CN109439699A - The method of Long carbon chain triglycerides in a kind of preparation of litsea cubeba kernel oil tea oil - Google Patents
The method of Long carbon chain triglycerides in a kind of preparation of litsea cubeba kernel oil tea oil Download PDFInfo
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- CN109439699A CN109439699A CN201811297708.2A CN201811297708A CN109439699A CN 109439699 A CN109439699 A CN 109439699A CN 201811297708 A CN201811297708 A CN 201811297708A CN 109439699 A CN109439699 A CN 109439699A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
- C12P7/6436—Fatty acid esters
- C12P7/6445—Glycerides
- C12P7/6463—Glycerides obtained from glyceride producing microorganisms, e.g. single cell oil
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Abstract
The method of Long carbon chain triglycerides in a kind of preparation of litsea cubeba kernel oil tea oil, litsea citrate oil is mixed with tea oil according to certain mass proportion, the decompression dehydration under solvent-free system, immobilized lipase is added, it is preheated to set temperature and realizes ester Ester exchange, then after the mixture for realizing ester Ester exchange being separated, adsorbent is added and is stirred under vacuum, obtains the product containing middle long carbon chain structure triglycerides after carrying out the rectifying of two-part molecule after then the material after absorption is filtered by vacuum.The present invention is using litsea cubeba kernel oil as raw material, the technique handled using enzyme immobilization technology, technological design is reasonable, enzyme loss late is low, it is low in cost, the residual of solvent is reduced, and structured triglyceride import drugs registered standard requirement bulk pharmaceutical chemicals is met for subsequent purification preparation by this method, acceptable material is provided, market potential is huge.
Description
Technical field
The invention belongs to the high-valued applied technical fields of woody oleiferous plants.More particularly to a kind of ester -ester under catalytic condition
The method that exchange reaction prepares Long carbon chain triglycerides in the litsea cubeba kernel oil tea oil preparation of functional triglyceride.
Background technique
The fruit of a cubeb litsea tree [litsea cubeba (Lour.) pers.] also known as cubeb litsen tree, Tetranthera citrata, the wooden ginger seed etc. are Lauraceae wood
The dungarunga that Jiang Zi belongs to is widely distributed in the mountainous region or hills that provinces and regions are waited on the south the Yangtze river basin.The fruit of a cubeb litsea tree be production litsea citrate oil,
The important species obtained through refining natural lemon aldehyde, manufacture natural essence raw material.The artificial growth fruit of a cubeb litsea tree is to develop hills, mountain area economy
One of the important channel that one of important channel and remote mountain areas farmers' extra earning are shaken off poverty and set out on the road to prosperity.Chinese litsea citrate oil annual output
More than 2000 tons, for maximum producing country and exported country, product are exported to the states such as beauty, day, English, method, moral, Switzerland, Holland, enjoy in the world
Reputation is domestic and international.But at this stage utilize the more volatile essential oil for the fruit of a cubeb litsea tree, and to containing fixedness grease, pectin,
The kernel of starch and protein then directly abandons, and the discarding of this large amount of kernel resource not only causes fruit of a cubeb litsea tree resource utilization
Lowly, and to ecological environment serious pollution is also resulted in.Litsea cubeba kernel oil is contained in clotbur seed after removing pericarp
Oil, the grey seed nuclei oil content in mountain oil content in the kernel after 27% or so, decladding is then up to 60%, be a kind of oil content very
High oil plant.The fatty acid of litsea cubeba kernel oil, which is mainly organized, to be become as lauric acid (C12H24O2) 56.4%, capric acid
(C10H20O2) 19.8%, dodecenoic acid (C12H22O2) 13.6%, these three ingredients account for the 89.8% of total amount, and great depth adds
Work Development volue.
Tea oil is referred to as " east olive oil ", not only has 80% or more unsaturated fatty acid, also contains physiological activity
Ingredient squalene, dimension E, tea saponin etc., oxygen-enriched ability is strong, can anti anoxia and antifatigue, and have and improve the immunity of the human body and increase
Into the function of gastrointestinal tract.Scientific research institution is to " tea oil and olive oil have carried out comparative study, oily although the two has similarity
The dietotherapy dual function of tea oil is actually superior to olive oil, and it's also better than any other oil, is the king of edible vegetable oil.
