CN107056574A - A kind of method for extracting lycopene - Google Patents
A kind of method for extracting lycopene Download PDFInfo
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- CN107056574A CN107056574A CN201710062650.2A CN201710062650A CN107056574A CN 107056574 A CN107056574 A CN 107056574A CN 201710062650 A CN201710062650 A CN 201710062650A CN 107056574 A CN107056574 A CN 107056574A
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- lycopene
- alcohol
- slurries
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- 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 75
- 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 75
- 235000012661 lycopene Nutrition 0.000 title claims abstract description 75
- 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 75
- 239000001751 lycopene Substances 0.000 title claims abstract description 75
- 229960004999 lycopene Drugs 0.000 title claims abstract description 75
- 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 75
- 238000000034 method Methods 0.000 title claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 104
- 238000000605 extraction Methods 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 35
- 235000013399 edible fruits Nutrition 0.000 claims description 33
- 239000002002 slurry Substances 0.000 claims description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 235000007688 Lycopersicon esculentum Nutrition 0.000 claims description 21
- 239000012043 crude product Substances 0.000 claims description 19
- 239000013049 sediment Substances 0.000 claims description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000010009 beating Methods 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 239000001273 butane Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 239000003345 natural gas Substances 0.000 claims description 2
- 241000227653 Lycopersicon Species 0.000 claims 2
- 235000003953 Solanum lycopersicum var cerasiforme Nutrition 0.000 abstract description 28
- 240000003040 Solanum lycopersicum var. cerasiforme Species 0.000 abstract description 28
- 238000013459 approach Methods 0.000 abstract description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
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- 239000007864 aqueous solution Substances 0.000 description 4
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
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- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
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- 238000007068 beta-elimination reaction Methods 0.000 description 1
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- 210000004369 blood Anatomy 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
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- 150000001793 charged compounds Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
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- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
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- 235000019629 palatability Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 235000020681 well water Nutrition 0.000 description 1
- 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 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Extraction Or Liquid Replacement (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention provides a kind of method for extracting lycopene, ultrasonic alcohol extracting and the combination of subcritical abstraction technique are employed first, the purity of the lycopene product of acquisition is higher, can be applied to food, cosmetics or health products trade as raw material；Extraction conditions are gentle, easy to operate, treating capacity is big, realize industrialization prepared by the extraction of lycopene, particularly realize that from cherry tomato extraction prepares the industrialization of lycopene, new approach is opened for the upgrading synergy of cherry tomato, the source of lycopene is added, with positive economic value.
Description
Technical field
The invention belongs to food processing field, it is related to a kind of method for extracting lycopene, more particularly to it is a kind of from tomato
The method that lycopene is extracted in the fruit of kind.
Background technology
Lycopene（Lycopene）It is a kind of natural carotenoid, molecular formula is C40H56, relative molecular weight is
536.85, due to containing 11 conjugated double bonds and 2 unconjugated double bonds, so with extremely strong oxidation resistance（Its is anti-oxidant
Ability is 2 times of beta carotene, 100 times of vitamin E）, with a variety of important physiologically actives, such as quenching singlet oxygen and
Free radical is removed, with reduction blood fat, slows down the functions such as atherosclerosis, anticancer and activating immune cell effect, therefore tool
There is high Development volue.
In recent years, lycopene colours the food additives of double action as natural food colour, nutrient and nutrition
And it is widely used in health food, medicine and cosmetics industry have become the subjects such as domestic and international nutrition, medical science, bromatology
Study hotspot.
Lycopene is distributed widely in various plants in nature, such as tomato, carrot, watermelon, citrus, red grape
Shaddock etc. contains lycopene, wherein lycopene content highest in tomato and cherry tomato, and fresh Lycopene in Tomatoes is about
For 30-200mg/kg, it is distributed mainly in the water-insoluble part and skin of tomato, accounts for the 72-92% of Lycopene in Tomatoes,
The content highest of lycopene wherein in tomato skin.
At present, lycopene is mainly extracted from tomato, less to be extracted from cherry tomato.Cherry tomato, also referred to as cherry and tomato,
It is the fruit of the annual herb plant in Solanaceae tomato genus, it is its lovely luster, sour and sweet palatability, nutritious, it is a kind of fruit
Type vegetables.Because domestic consumption is in great demand, China's cherry tomato yield increases sharply, and drives whole cherry tomato industry development.It is holy
In female's fruit harvest process, a large amount of cherry tomato inferior fruits can be produced, because process technology falls behind, these inferior fruit utilization rates are low, remove
Part is used outside as feed, is largely discarded in farmland, is caused the wasting of resources.
