CN104206562A - Method for preparing DHA (Docosahexaenoic acid)-enriched vegetable oil by adopting one-step process - Google Patents
Method for preparing DHA (Docosahexaenoic acid)-enriched vegetable oil by adopting one-step process Download PDFInfo
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Abstract
The invention discloses a method for preparing DHA (Docosahexaenoic acid)-enriched vegetable oil by adopting a one-step process. The method mainly comprises the following processes: uniformly mixing ground schizochytrium powder and a proper amount of vegetable oil to obtain a mixture, adding the mixture to an extraction kettle, and statically soaking under the certain temperature and pressure; and performing dynamic extraction, grinding obtained algae dregs once again after extraction, and repeating previous operations to extract twice. The method for extracting DHA, disclosed by the invention, has the advantages of being free from toxicity, slight in smell and low in cost, and the method avoids damage on the product quality and improves the DHA extraction efficiency; and the obtained DHA-enriched vegetable oil can be further refined as a raw material to prepare the vegetable oil containing the DHA; and therefore, the method has a relatively strong application value.
Description
Technical field
The invention belongs to technical field of natural product extraction, be specifically related to the method that the vegetable oil of DHA is rich in the preparation of a kind of one-step method.
Background technology
DHA (Docosahexaenoic acid, 22:6 △ 4.7.10.13.16.19, full name DHA) be a kind of long-chain polyunsaturated fatty acid (polyunsaturated fatty acid is called for short PUFA) belonging to ω-3 series.This material has many very important physiological functions, such as suppresses platelet aggregation, reduces thromboxane and is formed, thus the generation of prevention miocardial infarction, cerebral infarction; Reducing blood lipid, preventing arteriosclerosis; Anti-inflammatory; Brain tonic and intelligence development, improves ability of learning and memory, improves retinal function, vision protection; Anticancer; The effects such as control senile dementia.Because DHA has above effect, and human body itself cannot synthesize DHA, and (people and other mammal only have △ 4, △ 5, △ 6 and △ 9 desaturase, lack the desaturase of △ more than 9, therefore self DHA cannot be synthesized, must be provided by food), need to supplement from ordinary meal.Current DHA has been widely used in pharmaceuticals, food and feed industry.
Marine fishes are the main sources extracting DHA, but because fish oil has the shortcomings such as resource-constrained, output is unstable, yield is low, purifying process is complicated, depend merely on current deep sea fish oil to produce the demand that DHA far can not meet people, need to find new replaced resource.And proved in micro-algae to be rich in multiple polyunsaturated fatty acids as leukotrienes, linoleic acid, DHA, EPA etc., be the potential source carrying out DHA commercial development.Micro-algae has been developed to plurality kinds of health care product now as spirulina powder, spirulina chewing tablets etc.
American-European countries is 160-400mg/day to the suggestion of human body DHA every day intake, and compatriots are only about 40mg from the intake food every day, therefore how to prepare be rich in DHA edible oil to meet the life requirement of the mankind, be one of emphasis in aliphatic acid Application and Development.At present, the polyunsaturated fatty acids separation method applied in laboratory and actual production has low temperature staging, urea adduct method, solvent method, salt forming method, molecularly distilled, supercritical carbon dioxide extraction method, lipase method and high performance liquid chromatography etc.Supercritical carbon dioxide extraction method is owing to having larger prospects for commercial application in these methods, is subject to extensive concern.
Supercritical carbon dioxide extraction method utilizes carbon dioxide to have the extraction function of similar organic solvent character in the supercritical state to carry out material extracts active ingredients and a kind of advanced technology be separated.Have extracting power to carry by force, extraction efficiency is high; Critical-temperature is low, and operating temperature is low, can intact preservation extract active ingredient not be destroyed; Operating parameter easily controls; Cheaply be easy to get, operating cost is low; The advantages such as the rear no solvent residue of extraction, have broad application prospects in the development and utilization of living resources and the extraction of Effective Component of Chinese Medicine and refining.
The effect of extracting of supercritical carbon dioxide affects by several factors, comprises the character of extracting substance, temperature during extraction, pressure, and the use of polarity flux.Because carbon dioxide is nonpolar, the solubility of pure supercritical carbon dioxide fluid to the material with polarity is poor, therefore need to add polar solvent to improve the solubility of supercritical carbon dioxide, so correctly use polarity flux can widen the range of application of supercritical carbon dioxide when extracting physiological activator significantly, thus improve the selective of the solubility of target component in carbon dioxide and supercritical fluid.
