Device T-1 roof center is equipped with ingress pipe P-1, is used for introducing carbon dioxide and raw material；Ingress pipe P-1 is vertical with roof plane,
Ingress pipe P-1 is equipped with the first valve V-1, for controlling the switch and flow velocity of carbon dioxide and raw material；The dissolution of raw material device
T-1 is equipped with the first control temperature unit (not shown) of temperature controllable；
The top crystal separator T-2 is in cylindrical shape, and lower part is in inverted cone mesa-shaped, and cylindrical portion draw ratio is 1:2-
1:4, rounding frustum Partial Height and upper bottom surface diameter ratio are 1:0.4-1:1；Crystal separator T-2 roof center is equipped with dioxy
Change carbon discharge pipe P-3, carbon dioxide exhaust line P-3 is vertical with crystal separator T-2 roof plane, carbon dioxide discharge
Pipe P-3 is equipped with the second valve V-2, is used for control switch and flow velocity；The bottom crystal separator T-2 is equipped with crystallization collecting pipe,
The crystallization collecting pipe is vertical with crystal separator T-2 bottom plane；The crystallization collecting pipe is equipped with third valve V-3；The knot
Brilliant separator T-2 is equipped with the second control temperature unit (not shown) of temperature controllable；
Between the dissolution of raw material device T-1 and crystal separator T-2 be equipped with connecting tube, the connecting tube both ends respectively with the original
Expect that side wall of the dissolvers T-1 with crystal separator T-2 close to top is connect, and with the dissolution of raw material device T-1 and the crystallization
The side wall tangential direction of separator T-2 is vertical；The connecting tube is equipped with the 4th valve V-4, is used for control switch and flow velocity；
The volumetric ratio of the dissolution of raw material device T-1 and crystal separator T-2 is 1:3-1:20 (V/V).
Embodiment 1
Lycopene raw material are as follows: tamato fruit extract, lycopene content 6% (W/W).
Tamato fruit extract is prepared using supercritical carbon dioxide extraction method, detailed process are as follows: by fresh tomato
Fruit 1000kg squeezes separating pericarp and seed, collects pulp grinding homogenate.180 DEG C (inlet temperatures) to being spray dried to do
Powder.Supercritical carbon dioxide extraction tomato dry powder is used at 55 DEG C, 45MPa, obtains tamato fruit supercritical carbon dioxide
Fluid extract.
The device for preparing lycopene nano-powder uses device as shown in Figure 1, wherein the major diameter of dissolution of raw material device T-1
Than for 6:1, volume 200mL.Cylindrical portion draw ratio is 1:2, frustum-conical portion height and upper bottom in crystal separator T-2
Face diameter ratio is 1:0.4, and upper bottom surface and bottom surface diameter ratio are 1:0.1, volume 600mL.
The specific operation method is as follows:
1) it charges
Third valve V-3 is closed, the first valve V-1, the second valve V-2 and the 4th valve V-4 are open, from carbon dioxide
Discharge pipe P-3 access -0.06MPa negative pressure source makes tamato fruit extract raw material and imports from ingress pipe P-1, and importing volume is original
Expect the 1/8 of dissolvers T-1 volume, the temperature of control dissolution of raw material device T-1 is 55 DEG C.
2) device empties
Open first valve V-1, the second valve V-2 and third valve V-3, close the 4th valve V-4, from ingress pipe P-1
Introducing carbon dioxide gas (pressure=2MPa) empties air in system.
3) dissolution of raw material
Open first valve V-1, closes the second valve V-2, third valve V-3 and the 4th valve V-4, from ingress pipe P-1
Supercritical carbon dioxide fluid is imported, is made after pressure reaches 45MPa, temperature reaches 55 DEG C in dissolution of raw material device T-1, closes first
Valve V-1 stands 30min, makes supercritical carbon dioxide of the lycopene in dissolution of raw material device T-1 in lycopene raw material
Solubility in fluid reaches saturation.
