CN111214846B - Haematococcus pluvialis extract and preparation method thereof - Google Patents
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Abstract
The invention relates to a haematococcus pluvialis extract and a preparation method thereof, wherein haematococcus pluvialis powder is mixed with a subcritical extraction solvent and then subjected to continuous subcritical extraction, a haematococcus pluvialis subcritical extract is obtained after extraction is finished, the subcritical extract is collected, and continuous supercritical carbon dioxide extraction treatment is carried out to remove residual solvent in the extract, so that a haematococcus pluvialis extract is obtained; it is also possible to carry out thin film evaporation after supercritical desolvation in order to further desolvation. The method has the advantages of low equipment price, simple and convenient operation, complete removal of residual solvent and high yield, and is suitable for large-scale production of haematococcus pluvialis extract; the temperature and pressure of the continuous supercritical desolventizing are relatively low, the effective components in the extract are not easy to damage, and the solvent is completely removed, so that the astaxanthin content in the haematococcus pluvialis extract is more than 8 wt%, and the butane residue is less than 1 ppm.
Description
Technical Field
The invention relates to the technical field of preparation of haematococcus pluvialis extracts, and particularly relates to a haematococcus pluvialis extract and a preparation method thereof.
Background
Haematococcus pluvialis is a unicellular green alga which accumulates a large amount of astaxanthin under adverse conditions and is recognized as a major source of astaxanthin in nature. By supercritical fluid CO2The haematococcus pluvialis extract of the technology contains vitamin B besides natural antioxidant astaxanthin1、B2、B6、B12And monounsaturated fatty acids, unsaturated fatty acids, and other nutritional components essential to the human body.
The extraction method of haematococcus pluvialis includes a solvent method, a supercritical method, a microwave method, an ultrasonic method and the like, and the microwave method and the ultrasonic method are rarely used for large-scale production. The astaxanthin oil is a main functional substance in haematococcus pluvialis, has strong oxidation resistance and is unstable to light, heat, oxygen and humidity, so the process for extracting fat-soluble components by adopting a solvent method is easy to cause oxidative deterioration and has solvent residues. Chinese patent 201010548322.1 discloses a haematococcus pluvialis extract preparation, its preparation method and use, the astaxanthin ingredient in haematococcus pluvialis is extracted by using supercritical extraction technology, but because the supercritical extraction technology needs to be carried out under high pressure, the equipment requirement is high, the extraction equipment is expensive, and the large-scale production cost is high.
The subcritical extraction technology is an extraction technology which takes subcritical fluid or mixed solution thereof as a solvent, and extracts a target component from a natural product sequentially through the processes of leaching, evaporation desolventizing, compression, condensation recovery and the like with a solute in a system at room temperature and a certain pressure. Compared with supercritical extraction, subcritical extraction has the advantages of cheap equipment, large yield, easy operation and the like. At present, the method is widely applied to the fields of edible oil extraction, degreasing, plant pigment extraction and the like in the food industry of China. Subcritical fluids refer to substances in which certain compounds exist as fluids at temperatures above their boiling points but below their critical temperatures and at pressures below their critical pressures. Butane is one of the more common subcritical extraction fluids. The oil and fat processing agent is brought into the food processing agent catalogue by the Ministry of health in China and can be used for the oil and fat processing technology. But the production process can not avoid partial butane residue, the butane can not be metabolized in human body, and high concentration of butane has toxicity to human nervous system. Thus, the residual solvent in the product extracted with subcritical butane is a not negligible food safety issue. However, at present, the residual quantity of butane in the subcritical butane-extracted grease has no unified national standard. Enterprises need to strictly control the residual quantity of butane in products in the production process, and the method is an important guarantee for the safety of the products.
Disclosure of Invention
In order to solve the technical problems of high production cost of supercritical extraction of haematococcus pluvialis and large solvent residue after the haematococcus pluvialis is not suitable for solvent method treatment or solvent method treatment, a preparation method for extracting a haematococcus pluvialis extract by using a subcritical butane extraction technology and subsequently removing a residual solvent is provided. The method has the advantages of low equipment price, simple and convenient operation, complete removal of residual solvent and high yield, and is suitable for large-scale production of haematococcus pluvialis extract.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) mixing haematococcus pluvialis powder with a subcritical extraction solvent, carrying out continuous subcritical extraction, obtaining a haematococcus pluvialis subcritical extract after extraction is finished, and collecting the subcritical extract;
(2) and carrying out continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract to obtain haematococcus pluvialis extract.