The more polarity flux of current use is methyl alcohol, ethanol, acetone, propane etc., utilize organic solvent can face the solvent removal in later stage, the energy that this process need consumption is a large amount of, also easily brings residual to product, therefore need to find a kind of novel dissolvent removed without the need to the later stage.
Along with social progress, growth in the living standard, people more and more pay attention to the health-care effect of edible oil, therefore in edible oil, add the development trend that the polyunsaturated fatty acids such as DHA are edible oils.What prior art added in edible oil that the method for polyunsaturated fatty acid generally adopts is the method that external source is added, and the method complex operation, therefore needs to find a kind of method easy and simple to handle.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of one-step method to prepare the method being rich in the vegetable oil of DHA.
A method for the vegetable oil of DHA is rich in one-step method preparation, it is characterized in that, mainly comprises following step:
(1) micro-algae of being rich in DHA is collected;
(2) micro-algae step (1) obtained is dried to constant weight, obtains micro-algae powder, then is pulverized by micro-algae powder;
(3) the micro-algae powder after pulverizing step (2) obtained crosses 40 mesh sieves;
(4) the algae powder that step (3) obtains is mixed according to mass ratio 1:1 ~ 2 with vegetable oil, obtain the mixture of algae powder and vegetable oil;
(5) mixture obtained in step (4) is carried out immersion treatment;
(6) after step (5) has been soaked, mixture has been dropped in supercritical extracting equipment, control temperature 40 ~ 60 DEG C, be preferably 50 DEG C; Pressure 20 ~ 30MPa, is preferably 28MPa; Carbon dioxide flow 5-15L/h, extraction 120 ~ 300min, is preferably 180min;
(7) step (6) carries out decompression separation after having extracted, control temperature 35-65 DEG C, and be preferably 55 DEG C, one-level separating pressure is 8-10MPa, and the second-order separation pressure is 4-8MPa, obtains one-level algae oil and algae-residue;
(8) algae-residue obtained in step (7) is pulverized again, mix with vegetable oil mass ratio 1:1 ~ 2 according to algae-residue, repeat step (5) ~ (7) once, obtain secondary algae oil, the one-level algae oil itself and step (7) obtained mixes, and namely obtains the vegetable oil raw materials being rich in DHA.
Wherein, described micro-algae of being rich in DHA is for splitting kettle algae.
Wherein, described vegetable oil is any one or a few the mixture in rapeseed oil, corn oil, olive oil, peanut oil, sesame oil, soybean oil, sunflower oil, preferred soybean oil, sesame oil.
Wherein, the bake out temperature described in step (2) is 60 DEG C.
Wherein, described soaking conditions is 40 ~ 55 DEG C, preferably 50 DEG C; Soak 20 ~ 40min, preferred 30min.
The vegetable oil containing DHA that the above-mentioned preparation method being rich in the vegetable oil raw materials of DHA prepares is also within protection scope of the present invention.There are some researches show that the grease in micro-algae is harmless, therefore have also been developed the products such as micro-algae chewable tablets in the market, the preparation-obtained vegetable oil being rich in DHA of the present invention, its DHA content is more than 10%, and its DHA content of DHA edible oil that contains that market is sold is only 1-2%, the vegetable oil that therefore the present invention prepares has broad application prospects.
Beneficial effect:
The present invention has following distinguishing feature and effect:
(1) the present invention adds vegetable oil when extracting the DHA splitting in kettle algae grease, improves to split DHA extraction efficiency in kettle algae grease and provide a new thinking for using supercritical carbon dioxide extraction method.
(2) prior art uses more employing to add the organic solvents such as methyl alcohol, ethanol, acetone, propane, organic solvent extraction is utilized to carry out solvent removal, the energy that this process need consumption is a large amount of, the present invention adopts vegetable oil to add in extraction kettle, not only significantly improved and to have split in kettle algae grease DHA extraction efficiency but also eliminate the process that the later stage removes organic solvent simultaneously, achieved the effective new method of one splitting DHA in kettle algae grease with vegetable oil extracting directly.
(3) in the vegetable oil for preparing of the present invention, DHA content is high, has broad application prospects.
Accompanying drawing explanation
Fig. 1 in supercritical extract, when vegetable oil and dry algae powder add according to different proportion, the extraction efficiency of DHA.Wherein, abscissa is vegetable oil and algae powder dry ratio, represents with percentage; Ordinate is DHA extraction efficiency, represents with percentage.Data are the mean value of 3 parallel samplings.
