CN105542951A - Method for removing pigments from micro-algal oil - Google Patents
Method for removing pigments from micro-algal oil Download PDFInfo
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- CN105542951A CN105542951A CN201410606051.9A CN201410606051A CN105542951A CN 105542951 A CN105542951 A CN 105542951A CN 201410606051 A CN201410606051 A CN 201410606051A CN 105542951 A CN105542951 A CN 105542951A
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Abstract
The invention discloses a method for removing pigments from micro-algal oil. The method adopts a solid phase extraction column made by adopting graphitized carbon to adsorb and remove pigments in the micro-algal oil to improve the quality of the oil, and can be applied in separation, analysis and purification processes of micro-algal lipids and removal of the pigments in micro-algal high-added value lipid product (DHA and EPA) food technologies. The method is suitable for rapidly removing pigments in oil of green algae, chrysophytes, diatoms, blue algae and other algae, and the pigment removal rate reaches 92% or above. The method has the advantages of simple operation, avoiding of heating, stirring, filtering and centrifuging steps in traditional oil decolorizing technologies, and high pigment removal rate.
Description
Technical field
The present invention relates to grease technical field of purification, specifically a kind of method of microalgae grease pigment removal.
Background technology
Micro-algae has that kind is many, photosynthetic efficiency is high, biological yield is high, growth cycle is short and self fat content advantages of higher, be considered to one of biomass energy raw material preparing biofuel the best, therefore in microdisk electrode and production process, lipid analysis is studied all significant to the regulation culture of micro-algae and metabolism.In addition polyunsaturated fatty acid is rich in micro-algae, especially docosahexenoic acid (DHA) and timnodonic acid (EPA) have higher effect in nutrition and medical field, the extraction of micro-algae polyunsaturated fatty acid, all strict sterilization is needed to refining from purebred cultivation, aseptic technique, DHA, EPA purity of producing is high, pollution-free, and not containing fishy smell, quality far wins fish oil DHA.But pigment content is high in micro-algae, affect grease color and quality, therefore the removing as requisite step in grease compartment analysis and polyunsaturated fatty acid production technique of microalgae grease pigment.The decoloration process being directed to grease at present mainly adopts physical adsorption decolouring and SYNTHETIC OPTICAL WHITNER decolouring.Sorbent material decolouring utilizes some to have compared with the adsorbing material of strong selectivity, adsorpting pigment and other impurity are to carry out the method purified under certain condition, compared to the decolouring of SYNTHETIC OPTICAL WHITNER, adsorption bleaching can remove the interference of pigment and impurity, inherently changes oil quality and purity.Conventional decoloring material comprises gac, atlapulgite, hydrogen peroxide, and bleaching temperature is generally at 60-150 ゜ C, adsorption time 15-40min, under stirring, pigment is adsorbed, then through filtering, the operation such as centrifugal carries out being separated of sample and sorbent material, this process is more loaded down with trivial details, power consumption, time-consuming, and pigment removal rate is lower, at 50-80%.
Graphitized carbon is obtained through the surface activating process preparation of uniqueness by extraordinary carbon black material, the positive six-membered ring structure on its surface, it is made to have extremely strong avidity to planar molecule, there is high decontamination effect improving, high-recovery and the reproducible good characteristic of height, be applied in farming residual analysis, in the pre-treatment of the particularly sample that the pigment such as vegetable and fruit is higher.The present invention for material, carries out adsorbing and removing to pigment in microalgae grease with graphitized carbon solid-phase extraction column.
Summary of the invention
The object of the present invention is to provide a kind of method being applicable to microalgae grease pigment removal.
To achieve these goals, the technical solution used in the present invention content is:
(1) pigment removal
First by graphitized carbon solid-phase extraction column (200mg-1000mg) 1-5mL sample solvent activation, solvent flows out naturally.
Loading oil quality is the 2%-10% of graphitized carbon filler, can repeatedly loading, and applied sample amount or loading number of times are to adsorb rear required pigment removal rate for standard.Elutriant is fat solvent, and negative pressure vacuumizes and ensures that elutriant liquid is about 10-20 and drips/min outflow, and elution volume is 10-15 times of column volume.
(2) pigment removal rate calculates
Because there is chlorophyll class and the large class pigment of carotenoids two in micro-algae simultaneously, and the maximum absorption wavelength of different micro-algae two class pigments there are differences, so determine two maximum absorption wavelengths of two class pigments according to the kind full scan of micro-algae, and calculate pigment removal rate.