Lycopene extraction purification patented technology has had many kinds, mainly there is solvent extraction method, use such as dichloro more
Methane, chloroform, ethyl acetate, acetone equal solvent are extracted, and the solvent toxicity that the above method is used is larger, or exists inflammable and explosive etc.
Potential safety hazard, has larger harm to operator and environment；Also, to avoid polluting environment, solvent needs recycling, a side
Face increases production cost, on the other hand, and the heating concentration during recovery of solvent can cause the degraded of lycopene, influence product
Quality；More seriously, there is dissolvent residual in the residue material after solvent extraction, limit the application of the resource.Therefore,
Need a kind of method of new extraction lycopene badly.
The content of the invention
It is an object of the invention to provide a kind of method for extracting lycopene, wherein, this method comprises the following steps：Step
Rapid 1）The fruit of tomato kind is provided, and the first slurries will be obtained after the fruit crushing and beating；Step 2）Starch described first
Liquid carries out ultrasonic alcohol extracting and obtains the second slurries；Step 3）Second slurries are centrifuged, sediment is collected；It is described heavy to dry
Starch simultaneously crushes acquisition crushed material；Step 4）To step 3）It is thick that the crushed material of acquisition carries out subcritical abstraction acquisition lycopene
Product；Step 5）Purify the lycopene crude product and obtain lycopene product.
It is preferred that, in the step 2）In, alcohol extraction solvent is added in first slurries, transfers in retort
Row ultrasound alcohol extracting processing, wherein, the treatment temperature of ultrasonic alcohol extracting is 20 ~ 50 DEG C, and processing time is 0.5 ~ 3h；Supersonic frequency is 10
~ 60kHZ, ultrasound intensity is 20 ~ 200W/kg.
It is preferred that, the alcohol extraction solvent is the mixed solution of lower alcohol, low-alcohol solution or lower alcohol and ammoniacal liquor, described low
Level alcohol is methanol and/or ethanol, wherein, and the ratio of first slurries and the alcohol extraction solvent is 1kg: 1L ~ 1kg
: 3L。
It is preferred that, in the mixed solution of the lower alcohol and ammoniacal liquor, the volume of the total volume 30% ~ 70% of lower alcohol, ammonia
The volume of the total volume 10% ~ 20% of water.
It is preferred that, in the step 3）In, centrifugation uses flat board centrifugation, and centrifugal rotational speed is 2000 ~ 5000rpm, and
The sediment is collected using the filter cloth of 100 ~ 400 mesh.
It is preferred that, the step 4）In, sieve takes granularity to be less than or equal to crushed material described in 200 purposes and carries out subcritical extraction
Take, wherein, the extractant that the subcritical abstraction is used include propane, butane or liquefied natural gas, the crushed material with
The ratio range of the extractant is 1kg: 4L~ 1kg : 16L.
It is preferred that, the entrainer of 10% ~ 25% percent by volume is also contained in the extractant, the entrainer is second
Alcohol.
It is preferred that, the step 4）In, the temperature of the subcritical abstraction is 20 ~ 50 DEG C, and extraction times are 2 ~ 6 times, often
Secondary extraction time is 15 ~ 150min.
It is preferred that, the step 5）In, purification solvent is added in the lycopene crude product, -60 ~ 5 are adjusted the temperature to
DEG C, stand after 0.5 ~ 5h, crystallisation by cooling, suction filtration obtains the lycopene product；The purification solvent is for petroleum ether or just
The ratio of alkane or their mixed liquors, the lycopene crude product and purification solvent is 1kg: 1L ~ 1kg : 4L.
It is preferred that, the fruit of the tomato kind is cherry tomato.
Compared with prior art, the method for extraction lycopene of the invention employs ultrasonic alcohol extracting and subcritical extraction first
The combination of taking technique, has the advantages that：
1）The purity of the lycopene product of acquisition is higher, can be applied to food, cosmetics or health products trade as raw material；
2）Extraction conditions are gentle, and the chemical reagent corrosive very little used, security is good, and is easily recycled processing, reduces
Equipment anticorrosion and pollution treatment processing cost；
3）Easy to operate, treating capacity is big, realizes industrialization prepared by the extraction of lycopene, particularly realizes from cherry tomato
Extraction prepares the industrialization of lycopene, is that the upgrading synergy of cherry tomato opens new approach, adds lycopene
Source, with positive economic value.