Detailed description of the invention
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Extraction equipment used in following examples is provided by Huaan, Nantong, Jiangsu Province supercritical extract Co., Ltd, and model is HA120-50-01.
In following examples, algae oil detects as follows:
Step one: algae oil esterification.
Get the algae oil that 20mg obtains and add CHCl
3dissolve, proceed in 1.5ml Agilent vial, add the methanolic solution of 1ml1M, fill N
2sealing, in 100 DEG C of reaction 1h, naturally cools, adds 200 μ L deionized waters, mixing, and with 200 μ L n-hexane extraction 3 times, merging organic phase, with 200 μ L deionized water reextraction washing 3 times, gets organic phase, proceed in 1.5ml Agillient vial, N
2dry up, weigh.
Step 2: fatty acid methyl ester quantitative analysis.
The 7890 type gas chromatographs (GC) adopting Agilent company to produce carry out quantitative analysis to the fatty acid methyl ester in microalgae grease after esterification.
Analysis condition: the 7890 type gas chromatographs (GC) adopting Agilent company to produce carry out quantitative analysis to the fatty acid methyl ester in microalgae grease after esterification.DB-WAX capillary chromatographic column (30m × 0.32mm × 0.50 μm).Post heating schedule: rise to 200 DEG C from 50 DEG C, keeps 5min; Then rise to 250 DEG C with 10 DEG C/min, keep 10min.Carrier gas: nitrogen; Flow: 3ml/min.Detector: hydrogen flame detector, hydrogen: 30ml/min; Air: 300ml/min.Injector temperature: 280 DEG C; Detector temperature 300 DEG C.
Embodiment 1:
Split kettle algae dry algae powder from rapeseed oil according to the impact of different mass ratios for DHA extraction efficiency to investigate, kettle algae dry algae powder is split in setting and rapeseed oil mass ratio is 1:1,2:1.
Collect and culturedly split kettle algae, kettle algae powder will be split and dry, and after pulverizing, cross 40 mesh sieves.Take 30g algae powder powder, add respectively with algae powder powder quality than the ethanol of 95% (v/v) for 1:1 and with algae powder powder quality than being the rapeseed oil of 1:1 and 1:2, mix, drop in extraction kettle, extraction temperature rises to 50 DEG C, at this temperature static immersing 30min.Soak complete after be 50 DEG C in extraction temperature, extracting pressure is carry out dynamic extraction under 28MPa, and extraction time is 180min.Collect first time extraction gained algae oil.
Gained is split kettle algae algae-residue again to pulverize, add respectively with algae powder powder quality than for 1:1 95% ethanol and with algae powder powder quality than being the rapeseed oil of 1:1 and 1:2, mix, drop in extraction kettle, repeat and carry out single extraction.Collect second time extraction gained algae oil, itself and first time are extracted gained algae oil and mixes, namely obtain the vegetable oil raw materials being rich in DHA, adopt said method to analyze the component of algae oil.
The quality of DHA in gained algae oil is calculated according to formula (1):
M
dHA=m
algae oil× A
dH... ... ... .... (1).
M in formula (1)
algae oilrepresent the quality of algae oil that extraction 1 or extraction 2 obtain, A
dHArepresent the ratio of TFA shared by DHA in gas chromatographic analysis result.
Table 1 rapeseed oil counterincision kettle algae DHA extraction efficiency
As known from Table 1, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of rapeseed oil gained to be 6.34g and 7.09g, be 3.12 times when not using polar solvent and 3.46 times respectively.
Embodiment 2:
To carry out to the similar method of embodiment 1, except the polar solvent added be replaced by corn oil, olive oil, peanut oil, sesame oil, soybean oil, sunflower seeds wet goods any one.Split kettle algae DHA extraction efficiency to be shown in Table 2.
The different vegetable oil of table 2 is to the extraction effect of DHA
Embodiment 3:
To carry out to the similar method of embodiment 1, be replaced by corn oil except adding polar solvent.Split kettle algae DHA extraction efficiency to be shown in Table 3.
The impact of table 3 corn oil counterincision kettle algae DHA extraction efficiency
As known from Table 3, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of corn oil gained to be 6.88g, be 3.37 times when not using polar solvent.Corn oil gained DHA quality is used to be 1.12 times that use ethanol.
Embodiment 4:
To carry out to the similar method of embodiment 1, except the polar solvent added is replaced by olive oil.Split kettle algae DHA extraction efficiency to be shown in Table 4.
The impact of table 4 olive oil counterincision kettle algae DHA extraction efficiency
As known from Table 4, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of olive oil gained to be 6.21g, be 3.04 times when not using polar solvent.Olive oil gained DHA quality is used to be 1.01 times that use ethanol.