Further, the subcritical extraction solvent is butane; the mass volume ratio of the haematococcus pluvialis powder to the subcritical extraction solvent is 1kg (4-8) L. Preferably, the mass volume ratio of the haematococcus pluvialis powder to the extraction solvent is 1kg: 5L.
Further, the continuous subcritical extraction process comprises the following steps: and (2) adopting a subcritical fluid extraction device, continuously extracting at the extraction pressure of 8-12 MPa, the extraction temperature of 30-60 ℃ and the separation temperature of 25-40 ℃, wherein the extraction frequency is 3-6 times, and the extraction time is 1-2 h each time, and collecting the extract obtained by each extraction.
Preferably, the process of continuous subcritical extraction is: the continuous extraction is carried out under the extraction pressure of 10MPa, the extraction temperature of 50 ℃ and the separation temperature of 30 ℃, the extraction times are 4 times, and the extraction time is 1.5h each time.
Further, the process of the continuous supercritical carbon dioxide extraction treatment comprises the following steps:
firstly, in a supercritical extraction device, the flow velocity of carbon dioxide is 0.4cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 20min to 60min under the conditions of/s to 0.8, the extraction pressure of 15MPa to 25 and the extraction temperature of 60 ℃ to 80 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation conditions of the separation kettle I are that the temperature is 50-60 ℃ and the pressure is 7-8 MPa, the separation conditions of the separation kettle II are that the temperature is 30-50 ℃ and the pressure is 3-4 MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 2-5 times according to the first step and the second step, recovering carbon dioxide and subcritical extraction solvent separated each time, and purifying for reuse.
Preferably, the supercritical carbon dioxide extraction conditions in step (i) are as follows: carbon dioxide flow rate 0.6cm3The extraction pressure is 20MPa, the extraction temperature is 70 ℃, and the extraction time is 30 min; the separation conditions of the separation kettle I are 55 ℃ and 7.5Mpa, and the separation conditions of the separation kettle II are 40 ℃ and 3.5 Mpa; and step three, the repeated treatment is carried out for 3 times.
Further, the preparation method also comprises a thin film evaporation treatment after the supercritical carbon dioxide extraction treatment to further remove the residual solvent.
Further, the conditions of the thin film evaporation treatment are as follows: treating at 70-90 ℃ for 2-5 s.
Preferably, the conditions of the thin film evaporation treatment are as follows: the treatment was carried out at 80 ℃ for 3 s.
In another aspect, the present invention provides a haematococcus pluvialis extract having an astaxanthin content of >8 wt% and a butane residue of < 1ppm, obtainable by the above preparation method.
The beneficial technical effects are as follows: the invention adopts the subcritical butane extraction technology to extract fat-soluble substances in haematococcus pluvialis powder, the obtained extract is in a grease shape and has higher viscosity, and after the butane solvent is separated from the extract after the subcritical butane extraction of the extract, a large amount of solvent residues still exist in the obtained haematococcus pluvialis extract. In order to improve the safety of products and solve the problem of a large amount of residual solvent in haematococcus pluvialis extract produced by subcritical butane extraction, the invention adopts a supercritical carbon dioxide extraction technology to remove the residual solvent from the haematococcus pluvialis extract, after carbon dioxide is in a liquid state and is mixed with the subcritical extract under a supercritical state, the carbon dioxide, the residual solvent butane and fat-soluble components in the haematococcus pluvialis are all non-polar substances, based on a similar compatibility principle, the residual solvent butane and the fat-soluble components are carried out by the carbon dioxide supercritical fluid, and the carbon dioxide and the residual solvent butane are separated out by cooling and decompressing in 2 separation kettles, so that the haematococcus pluvialis extract is finally prepared. The temperature and pressure of the supercritical desolventizing agent are relatively low, so that the effective components in the extract are not easy to damage; the impurities and the solvent in the extract can be further removed by re-extraction, so that the content of the astaxanthin in the extract is increased; and the solvent is removed completely, so that the butane residue in the haematococcus pluvialis extract is less than 1 ppm; in order to further remove the residual solvent, after the subcritical extraction and the supercritical desolventization, the residual solvent can be removed by thin film evaporation, so that the solvent residue in the haematococcus pluvialis extract is less than 0.5 ppm.
Detailed Description
The invention is further described below with reference to specific examples, but without limiting the scope of the invention.