4) it crystallizes
After opening the second valve V-2, the 4th valve V-4 is slowly opened, the second valve V-2 and the 4th valve V-4 is adjusted, makes
Pressure in crystal separator T-2 is maintained at 0.6MPa, and temperature is maintained at 4 DEG C.To all lycopenes in dissolution of raw material device T-1
After being transferred to crystal separator T-2, the first valve V-1 is closed, stops input supercritical carbon dioxide fluid.
5) crystallization is collected
After device internal pressure is reduced to 1 atmospheric pressure, temperature control opens third valve at 70 DEG C in crystal separator T-2
Door V-3, collects crystal of lycopene.
Crystal separator lower part is in inverted cone mesa-shaped, is conducive to the collection of lycopene crystal after crystallization sedimentation.
As shown in Fig. 2, for qualifications (temperature in the present embodimentT-1=55 DEG C, temperatureT-2=4 DEG C) under lycopene receive
In rice flour body preparation facilities in raw material dissolvers T-1 container in pressure and crystal separator T-2 container pressure to lycopene knot
The influence schematic diagram of crystal size.Wherein, pressure in different pictorial representation dissolution of raw material device T-1 containers, low pressure vessel pressure refer to knot
Pressure in brilliant separator T-2 container.
When in crystal separator pressure carbon dioxide and temperature be lower than its critical pressure (7.2MPa) and critical-temperature (32
DEG C) when, carbon dioxide is in gaseous state, and the lycopene being dissolved in supercritical carbon dioxide fluid is precipitated, crystallization is formed,
It is separated from carbon dioxide medium.From figure 2 it can be seen that the present invention is by adjusting dissolution of raw material device and crystal separator
Interior pressure difference and temperature difference obtain the lycopene powder of different-grain diameter.Pressure between dissolution of raw material device and crystal separator
Difference and temperature difference are bigger, and the partial size of lycopene powder is smaller.Pressure difference and temperature between dissolution of raw material device and crystal separator
Difference is smaller, and the partial size of lycopene powder is bigger.
The crystallization particle diameter of method measurement lycopene is penetrated using laser refraction.Through detecting crystal of lycopene grain as shown in Figure 3
The powder that diameter reaches 100nm accounts for 5.04%.Compared with the crystallization (2 μm of partial size >) that lycopene is formed in organic solvent, grain
The lycopene powder that diameter is 100nm has better bioavilability.
Embodiment 2
Lycopene raw material are as follows: Blakeslea trispora extract oil dispersant, lycopene content 20% (W/W).
It is mould (Blakeslea trispora) that three spore cloth Laplaces are extracted using supercritical carbon dioxide extraction method.
Trispore Bruce mould is under the jurisdiction of Mucoales (Muco-rales) Ji Mei section (Choanephoraceae), and Bradley is mould
Pseudomonas (Blakeslea).Trispore Bruce mould is a kind of Producing Strain for producing beta carotene, which has unique be metabolized
Journey lycopene is that an intermediate product in its metabolic pathway inhibits beta carotene biosynthesis by addition blocking agent
The activity of lycopene cyclase in approach, to accumulate lycopene.
Extract the three mould detailed processes of spore cloth Laplace are as follows: Blakeslea trispora powder 5kg, with overcritical two at 55 DEG C, 45MPa
Carbon oxide fluid extracts Blakeslea trispora powder, obtains Blakeslea trispora supercritical carbon dioxide extraction object.Extract point
It dissipates in the soya-bean oil of 10 times of volumes.
The device for preparing lycopene nano-powder uses device as shown in Figure 1, wherein the major diameter of dissolution of raw material device T-1
Than for 6:1, volume 200mL.Cylindrical portion draw ratio is 1:2, (the upper bottom frustum-conical portion Gao Jing in crystal separator T-2
Area diameter) than being 1:0.4, upper bottom surface and bottom surface diameter ratio are 1:0.1, volume 600mL.