A in formula
0for the light absorption value of the front grease that decolours; A
1for the light absorption value of grease after decolouring
The present invention compared with prior art tool has the following advantages:
The present invention compared with prior art tool has the following advantages:
1. method is simple: only need solid-phase extraction device a set of, without the need to heating compared with existing pigment removal technique, and the operations such as stirring, without the need to absorption reaction still and filtration, non-pigment adsorption time.
2. pigment removal rate is high: pigment removal rate up to more than 92%, higher than the pigment removal rate of hydrogen peroxide, gac and atlapulgite.
3. avoid the oxidation of polyunsaturated fatty acid: present method can adopt normal temperature or cold operation, the oxidation of the polyunsaturated fatty acid avoiding heating or use oxidisability discoloring agent to cause.
Accompanying drawing explanation
Fig. 1 graphitized carbon Solid-Phase Extraction is to lsochrysis zhanjiangensis pigment removal
Grease applied sample amount is on the contrast (b) 1 of grease before and after the impact (a) of percent of decolourization and decolouring: before decolouring; 2: after decolouring
Fig. 2 graphitized carbon Solid-Phase Extraction removes micro-plan ball phycochrome
Grease applied sample amount is on the contrast (b) 1 of grease before and after the impact (a) of percent of decolourization and decolouring: before decolouring; 2: after decolouring
Fig. 3 graphitized carbon Solid-Phase Extraction diagonal angle hair phycochrome removes
Grease applied sample amount is on the contrast (b) 1 of grease before and after the impact (a) of percent of decolourization and decolouring: before decolouring; 2: after decolouring.
Fig. 4 graphitized carbon Solid-Phase Extraction is to spirulina pigment removal
Grease applied sample amount is on the impact of percent of decolourization.
Embodiment
Below by specific embodiment, method of the present invention and result are described.
Embodiment 1
Micro-algae used is lsochrysis zhanjiangensis (Isochrysiszhangjiangensis), and pigment removal step is as follows
(1) microalgae grease extracts
Take the micro-algae powder of 100mg, add Extraction solvent chloroform-methanol-water (1:2:0.8v/v/v) 3.8mL and carry out ultrasonication extraction (400w, ultrasonic 5s, interval 5s, ultrasonic 5 times), add 1mL chloroform and 1mL water mixes, after centrifugal layering, get chloroform layer constant volume in 2mL volumetric flask.
(2) pigment removal
First by graphitized carbon solid-phase extraction column (filler 200mg) 2mL chloroform activation, loading oil quality is respectively 4.86,7.29,9.72,12.15mg, be respectively 2.43% of graphitized carbon filler, 3.65%, 4.86%, 6.08%, the volume of eluting solvent chloroform is 10 times of column volume.
(3) pigment removal rate calculates
Because there is the large class pigment of chlorophyll class and carotenoids two in micro-algae simultaneously so, and the maximum absorption wavelength of different micro-algae two class pigments there are differences, so determine two maximum absorption wavelengths of two class pigments according to the kind full scan of micro-algae, be respectively 662nm and 466nm at the maximum absorption wavelength of lsochrysis zhanjiangensis Determination of Chlorophyll and carotenoid, and calculate pigment removal rate.
A in formula
0for the light absorption value of the front grease that decolours; A
1for the light absorption value of grease after decolouring
(4) pigment takes off result
Fig. 1 a shows applied sample amount to the impact of pigment decreasing ratio, and within the scope of applied sample amount 2.43%-6.08%, graphitized carbon reaches more than 99.8% to chlorophyll class decreasing ratio.When applied sample amount increases, the decreasing ratio of carotenoid declines, and when applied sample amount is 6.08%, the decreasing ratio of graphitized carbon filler to lsochrysis zhanjiangensis Determination of Chlorophyll class reaches 99.8%, and the decreasing ratio of carotenoids is 92.4%.Fig. 1 b shows the change of grease before and after decolouring, and before and after display decolouring, grease is substantially unchanged
Embodiment 2
Micro-algae used is micro-plan ball algae (NannochloropsisoceanicaIMET1), and pigment removal step is as follows
(1) microalgae grease extracts
Take the micro-algae powder of 100mg, add Extraction solvent chloroform-methanol-water (1:2:0.8v/v/v) 3.8mL and carry out ultrasonication extraction (400w, ultrasonic 5s, interval 5s, ultrasonic 5 times), add 1mL chloroform and 1mL water mixes, after centrifugal layering, get chloroform layer constant volume in 2mL volumetric flask.