Embodiment
To embodiments of the invention be provided with detailed description below.Although the present invention will combine some embodiments
It is illustrated and illustrates, but should be noted that the present invention is not merely confined to these embodiments.On the contrary, to the present invention
The modification of progress or equivalent substitution, all should cover among scope of the presently claimed invention.
In addition, in order to better illustrate the present invention, numerous details are given in embodiment below.
It will be understood by those skilled in the art that without these details, the present invention can equally be implemented.
The invention provides a kind of method for extracting lycopene, wherein, this method comprises the following steps：Step 1）There is provided
The fruit of tomato kind, and the first slurries will be obtained after the fruit crushing and beating；Step 2）First slurries are surpassed
Sound alcohol extracting obtains the second slurries；Step 3）Second slurries are centrifuged, sediment is collected；Dry the sediment and powder
Broken acquisition crushed material；Step 4）To step 3）The crushed material of acquisition carries out subcritical abstraction and obtains lycopene crude product；Step 5）
Purify the lycopene crude product and obtain lycopene product.
In one embodiment of the invention, the fruit of tomato kind can use tomato or cherry tomato.It is excellent
Choosing, using cherry tomato.
Due in cherry tomato harvest process, a large amount of cherry tomato inferior fruits can be produced, because process technology falls behind, these times
Fruit utilization rate is low, in addition to being used except part as feed, largely discards in farmland, causes the wasting of resources.Therefore, in the present invention
One more preferably in embodiment, the fruit of tomato kind can use cherry tomato inferior fruit." cherry tomato inferior fruit " refers to field
Between the cherry tomato either removed by classifying screen discarded, reject remaining after mouldy and green fruit.
In one embodiment of the invention, step 1）The fruit of the tomato kind of offer is cleaned by removal of impurities
Fruit." removal of impurities " refers to remove prematurity, mouldy fruit, leaf, branch etc.." cleaning " is mainly the mud on cleaning fruit
Husky and dust；Water for cleaning can be running water, well water or deionized water.
In one embodiment of the invention, step（1）Described in " crushing and beating " can be using conventional
Fruits and vegetables crushing and beating machine is handled, and obtains substantially uniform fruit slurries（First slurries）.
In one embodiment of the invention, in the step 2）In, alcohol extracting is added in, the first slurries molten
Agent, transfers in retort and carries out ultrasonic alcohol extracting processing, wherein, the treatment temperature of ultrasonic alcohol extracting is 20 ~ 50 DEG C, processing time
For 0.5 ~ 3h；Supersonic frequency is 10 ~ 60kHZ, and ultrasound intensity is 20 ~ 200W/kg.It is preferred that, the treatment temperature of ultrasonic alcohol extracting can
Think 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C or 50 DEG C；The processing time of ultrasonic alcohol extracting can for 0.5h, 1h, 1.5h,
2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h；Supersonic frequency can be 20kHZ, 40kHZ, 59kHZ or their alternate group
Close；Ultrasound intensity can be 20W/kg, 50W/kg, 80W/kg, 100W/kg, 120W/kg, 150W/kg, 180W/kg or 200W/
kg。
In a preferred embodiment of the invention, the process of the ultrasonic alcohol extracting uses double-frequency ultrasound.Inventor passes through
Excessive quantifier elimination experiment finds that double-frequency ultrasound can more effectively destroy the cell of holy girl's fruits, be follow-up tomato red
Advantage is established in the extraction of element.
In a preferred embodiment of the invention, the alcohol extraction solvent is lower alcohol, low-alcohol solution or lower alcohol
With the mixed solution of ammoniacal liquor, the lower alcohol is methanol and/or ethanol, wherein, and first slurries and the alcohol extracting are molten
The ratio of agent is 1kg: 1L ~ 1kg : 3L.
In the further preferred embodiment of the present invention, the ratio of the first slurries and the alcohol extraction solvent（That is feed liquid
Ratio）For 1kg: 1L、1kg : 1.5L、1kg : 2L、1kg :2.5L or 1kg: 3L.