Embodiment 5
To carry out to the similar method of embodiment 1, except the polar solvent added is replaced by peanut oil.Split kettle algae DHA extraction efficiency to be shown in Table 5.
The impact of table 5 peanut oil counterincision kettle algae DHA extraction efficiency
As known from Table 5, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of peanut oil gained to be 6.27g, be 3.04 times when not using polar solvent.Peanut oil gained DHA quality is used to be 1.02 times that use ethanol.
Embodiment 6
To carry out to the similar method of embodiment 1, except the polar solvent added is replaced by sesame oil.Split kettle algae DHA extraction efficiency to be shown in Table 6.
The impact of table 6 sesame oil counterincision kettle algae DHA extraction efficiency
As known from Table 6, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of sesame oil gained to be 7.55g, be 3.70 times when not using polar solvent.Sesame oil gained DHA quality is used to be 1.23 times that use ethanol.
Embodiment 7
To carry out to the similar method of embodiment 1, except the polar solvent added is replaced by soybean oil.Split kettle algae DHA extraction efficiency to be shown in Table 7.
The impact of table 7 soybean oil counterincision kettle algae DHA extraction efficiency
As known from Table 7, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of soybean oil gained to be 7.16g, be 3.51 times when not using polar solvent.Soybean oil gained DHA quality is used to be 1.17 times that use ethanol.
Embodiment 8
To carry out to the similar method of embodiment 1, except the polar solvent added is replaced by sunflower oil.Split kettle algae DHA extraction efficiency to be shown in Table 8.
The impact of table 8 sunflower oil counterincision kettle algae DHA extraction efficiency
As known from Table 8, when not using polar solvent, 30g splits in kettle algae powder powder to extract and obtains 2.04g DHA, the quality using the DHA of ethanol gained is 6.14g, 3.01 times when not using polar solvent, and use the DHA quality of sunflower oil gained to be 6.49g, be 3.18 times when not using polar solvent.Sunflower oil gained DHA quality is used to be 1.06 times that use ethanol.
Claims (6)
1. a method for the vegetable oil of DHA is rich in one-step method preparation, it is characterized in that, mainly comprises following step:
(1) micro-algae of being rich in DHA is collected;
(2) micro-algae step (1) obtained is dried to constant weight, obtains micro-algae powder, then is pulverized by micro-algae powder;
(3) the micro-algae powder after pulverizing step (2) obtained crosses 40 mesh sieves;
(4) the algae powder that step (3) obtains is mixed according to mass ratio 1:1 ~ 2 with vegetable oil, obtain the mixture of algae powder and vegetable oil;
(5) mixture obtained in step (4) is carried out immersion treatment;
(6) after step (5) has been soaked, mixture has been dropped in supercritical extracting equipment, control temperature 40 ~ 60 DEG C, pressure 20 ~ 30MPa, carbon dioxide flow 5-15L/h, extraction 120 ~ 300min;
(7) step (6) carries out decompression separation after having extracted, control temperature 35-65 DEG C, and one-level separating pressure is 8-10MPa, and the second-order separation pressure is 4-8MPa, obtains one-level algae oil and algae-residue;
(8) algae-residue obtained in step (7) is pulverized again, mix with vegetable oil mass ratio 1:1 ~ 2 according to algae-residue, repeat step (5) ~ (7) once, obtain secondary algae oil, the one-level algae oil itself and step (7) obtained mixes, and namely obtains the vegetable oil being rich in DHA.
2. the method for the vegetable oil of DHA is rich in one-step method preparation according to claim 1, and it is characterized in that, described micro-algae of being rich in DHA is for splitting kettle algae.
3. the method for the vegetable oil of DHA is rich in one-step method preparation according to claim 1, it is characterized in that, described vegetable oil is any one or a few the mixture in rapeseed oil, corn oil, olive oil, peanut oil, sesame oil, soybean oil, sunflower oil.
4. the method for the vegetable oil of DHA is rich in one-step method preparation according to claim 1, and it is characterized in that, the bake out temperature described in step (2) is 60 DEG C.
5. the method for the vegetable oil of DHA is rich in one-step method preparation according to claim 1, and it is characterized in that, described soaking conditions is 40 ~ 55 DEG C, soaks 20 ~ 40min.
6. the vegetable oil containing DHA that the method that the vegetable oil of DHA is rich in the one-step method preparation according to any one of Claims 1 to 5 prepares.
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Application publication date: 20141217 |