(2) pigment removal
First by graphitized carbon solid-phase extraction column (filler 200mg) 2mL chloroform activation, loading oil quality is respectively 5.82,8.73,11.64,17.46mg, be respectively 2.91% of graphitized carbon filler, 4.37%, 5.82%, 8.73%, the volume of eluting solvent chloroform is 10 times of column volume.
(3) pigment removal rate calculates
Because there is the large class pigment of chlorophyll class and carotenoids two in micro-algae simultaneously so, and the maximum absorption wavelength of different micro-algae two class pigments there are differences, so determine two maximum absorption wavelengths of two class pigments according to the kind full scan of micro-algae, be respectively 662nm and 436nm at the maximum absorption wavelength of micro-plan ball algae Determination of Chlorophyll and carotenoid, and calculate pigment removal rate.
A in formula
0for the light absorption value of the front grease that decolours; A
1for the light absorption value of grease after decolouring
(4) pigment takes off result
Fig. 2 shows the impact of applied sample amount on pigment decreasing ratio, and within the scope of applied sample amount 2.91%-8.73%, graphitized carbon reaches more than 99.8% to chlorophyll class decreasing ratio.When applied sample amount increases, the decreasing ratio of carotenoid declines, and when applied sample amount is 8.73%, the decreasing ratio of graphitized carbon filler to lsochrysis zhanjiangensis Determination of Chlorophyll class reaches 99.8%, and the decreasing ratio of carotenoids is 96.1%.Fig. 2 shows the change of grease before and after decolouring, and before and after display decolouring, grease is substantially unchanged.
Embodiment 3
Micro-algae used is Chaetoceros (Chaetoceros), and pigment removal step is as follows
(1) microalgae grease extracts
Take the micro-algae powder of 100mg, add Extraction solvent chloroform-methanol-water (1:2:0.8v/v/v) 3.8mL and carry out ultrasonication extraction (400w, ultrasonic 5s, interval 5s, ultrasonic 5 times), add 1mL chloroform and 1mL water mixes, after centrifugal layering, get chloroform layer constant volume in 2mL volumetric flask.
(2) pigment removal
First by graphitized carbon solid-phase extraction column (filler 200mg) 2mL chloroform activation, loading oil quality is respectively 3.1,6.2,9.3,13.2mg, be respectively 1.55% of graphitized carbon filler, 3.10%, 4.65%, 6.58%, the volume of eluting solvent chloroform is 10 times of column volume.
(3) pigment removal rate calculates
Because there is the large class pigment of chlorophyll class and carotenoids two in micro-algae simultaneously so, and the maximum absorption wavelength of different micro-algae two class pigments there are differences, so determine two maximum absorption wavelengths of two class pigments according to the kind full scan of micro-algae, be respectively 662nm and 428nm at the maximum absorption wavelength of Chaetoceros Determination of Chlorophyll and carotenoid, and calculate pigment removal rate.
A in formula
0for the light absorption value of the front grease that decolours; A
1for the light absorption value of grease after decolouring
(4) pigment takes off result
Fig. 4 a shows the impact of applied sample amount on pigment decreasing ratio, and within the scope of applied sample amount 1.55%-6.58%, graphitized carbon reaches more than 99.2% to chlorophyll class decreasing ratio.When applied sample amount increases, the decreasing ratio of carotenoid declines, and when applied sample amount is 6.58%, the decreasing ratio of graphitized carbon filler to lsochrysis zhanjiangensis Determination of Chlorophyll class reaches 99.2%, and the decreasing ratio of carotenoids is 98.2%.Fig. 4 b shows the change of grease before and after decolouring, and before and after display decolouring, grease is substantially unchanged.
Embodiment 4
Micro-algae used is spirulina (Spirulinaplatensis), and pigment removal step is as follows
(1) microalgae grease extracts
Take the micro-algae powder of 100mg, add Extraction solvent chloroform-methanol-water (1:2:0.8v/v/v) 3.8mL and carry out ultrasonication extraction (400w, ultrasonic 5s, interval 5s, ultrasonic 5 times), add 1mL chloroform and 1mL water mixes, after centrifugal layering, get chloroform layer constant volume in 2mL volumetric flask.