Specific steps are as follows:
1) it charges
Third valve V-3 is closed, the first valve V-1, the second valve V-2 and the 4th valve V-4 are open.From carbon dioxide
Discharge pipe P-3 access -0.06MPa negative pressure source enables tamato fruit to extract raw material and imports from ingress pipe P-1.Import raw material
Volume be dissolution of raw material device T-1 volume 1/8.The temperature of dissolution of raw material device T-1 is 55 DEG C.
2) device empties
Open first valve V-1, the second valve V-2 and third valve V-3, close the 4th valve V-4.From ingress pipe P-1
Introducing carbon dioxide gas (pressure=2MPa) empties air in system,
3) dissolution of raw material
Open first valve V-1, closes the second valve V-2, third valve V-3 and the 4th valve V-4, from ingress pipe P-1
Supercritical carbon dioxide fluid is imported, after pressure reaches 60MPa, temperature reaches 55 DEG C in dissolution of raw material device T-1, closes the first valve
Door V-1.30min is stood, stream of supercritical carbon dioxide of the lycopene in dissolution of raw material device T-1 in lycopene raw material is made
Solubility in body reaches saturation.
4) it crystallizes
After opening the second valve V-2, the 4th valve V-4 is slowly opened, the second valve V-2 and the 4th valve V-4 is adjusted, makes
Pressure in crystal separator T-2 is maintained at 0.1MPa, and temperature is maintained at -10 DEG C.To all tomato reds in dissolution of raw material device T-1
After element is transferred to crystal separator T-2, the first valve V-1 is closed, stops input supercritical carbon dioxide fluid.
5) crystallization is collected
After device internal pressure is reduced to 1 atmospheric pressure, temperature control opens third valve at 70 DEG C in crystal separator T-2
Door V-3, collects crystal of lycopene.
Use the crystallization particle diameter of laser refraction scattering method lycopene.Through detecting crystal of lycopene as shown in Figure 4
The powder that partial size reaches 80nm accounts for 8.04%, compared with the crystallization (2 μm of partial size >) that lycopene is formed in organic solvent, grain
The lycopene powder that diameter is 80nm has better bioavilability.Meanwhile embodiment 2 the results showed that passing through control
The temperature and pressure of dissolution of raw material device processed and the temperature and pressure of Crystallization Separation container, the lycopene that can prepare different-grain diameter are received
Rice flour body.
From above-described embodiment as can be seen that the device and method provided by the invention for preparing lycopene nano-powder can be made
Standby lycopene nano-powder of the crystallization particle diameter at 10nm-2 μm out passes through the crystal grain in existing organic solvent with lycopene
Diameter (200-600 μm) is compared, and (10nm-2 μm) of lycopene particle diameter of nanometer powder has better bioavilability.
Above-described embodiment is only intended to clearly illustrate examples of the invention, and does not limit the embodiments.It is right
In the professional of fields, other different forms of changes or modifications may be made based on the above description.This
In there is no need to be exhaustive to all embodiments.And extended from this, obvious changes or variations are still
Among protection scope of the present invention.