In another further preferred embodiment of the present invention, the alcohol extraction solvent can be absolute methanol, methanol
The aqueous solution, absolute ethyl alcohol, the aqueous solution of ethanol, absolute methanol and absolute ethyl alcohol mixed liquor（The mixed liquor of arbitrary proportion）Or first
The mixed aqueous solution of alcohol and ethanol（The mixed aqueous solution of arbitrary proportion）, wherein the percent by volume of lower alcohol can for 50%,
60%th, 70%, 80%, 90% or 100%.
It is rudimentary in the mixed solution of the lower alcohol and ammoniacal liquor in another further preferred embodiment of the present invention
The volume of the total volume 30% ~ 70% of alcohol, the volume of the total volume 10% ~ 20% of ammoniacal liquor.Inventor is by substantial amounts of research examination
Issue after examination and approval now, during ultrasonic alcohol extracting, addition ammoniacal liquor can effectively accelerate β-elimination reaction of pectin in alcohol extraction solvent, improve
Cyto-architectural destructiveness, is that advantage is established in the extraction of lycopene.
In one embodiment of the invention, in the step 3）In, centrifugal rotational speed is 2000 ~ 5000rpm, and
The sediment is collected using the filter cloth of 100 ~ 400 mesh.It is preferred that, step 3）In can be centrifuged using plate centrifuge.
It is preferred that, centrifugal rotational speed can for 2000rpm, 2500 rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm or
5000rpm.It is preferred that, the mesh number of filter cloth can be 100 mesh, 150 mesh, 200 mesh, 250 mesh, 300 mesh, 350 mesh or 400 mesh.
In one embodiment of the invention, in the step 3）In, the drying temperature of the sediment for 40 ~
65 DEG C, drying time is 3 ~ 10h.It is preferred that, the drying temperature of sediment can for 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or
65℃.It is preferred that, drying time can be 3h, 4h, 5h, 6h, 7h, 8h, 9h or 10h.
In one embodiment of the invention, the drying mode of the sediment can be forced air drying, vacuum
Dry or microwave drying.
In one embodiment of the invention, the step 4）In, sieve takes granularity less than or equal to the institute of 200 mesh
State crushed material and carry out subcritical abstraction, the extractant that the subcritical abstraction is used is natural comprising propane, butane or liquefaction
The ratio range of gas, the crushed material and the extractant is 1kg: 4L~ 1kg : 16L.
In a preferred embodiment of the invention, 10% ~ 25% percent by volume is also contained in the extractant
Entrainer, the entrainer is ethanol.Inventor tests by numerous studies and found, in subcritical abstraction, in extractant
Middle addition ethanol is as entrainer, while the polarity of extractant is improved, and also promotes to infiltrate inside material, and this is all conducive to kind
Lycopene is migrated into solvent from material.
It is preferred that, crushed material is crossed to the sieve of 200 mesh, 180 mesh, 150 mesh, 120 mesh, 100 mesh, 80 mesh, 60 mesh or 40 mesh.
" subcritical abstraction " technology makes extractant reach subcritical state, foundation by control pressure and temperature
The similar principle mixed of organic matter（By extracting material and molecule diffusion process of the extractant in immersion process, reach solid
Liposoluble constituent in body material is transferred in the extractant of liquid）After target substance is extracted in material, with latter
Rise and enter in material collection tank, then realize that extractant is separated with purpose product by the process being evaporated under reduced pressure and solvent gasifies.
Inventor is tested by numerous studies and found, subcritical abstraction technology is applied into the preparation of lycopene and adding for prior art
The process of hot concentration and recovery solvent is compared, and on the one hand due to extraction link and solvent link mild condition, greatly reduces tomato red
The loss of element, the extraction efficiency of lycopene is higher, on the other hand, and the dissolvent residual in material residue after extraction is few, ring
Border pressure is small, also provides possibility for the follow-up further utilization of resources.
In one embodiment of the invention, the step 4）In, the temperature of the subcritical abstraction is 20 ~ 50
DEG C, extraction times are 2 ~ 6 times, and each extraction time is 15 ~ 150min.It is preferred that, the temperature of subcritical abstraction is 20 DEG C, 25
DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C or 50 DEG C；It is preferred that, extraction times are 2 times, 3 times, 4 times, 5 times or 6 times；It is preferred that, often
Secondary extraction time is 15min, 30min, 45min, 60min, 90min, 120min or 150min.