Middle Long carbon chain triglycerides refers on a glycerol backbone simultaneously containing medium-chain fatty acid and Long carbon chain fat
The triglycerides of acid.It relative to sweet three ester of Long carbon chain have it is more low in calories, belong to low calorie fats, while it has middle carbochain again
The essential fatty acid that triglycerides does not have.Therefore it can not only quickly be energized for body, and be rich in more insatiable hungers
And fatty acid, nitrogen balance can be enhanced and improve the bioavilability of nutritional ingredient, be therefore widely used in medicine, food etc.
Field.CN 103891920A discloses a kind of fat or oil composition and preparation method thereof of middle Long carbon chain triglycerides, mainly adopts
It is catalyst with sodium methoxide, but wherein chain triglyceride content is not expressed.It is developed using litsea cubeba kernel oil and tea oil as base-material
The middle Long carbon chain triglyceride of high added value can satisfy the needs of different crowd, effectively facilitates the extension of industrial chain, exists at present
The area research is less, if being applied to the exploitation of edible oil and fat, can also avoid miscella caused by simple physical mixture
Functional the defects of not having of physical instability, lipid.
The research both at home and abroad for Long carbon chain triglycerides in litsea cubeba kernel oil-tea oil preparation functionality yet there are no at present
Report, the present invention mainly from the grey seed resources effective utilization angle in mountain, improve the overall economic efficiency of the industry, while also expanding
The application field of big tea oil resource.
Summary of the invention
Technical problem solved by the invention is to provide Long carbon chain glycerol three in a kind of litsea cubeba kernel oil tea oil preparation
The method of ester, this method using litsea cubeba kernel oil and tea oil as base-material, under the conditions of enzyme can be efficient, single-minded prepare
Long-chain carbon glyceride realizes the production of functional high value added product.
Technical problem solved by the invention is realized using following technical scheme:
The method of Long carbon chain triglycerides in a kind of preparation of litsea cubeba kernel oil tea oil, by litsea citrate oil and tea oil according to one
Determine quality proportioning mixing, the decompression dehydration under solvent-free system is added immobilized lipase, is preheated to set temperature, vacuum is stirred
It mixes, absorption filters, and the product containing middle long carbon chain structure triglycerides is obtained after molecule rectifying.
Its concrete operation method are as follows:
1) decompression dehydration: the ratio of litsea cubeba kernel oil, tea oil mass ratio 1: 1~2: 1 is mixed, progress is added to the container
Decompression dehydration, carry out decompression dehydration time control container dehydration temperaturre 80~100 DEG C are risen in 20min~40min, until liquid level without
Bubble generates, then 100~120 DEG C are continuously heating in 10~20min, then keeps vacuum, breaks heat source, keeps material cooling
To 30~50 DEG C, restore normal pressure, it is spare.
2) ester Ester exchange: the raw material of step 1) processing being taken out and is used as substrate, is carried out gel embedding using immobilised enzymes and is urged
Change and realize ester Ester exchange, control reaction temperature is 45 DEG C~95 DEG C when reaction, and vacuum degree is 0.08MPa~0.09MPa, when reaction
Between be 2h~6h, then reactant is centrifuged.
3) absorption filters: keeping the temperature to the rich mixture being centrifuged in step 2), control temperature of charge is 60 DEG C, is added
Entering adsorbent, adsorbent is mixture, it matches as active carbon: carclazyte: adsorption silica gel=2: 5: 3, additional amount is rich mixture
The 3%~5% of quality reacts 20min~40min, finishes and be filtered by vacuum, and it is spare that material enters subsequent workshop section.
4) two-part rectifying molecule rectifying: is carried out to the material of step 3) preparation:
First stage parameter: charging rate 0.1ml/min~0.3ml/min, 200 DEG C~210 DEG C of autoclave body temperature, revolving speed
150r/min~200r/min, 10 DEG C~20 DEG C of cooling temperature, vacuum degree 5Pa~10Pa collects heavy phase, into next stage
Molecule rectifying.
Second stage parameter: charging rate 0.1ml/min~0.3ml/min, 230 DEG C~250 DEG C of autoclave body temperature, revolving speed
200r/min~250r/min, 10 DEG C~20 DEG C vacuum degree 1Pa~5Pa of cooling temperature collect light phase to get finished product.
As further technology limiting of the invention:
In the step 1), litsea cubeba kernel oil is preferably fruit of a cubeb litsea tree kernel polished fat, and tea oil is preferably low-temperature physics
Squeeze non-polished fat.
It, can be by litsea cubeba kernel oil, tea oil together with catalyst in order to improve the speed of decompression dehydration in the step 1)
It is added to the container and carries out catalysis reaction.