Claims (6)
1. a kind of device for preparing lycopene nano-powder, it is characterised in that: be made of dissolution of raw material device and crystal separator；
Wherein, which is in cylindrical shape, and draw ratio 1:1-48:1, which, which is equipped with, imports
Pipe is used for introducing carbon dioxide and raw material；The ingress pipe is vertical with roof plane, which is equipped with the first valve, is used for
Control the switch and flow velocity of carbon dioxide and raw material；The dissolution of raw material device is equipped with the first control temperature unit of temperature controllable；
The crystal separator top is in cylindrical shape, and lower part is in inverted cone mesa-shaped, and cylindrical portion draw ratio is 1:2-1:4,
Frustum-conical portion height and upper bottom surface diameter ratio are 1:0.4-1:1, and upper bottom surface and bottom surface diameter ratio are 1:0.05-1:0.1, should
Crystal separator roof center is equipped with carbon dioxide exhaust line, and the carbon dioxide exhaust line and the crystal separator roof plane are hung down
Directly, which is equipped with the second valve, is used for control switch and flow velocity；The crystal separator bottom is equipped with crystallization
Collecting pipe, the crystallization collecting pipe are vertical with the crystal separator bottom plane；The crystallization collecting pipe is equipped with third valve；The knot
Brilliant separator is equipped with the second control temperature unit of temperature controllable；
Between the dissolution of raw material device and the crystal separator be equipped with connecting tube, the connecting tube both ends respectively with the dissolution of raw material device with
Side wall of the crystal separator close to top connects, and the side wall tangential direction with the dissolution of raw material device and the crystal separator
Vertically；The connecting tube is equipped with the 4th valve, is used for control switch and flow velocity；
The volumetric ratio of the dissolution of raw material device and the crystal separator is 1:3-1:20.
2. a kind of method for preparing lycopene nano-powder, which comprises the steps of:
1) it charges
By the first valve, the second valve, the 4th valve in the device for preparing lycopene nano-powder as described in claim 1
Door is open, and third valve is closed, from carbon dioxide exhaust line access -0.06MPa negative pressure source, so that lycopene raw material is from importing
Pipe imports, and lycopene raw material import volume is the 1/4-1/ of raw material dissolvers volume in the device for prepare lycopene nano-powder
8, the temperature of control dissolution of raw material device is 50-55 DEG C；
2) device empties
Open first valve, the second valve, third valve, close the 4th valve, import 1 atmospheric pressure of pressure > from ingress pipe
Carbon dioxide gas empties air in system；
3) dissolution of raw material
Open first valve, closes the second valve, third valve, the 4th valve, imports stream of supercritical carbon dioxide from ingress pipe
Body makes after pressure reaches 7.2-60MPa, temperature reaches 32-65 DEG C in dissolution of raw material device, closes the first valve, stands 30-
300min makes solubility of the lycopene in the supercritical carbon dioxide fluid in dissolution of raw material device in lycopene raw material
Reach saturation；
4) it crystallizes
After opening the second valve, the 4th valve is slowly opened, the second valve and the 4th valve is adjusted, makes the pressure in crystal separator
Power is maintained at 0.1-7.2MPa, and temperature is maintained at 4-32 DEG C.Crystallization Separation is transferred to all lycopenes in dissolution of raw material device
After device, the first valve is closed, stops input supercritical carbon dioxide fluid；
5) crystallization is collected
After device internal pressure is reduced to 1 atmospheric pressure, temperature control opens third valve at 70-90 DEG C in crystal separator,
Collect crystal of lycopene.
3. the method for preparing lycopene nano-powder as claimed in claim 2, which is characterized in that the lycopene raw material
Are as follows: (1) lycopene synthetic, purity is by weight >=96%；(2) lycopene tunning extract, purity are pressed
Poidometer 6-99%；Or, (3) tamato fruit extract, purity 6-20% by weight.
4. the method for preparing lycopene nano-powder as claimed in claim 3, which is characterized in that the lycopene fermentation produces
Object extract is mould (Blakeslea trispora) tunning of three spore cloth Laplaces through organic solvent or supercritical carbon dioxide
Fluid extraction obtains.
5. the method for preparing lycopene nano-powder as claimed in claim 3, which is characterized in that the tamato fruit extraction
Object is obtained by extraction using organic solvent extraction or supercritical carbon dioxide extraction method.
6. the method for preparing lycopene nano-powder as claimed in claim 2, which is characterized in that the crystal of lycopene
Crystal particle diameter range is 10nm-2 μm.
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| CN115176601A (en) * | 2021-03-28 | 2022-10-14 | 北京联合大学 | Flesh seed separator |
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