In one embodiment of the invention, the step 5）In, added in the lycopene crude product pure
Change solvent, adjust the temperature to -60 ~ 5 DEG C, stand after 0.5 ~ 5h, crystallisation by cooling, suction filtration obtains the lycopene product；It is described
Purification solvent is petroleum ether or normal hexane or their mixed liquors（Mixed liquor refers to the mixing of the arbitrary proportion of petroleum ether and normal hexane
Liquid）, the ratio of the lycopene crude product and purification solvent（That is feed liquid ratio）For 1kg: 1L ~ 1kg : 4L.It is preferred that,
Chilling temperature can be -60 DEG C, -50 DEG C, -40 DEG C, -30 DEG C, -20 DEG C, -10 DEG C, -5 DEG C, 0 DEG C or 5 DEG C.It is preferred that, described kind
Lycopene crude product and the ratio of purification solvent can be 1kg: 1L、1kg : 1.5L、1kg : 2L、1kg : 2.5L、1kg :
3L、1kg :3.5L or 1kg: 4L.
In one embodiment of the invention, in the step 5）In, the lycopene crude product is loaded close
Seal in container, add the purification solvent, after being filled with nitrogen in the sealing container, sealing and standing.
In a preferred embodiment of the invention, method of the invention from cherry tomato suitable for extracting tomato red
Element.
The method of the extraction lycopene of the present invention employs ultrasonic alcohol extracting and the combination of subcritical abstraction technique first, anticipates
Outer to find, the purity for the lycopene product that the extraction process that both combine is obtained is higher, and extraction conditions are gentle, security
Good, solvent is easily recycled processing；What is more important, the method for extracting lycopene of the invention, easy to operate, treating capacity
Greatly, industrialization prepared by the extraction of lycopene is realized, particularly realizes that from cherry tomato extraction prepares the work of lycopene
Industry, is that the upgrading synergy of cherry tomato opens new approach, the source of lycopene is added, with positive economy
Value.
Embodiment 1
A kind of embodiment 1 prepares lycopene method in providing inferior fruit from cherry tomato, it comprises the following steps：
Step 1）：The discarded cherry tomato 10kg in field is collected, mouldy and immature fruit is rejected, removing mud is cleaned with running water
Sand, obtains the first slurries after draining, after crushing and beating；
Step 2）：In step 1）15L absolute ethyl alcohols are added in the first slurries obtained, then global transfer enters ultrasonic wave extraction apparatus
In, use 20kHZ frequencies with 1000W ultrasound intensities at 40 DEG C, 300rpm circulation stirrings 90min obtains the second slurries, 4 DEG C
Lucifuge is standby；
Step 3）：By step 2）The second slurries obtained are added in the plate centrifuge of 300 mesh filter clothes of configuration, are used
3000rpm is centrifuged, and collects the sediment on filter cloth；Sediment is added in vacuum drying chamber again, using 50 DEG C of dry 6h, then
Crush and obtain crushed material；
Step 4）：By step 3）Crushed material cross 100 mesh sieves, obtain the crushed material that granularity is less than or equal to 100 mesh；Will
0.435kg crushed materials are fitted into 200 mesh Nylon Bags, are reloaded into subcritical abstraction tank, using 8L subcritical abstraction agent（Wherein third
Alkane 7.2L, entrainer ethanol 0.8L）, extracted 5 times at 40 DEG C, each extraction time is 30min, and extract is transferred into material pot
In, propane is reclaimed, lycopene crude product is obtained；
Step 5）：By step 4）The lycopene crude product of acquisition, is fitted into sealing Brown Glass Brown glass bottles and jars only, adds 1L normal hexanes, be filled with
Nitrogen, sealing is placed in 3h in -5 DEG C, and suction filtration reclaims normal hexane, obtains the g of crystal 4.53.
The crystal of acquisition passes through Mass Spectrometric Identification, and its molecular ion peak is 536.3（With lycopene relative molecular weight
536.89g/mol it is basically identical）, can determine that it is lycopene；Product purity is 95%.