In the step 1), when the decompression dehydration operates, by container vacuum-pumping to 0.1~0.3MPa, and constant temperature is utilized
The control of container for stirring revolving speed is carried out dehydrating operations by magnetic stirring apparatus in the range of 200~400r/min.
In the step 2), the catalyst system due to participating in reaction is solvent-free catalyst system, for optimal reaction effect
Fruit, catalyst can be added by needing for substrate to be preheated to 40 DEG C.
In the step 2), the immobilised enzymes is that the mass ratio of Lipozyme 435 and porcine pancreatic lipase PPL is 1
: 1~1: 3 mixture, and the usage amount of the immobilised enzymes is the 3%~10% of substrate quality.
In the step 2), when being centrifuged, the mixture of end of reaction is subjected to high-speed separation, will be mixed when cooling
Close object and be cooled to room temperature 25~30 DEG C, centrifuge speed is 4000r/min~8000r/min, centrifugation time be 10min~
20min。
Advantages of the present invention and beneficial effect are:
(1) present invention in developed with litsea cubeba kernel oil resource, waste material is not only utilized, make its change give up into
Treasured, and reduce the destruction to ecological environment.
(2) present invention uses enzyme immobilization technology, can reduce the loss of enzyme while guaranteeing enzymatic effect, and
And end of reaction can quick separating, simplify technique.
(3) present invention is reacted using solvent-free system, can effectively reduce the residual of solvent.
(4) present invention is catalyzed and synthesized using enzyme process, single can not only be efficiently promoting the progress of reaction positive direction,
It also can avoid pollution of the chemical catalyst to lipid product simultaneously, reduce residual.
(5) the middle Long carbon chain triglycerides in the present invention can not only be applied to healthcare field, can also be using medicine, baby children
The fields such as youngster's milk powder greatly improve the economic value of raw material.
Detailed description of the invention
Fig. 1 is processing process schematic diagram of the invention.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment and artwork flow diagram shown in FIG. 1 are closed, the present invention is further explained.
Embodiment one:
Litsea citrate oil is mixed with tea oil according to the proportion of quality 1: 1, the decompression dehydration under solvent-free system, dehydration temperaturre control
25min processed rises to 90 DEG C, until liquid level bubble-free generates；110 DEG C are continuously heating to, time 10min.Continue to keep vacuum,
Heat source is broken, material is cooled to 35 DEG C, restores normal pressure, spare.Substrate is preheated to 40 DEG C of addition catalyst (Lipozyme 435
It is 1: 1 with porcine pancreatic lipase PPL proportion, usage amount is the 6% of substrate quality), reaction time 3h, reaction temperature is 80 DEG C, very
Reciprocal of duty cycle is 0.09MPa.The mixture of end of reaction is subjected to high-speed separation, mixture is cooled to room temperature 30 DEG C, centrifuge speed
For 6000r/min, it is centrifuged 10min.Adsorbent is added in the rich mixture being centrifuged, 60 DEG C of temperature of charge, adsorbent is added
Amount 3%, reaction time 20min is finished and is filtered by vacuum.
Molecular distillation technique carries out rectifying.
First stage parameter: charging rate 0.1ml/min, 200 DEG C of autoclave body temperature, revolving speed 150r/min, cooling temperature 20
DEG C, vacuum degree 5Pa.Heavy phase is collected, into next stage molecule rectifying.
Second stage parameter: charging rate 0.1ml/min, 230 DEG C of autoclave body temperature, revolving speed 200r/min, cooling temperature 10
DEG C, vacuum degree 1Pa.Light phase is collected, as product, the content of middle Long carbon chain triglycerides is 71.2%.
Specific embodiment 2
Litsea citrate oil is mixed with tea oil according to the proportion of quality 1: 1.2, the decompression dehydration under solvent-free system, dehydration temperaturre
Control 20min rises to 100 DEG C, until liquid level bubble-free generates；120 DEG C are continuously heating to, time 10min.Continue to keep true
Sky breaks heat source, and material is cooled to 35 DEG C, restores normal pressure, spare.Substrate is preheated to 40 DEG C of addition catalyst (Lipozyme
435 and porcine pancreatic lipase PPL proportion is 1: 1, and usage amount is the 7% of substrate quality), reaction time 6h, reaction temperature is 85 DEG C,
Vacuum degree is 0.09MPa.The mixture of end of reaction is subjected to high-speed separation, mixture is cooled to room temperature 30 DEG C, centrifugal basket
Speed is 6000r/min, is centrifuged 10min.Adsorbent is added in the rich mixture being centrifuged, 60 DEG C of temperature of charge, adsorbent adds
Enter amount 3%, reaction time 20min is finished and is filtered by vacuum.