(2) pigment removal
First by graphitized carbon solid-phase extraction column (filler filler 200mg) 2mL chloroform activation, loading oil quality is respectively 2.7,5.4,8.1,10.8mg, be respectively 1.35% of graphitized carbon filler, 2.70%, 4.05%, 5.40%, the volume of eluting solvent chloroform is 10 times of column volume.
(3) pigment removal rate calculates
Because there is the large class pigment of chlorophyll class and carotenoids two in micro-algae simultaneously so, and the maximum absorption wavelength of different micro-algae two class pigments there are differences, so determine two maximum absorption wavelengths of two class pigments according to the kind full scan of micro-algae, be respectively 662nm and 428nm at the maximum absorption wavelength of spirulina Determination of Chlorophyll and carotenoid, and calculate pigment removal rate.
A in formula
0for the light absorption value of the front grease that decolours; A
1for the light absorption value of grease after decolouring
(4) pigment takes off result
Fig. 3 shows the impact of applied sample amount on pigment decreasing ratio, and when applied sample amount is 5.40%, the decreasing ratio of graphitized carbon filler to lsochrysis zhanjiangensis Determination of Chlorophyll class reaches 94.9%, and the decreasing ratio of carotenoids is 92.6%.Because in spirulina, fat content is few, do not show the change of the grease before and after decolouring.
Claims (7)
1. a microalgae grease pigment removal method, its feature exists: utilize graphitized carbon solid-phase extraction column to carry out adsorbing and removing to the pigment contained by the microalgae grease be dissolved in solvent.
2. in accordance with the method for claim 1, it is characterized in that: concrete steps are as follows: (1) solid-phase extraction column activates; Refer to and adopt solvent soaking graphitized carbon solid-phase extraction column, activating solvent and the solvent phase dissolving grease with, suitable solvents scope comprises: one or two or more kinds in chloroform, methyl alcohol, acetone, normal hexane, normal heptane, water; (2) loading; (3) wash-out.
3. in accordance with the method for claim 3, it is characterized in that: in described step (3), eluting solvent is the solvent dissolving grease, eluting solvent consumption is 10-15 times of packing volume in post.
4. according to the method described in claim 1,2 or 3, it is characterized in that: dissolving the solvent of grease is one or two or more kinds in chloroform, methyl alcohol, acetone, normal hexane, normal heptane, water.
5. in accordance with the method for claim 2, it is characterized in that: in described step (2), sample applied sample amount is the 2%-10% of graphitized carbon packing quality.
6. according to method described in claim 1, it is characterized in that: described micro-algae comprises one or two or more kinds in green alga, blue-green algae, chrysophyceae and diatom.
7. according to method described in claim 1, it is characterized in that: the filler of described solid-phase extraction column is graphitized carbon, filler mean particle size: 120-400 order, specific surface area: 100m2/g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734466A (en) * | 2018-07-19 | 2020-01-31 | 中国科学院大连化学物理研究所 | method for extracting monogalactosyldiacylglycerol from microalgae |
| CN111100173A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院大连化学物理研究所 | Method for selectively enriching monogalactosyldiacylglycerol in microalgae |
| CN113122387A (en) * | 2019-12-30 | 2021-07-16 | 丰益(上海)生物技术研发中心有限公司 | Method for decoloring oil and removing plasticizer |
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| CN102489249A (en) * | 2011-11-25 | 2012-06-13 | 中国检验检疫科学研究院 | Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof |
| CN102965182A (en) * | 2012-11-27 | 2013-03-13 | 新奥科技发展有限公司 | Method for extracting grease from schizochytrium |
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| US5494500A (en) * | 1990-11-26 | 1996-02-27 | The Social Welfare Foundation Hokkaido Rehabily | Activated carbon, production thereof and adsorption using activated carbon |
| CN102489249A (en) * | 2011-11-25 | 2012-06-13 | 中国检验检疫科学研究院 | Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734466A (en) * | 2018-07-19 | 2020-01-31 | 中国科学院大连化学物理研究所 | method for extracting monogalactosyldiacylglycerol from microalgae |
| CN111100173A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院大连化学物理研究所 | Method for selectively enriching monogalactosyldiacylglycerol in microalgae |
| CN113122387A (en) * | 2019-12-30 | 2021-07-16 | 丰益(上海)生物技术研发中心有限公司 | Method for decoloring oil and removing plasticizer |
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