Embodiment 2
A kind of embodiment 2 prepares lycopene method in providing inferior fruit from cherry tomato, it comprises the following steps：
Step 1）：The discarded cherry tomato 50kg in field is collected, mouldy and immature fruit is rejected, removing mud is cleaned with deionized water
Sand, obtains the first slurries after draining, after crushing and beating；
Step 2）：In step 1）The mixed solution of 100L methanol and ammoniacal liquor is added in the first slurries obtained（Wherein, methanol volume
The 50% of overall solution volume is accounted for, ammoniacal liquor accounts for the 15% of overall solution volume）, then global transfer enters in ultrasonic wave extraction apparatus, using 40kHZ
Frequency is with 3000W ultrasound intensities at 35 DEG C, and 500 rpm circulation stirrings effect 150min obtains the second slurries, and 4 DEG C of lucifuges are standby
With；
Step 3）：By step 2）The second slurries obtained are added in the plate centrifuge of 400 mesh filter clothes of configuration, are used
5000rpm is centrifuged, and collects the sediment on filter cloth；Sediment is added in air dry oven again, using 60 DEG C of dry 8h, then
Crush and obtain crushed material；
Step 4）：By step 3）Crushed material cross 80 mesh sieves, obtain the crushed material that granularity is less than or equal to 80 mesh；By 4.5kg powder
Mince and be fitted into 300 mesh Nylon Bags, be reloaded into subcritical abstraction tank, using 40L subcritical abstraction agent（Wherein 32L butane, 8L
Entrainer ethanol）, extracted 4 times at 50 DEG C, each extraction time is 40min, and extract is transferred in material pot, reclaim fourth
Alkane, obtains lycopene crude product；
Step 5）：By step 4）The lycopene crude product of acquisition, is fitted into sealing Brown Glass Brown glass bottles and jars only, adds 5L petroleum ethers, be filled with
Nitrogen, sealing is placed in 2h in -10 DEG C, and suction filtration reclaims petroleum ether, obtains crystal 21.35g.
Likewise, the crystal obtained passes through Mass Spectrometric Identification, can determine that it is lycopene；Product purity is 94.65%.
Embodiment 3
A kind of embodiment 3 prepares lycopene method in providing inferior fruit from cherry tomato, it comprises the following steps：
Step 1）：The discarded cherry tomato 30kg in field is collected, mouldy and immature fruit is rejected, removing mud is cleaned with deionized water
Sand, obtains the first slurries after draining, after crushing and beating；
Step 2）：In step 1）The mixed solution of 60L ethanol and ammoniacal liquor is added in the first slurries obtained（Wherein ethanol accounts for totality
Long-pending 40%, ammoniacal liquor of the total volume 10%）, then global transfer enters in ultrasonic wave extraction apparatus, is surpassed using 20kHZ and 59kHZ double frequencies
Sound wave（Two kinds of ultrasonic powers are identical, are 1800W）At 40 DEG C, 800 rpm circulation stirring 60min obtain the second slurries,
4 DEG C of lucifuges are standby；
Step 3）：By step 2）The second slurries obtained are added in the plate centrifuge of 200 mesh filter clothes of configuration, are used
3500rpm is centrifuged, and collects the sediment on filter cloth；Sediment is added in microwave drying oven again, using 50 DEG C of dry 4h, then
Crush and obtain crushed material；
Step 4）：By step 3）Crushed material cross 120 mesh sieves, obtain the crushed material that granularity is less than or equal to 120 mesh；By 1.53kg
Crushed material is fitted into 300 mesh Nylon Bags, is reloaded into subcritical abstraction tank, using 10L subcritical abstraction agent（Wherein 8.5L liquefies
Natural gas, 1.5L entrainer ethanol）, extracted 3 times at 35 DEG C, each extraction time is 60min, and extract is transferred into material pot
In, liquefied natural gas is reclaimed, lycopene crude product is obtained；
Step 5）：By step 4）The lycopene crude product of acquisition, is fitted into sealing Brown Glass Brown glass bottles and jars only, adds 5L petroleum ethers, be filled with
Nitrogen gas, sealing is placed in 1h in -5 DEG C, and suction filtration reclaims petroleum ether, obtains crystal 16.33g.
Likewise, the crystal obtained passes through Mass Spectrometric Identification, can determine that it is lycopene；Product purity is 94.06%.
The comparative example of embodiment 3
Comparative example and the raw material of embodiment 3 and operating process are essentially identical, differ only in：
The step 2 of comparative example）In alcohol extraction solvent use 60L ethanol solutions（The volume ratio of ethanol is 40%）, and embodiment 3
Step 2）In alcohol extraction solvent using 60L ethanol and ammoniacal liquor mixed solution（Wherein ethanol of the total volume 40%, ammoniacal liquor is accounted for always
The 10% of volume）；The step 4 of comparative example）In, using 10L liquefied natural gas as subcritical abstraction solvent, do not add entrainment
Agent, and and the step 4 of embodiment 3）Middle use 10L subcritical abstraction agent（Wherein 8.5L liquefied natural gas, 1.5L entrainer second
Alcohol）；
The lycopene crystal that comparative example is obtained is 12.05 g, and purity is 94.02%, far below embodiment 3 in yield
16.33g。
3 it can be seen that with the contrast of comparative example from the embodiments above and add ammoniacal liquor in alcohol extraction solvent, in subcritical abstraction
Increase ethanol in solvent as entrainer, the yield that lycopene is extracted from cherry tomato can be significantly improved.