Molecular distillation technique carries out rectifying.
First stage parameter: charging rate 0.1ml/min, 200 DEG C of autoclave body temperature, revolving speed 180r/min, cooling temperature 10
DEG C, vacuum degree 3Pa.Heavy phase is collected, into next stage molecule rectifying.
Second stage parameter: charging rate 0.1ml/min, 250 DEG C of autoclave body temperature, revolving speed 220r/min, cooling temperature 10
DEG C, vacuum degree 0.8Pa.Light phase is collected, as product, the content of middle Long carbon chain triglycerides is 81.2%.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of method of Long carbon chain triglycerides in litsea cubeba kernel oil tea oil preparation, which is characterized in that concrete operation method
Are as follows:
1) decompression dehydration: the ratio of litsea cubeba kernel oil, tea oil mass ratio 1: 1~2: 1 is mixed, is added to the container and is depressurized
Dehydration carries out decompression dehydration time control container dehydration temperaturre and rises to 80~100 DEG C in 20min~40min, until liquid level bubble-free
It generates, then is continuously heating to 100~120 DEG C in 10~20min, then keep vacuum, break heat source, material is made to be cooled to 30
~50 DEG C, restore normal pressure, it is spare；
2) ester Ester exchange: the raw material of step 1) processing being taken out and is used as substrate, and it is real to carry out gel embedding catalysis using immobilised enzymes
Existing ester Ester exchange, control reaction temperature is 45 DEG C~95 DEG C when reaction, and vacuum degree is 0.08MPa~0.09MPa, and the reaction time is
Then 2h~6h is centrifuged reactant；
3) absorption filters: keeping the temperature to the rich mixture being centrifuged in step 2), control temperature of charge is 60 DEG C, is added and inhales
Attached dose, adsorbent is mixture, is matched as active carbon: carclazyte: adsorption silica gel=2: 5: 3, additional amount is rich mixture quality
3%~5%, react 20min~40min, finish and be filtered by vacuum, material enter subsequent workshop section it is spare；
4) two-part rectifying molecule rectifying: is carried out to the material of step 3) preparation:
First stage parameter: charging rate 0.1ml/min~0.3ml/min, 200 DEG C~210 DEG C of autoclave body temperature, revolving speed 150r/
Min~200r/min, 10 DEG C~20 DEG C of cooling temperature, vacuum degree 5Pa~10Pa collects heavy phase, into next stage molecule
Rectifying；
Second stage parameter: charging rate 0.1ml/min~0.3ml/min, 230 DEG C~250 DEG C of autoclave body temperature, revolving speed 200r/
Min~250r/min, 10 DEG C~20 DEG C vacuum degree 1Pa~5Pa of cooling temperature collect light phase to get finished product.
2. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
In the litsea cubeba kernel oil is fruit of a cubeb litsea tree kernel polished fat.
3. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
In the tea oil is the non-polished fat of low-temperature physics squeezing.
4. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
When carrying out decompression dehydration operation in, the step 1), stirred by container vacuum-pumping to 0.1~0.3MPa, and using constant temperature magnetic force
It mixes device and the control of container for stirring revolving speed is subjected to dehydrating operations in the range of 200~400r/min.
5. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
In needing that catalyst is added after substrate to be preheated to 40 DEG C in the step 2).
6. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
In the immobilised enzymes is the mixture that the mass ratio of Lipozyme 435 and porcine pancreatic lipase PPL is 1: 1~1: 3.
7. Long carbon chain triglycerides in any litsea cubeba kernel oil tea oil preparation according to claim 1 or in 6
Method, which is characterized in that the usage amount of the immobilised enzymes be substrate quality 3%~10%.
8. the method for Long carbon chain triglycerides, feature exist in litsea cubeba kernel oil tea oil preparation according to claim 1
In in the step 2), when being centrifuged, by the mixture progress high-speed separation of end of reaction, by mixture when cooling
25~30 DEG C are cooled to room temperature, centrifuge speed is 4000r/min~8000r/min, and centrifugation time is 10min~20min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113073122A (en) * | 2021-04-29 | 2021-07-06 | 江南大学 | Method for preparing hot pot seasoning oil rich in medium-long carbon chain triglyceride by enzyme method |
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Application publication date: 20190308 |