It should be understood that, although the present specification is described in terms of embodiments, but not each embodiment only includes one
Individual independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art will should say
Bright book is as an entirety, and the technical scheme in each embodiment may also be suitably combined to form those skilled in the art can
With the other embodiment of understanding.
Those listed above is a series of to be described in detail only for feasibility embodiment of the invention specifically
Bright, they simultaneously are not used to limit the scope of the invention, all equivalent implementations made without departing from skill spirit of the present invention
Or change should be included in the scope of the protection.
Claims (10)
1. a kind of method for extracting lycopene, it is characterised in that this method comprises the following steps：
Step 1）The fruit of tomato kind is provided, and the first slurries will be obtained after the fruit crushing and beating；
Step 2）First slurries are carried out with ultrasonic alcohol extracting and obtains the second slurries；
Step 3）Second slurries are centrifuged, sediment is collected；Dry the sediment and crush acquisition crushed material；
Step 4）To step 3）The crushed material of acquisition carries out subcritical abstraction and obtains lycopene crude product；
Step 5）Purify the lycopene crude product and obtain lycopene product.
2. the method as described in claim 1, it is characterised in that
In the step 2）In, alcohol extraction solvent is added in first slurries, transfers in retort and carries out ultrasonic alcohol extracting
Processing, wherein, the treatment temperature of ultrasonic alcohol extracting is 20 ~ 50 DEG C, and processing time is 0.5 ~ 3h；Supersonic frequency is 10 ~ 60kHZ, is surpassed
Sound intensity is 20 ~ 200W/kg.
3. method as claimed in claim 2, it is characterised in that the alcohol extraction solvent is lower alcohol, low-alcohol solution or rudimentary
The mixed solution of alcohol and ammoniacal liquor, the lower alcohol is methanol and/or ethanol, wherein, and first slurries and the alcohol extracting
The ratio of solvent is 1kg: 1L ~ 1kg : 3L.
4. method as claimed in claim 3, it is characterised in that in the mixed solution of the lower alcohol and ammoniacal liquor, lower alcohol
Volume of the total volume 30% ~ 70%, the volume of the total volume 10% ~ 20% of ammoniacal liquor.
5. the method as described in claim 1, it is characterised in that in the step 3）In, centrifugation uses flat board centrifugation, from
Heart rotating speed is 2000 ~ 5000rpm, and collects the sediment using the filter cloth of 100 ~ 400 mesh.
6. the method as described in claim 1, it is characterised in that the step 4）In, sieve takes granularity to be less than or equal to 200 purposes
The crushed material carries out subcritical abstraction, wherein, the extractant that the subcritical abstraction is used includes propane, butane or liquid
The ratio range of change natural gas, the crushed material and the extractant is 1kg: 4L~ 1kg : 16L.
7. method as claimed in claim 6, it is characterised in that also contain 10% ~ 25% percent by volume in the extractant
Entrainer, the entrainer be ethanol.
8. method as claimed in claim 6, it is characterised in that the step 4）In, the temperature of the subcritical abstraction for 20 ~
50 DEG C, extraction times are 2 ~ 6 times, and each extraction time is 15 ~ 150min.
9. the method as described in claim 1, it is characterised in that the step 5）In, added in the lycopene crude product
Purification solvent, adjusts the temperature to -60 ~ 5 DEG C, stands after 0.5 ~ 5h, crystallisation by cooling, and suction filtration obtains the lycopene product；Institute
Purification solvent is stated for petroleum ether or normal hexane or their mixed liquors, the ratio of the lycopene crude product and purification solvent is 1kg
: 1L ~ 1kg : 4L。
10. method as in one of claimed in any of claims 1 to 9, it is characterised in that the fruit of the tomato kind is holy girl
Really.
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| CN110256189A (en) * | 2019-07-19 | 2019-09-20 | 长沙卫一生物科技有限公司 | The technique of lycopene is extracted from tomato peel |
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