Example 1
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 4L of butane, then carrying out continuous subcritical butane extraction, carrying out continuous extraction at the extraction pressure of 8MPa, the extraction temperature of 30 ℃ and the separation temperature of 25 ℃, carrying out extraction for 3 times, wherein the extraction time is 1h each time, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment to perform continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract, wherein the continuous supercritical carbon dioxide extraction treatment process comprises the following steps:
first, the flow rate of carbon dioxide is 0.4cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 20min under the conditions of extraction pressure of 15MPa and extraction temperature of 60 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation conditions of the separation kettle I are that the temperature is 50 ℃ and the pressure is 7MPa, and the separation conditions of the separation kettle II are that the temperature is 30 ℃ and the pressure is 3MPa, so that the haematococcus pluvialis supercritical extract is obtained;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 2 times according to the first step and the second step to finally obtain the haematococcus pluvialis extract, recovering carbon dioxide and subcritical extraction solvent separated each time, and reusing the haematococcus pluvialis extract after purification.
Example 2
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 8L of butane, performing continuous subcritical butane extraction, performing continuous extraction at an extraction pressure of 12MPa, an extraction temperature of 60 ℃ and a separation temperature of 40 ℃, wherein the extraction frequency is 6 times, each extraction time is 2 hours, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) the process of performing continuous supercritical carbon dioxide extraction treatment on the extract by adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment comprises the following steps:
firstly, the flow velocity of carbon dioxide is 0.8cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 60min under the conditions of extraction pressure of 25MPa and extraction temperature of 80 ℃;
secondly, separating supercritical fluid carbon dioxide through a separation kettle I, and separating out a subcritical extraction solvent remained in the haematococcus pluvialis extract through a separation kettle II, wherein the separation condition of the separation kettle I is that the temperature is 60 ℃ and the pressure is 8MPa, and the separation condition of the separation kettle II is that the temperature is 50 ℃ and the pressure is 4MPa, so that the haematococcus pluvialis supercritical extract is obtained;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 5 times according to the first step and the second step to finally obtain the haematococcus pluvialis extract, recovering carbon dioxide and subcritical extraction solvent separated each time, and reusing the haematococcus pluvialis extract after purification.
Example 3
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 5L of butane, performing continuous subcritical butane extraction, performing continuous extraction at an extraction pressure of 10MPa, an extraction temperature of 50 ℃ and a separation temperature of 30 ℃, wherein the extraction time is 4 times, each extraction time is 1.5 hours, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment to perform continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract, wherein the continuous supercritical carbon dioxide extraction treatment process comprises the following steps:
first, the flow rate of carbon dioxide is 0.6cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 30min under the conditions of extraction pressure of 20MPa and extraction temperature of 70 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation condition of the separation kettle I is that the temperature is 55 ℃ and the pressure is 7.5MPa, and the separation condition of the separation kettle II is that the temperature is 40 ℃ and the pressure is 3.5MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 3 times according to the first step and the second step to finally obtain the haematococcus pluvialis extract, recovering carbon dioxide and subcritical extraction solvent separated each time, and reusing the haematococcus pluvialis extract after purification.
Example 4
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 5L of butane, performing continuous subcritical butane extraction, performing continuous extraction at an extraction pressure of 10MPa, an extraction temperature of 50 ℃ and a separation temperature of 30 ℃, wherein the extraction time is 4 times, each extraction time is 1.5 hours, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment to perform continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract, wherein the continuous supercritical carbon dioxide extraction treatment process comprises the following steps:
first, the flow rate of carbon dioxide is 0.6cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 30min under the conditions of extraction pressure of 20MPa and extraction temperature of 70 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation condition of the separation kettle I is that the temperature is 55 ℃ and the pressure is 7.5MPa, and the separation condition of the separation kettle II is that the temperature is 40 ℃ and the pressure is 3.5MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 3 times according to the first step and the second step, recovering carbon dioxide and subcritical extraction solvent separated each time, and purifying and reusing the extract;
(3) performing thin film evaporation treatment on the haematococcus pluvialis supercritical extract in the step (2) at the temperature of 70 ℃ for 2s to further remove residual solvent to finally obtain the haematococcus pluvialis extract,
example 5
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 5L of butane, performing continuous subcritical butane extraction, performing continuous extraction at an extraction pressure of 10MPa, an extraction temperature of 50 ℃ and a separation temperature of 30 ℃, extracting for 4 times, wherein the extraction time of each time is 1.5h, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment to perform continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract, wherein the continuous supercritical carbon dioxide extraction treatment process comprises the following steps:
firstly, the flow velocity of carbon dioxide is 0.6cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 30min under the conditions of extraction pressure of 20MPa and extraction temperature of 70 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation condition of the separation kettle I is that the temperature is 55 ℃ and the pressure is 7.5MPa, and the separation condition of the separation kettle II is that the temperature is 40 ℃ and the pressure is 3.5MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 3 times according to the first step and the second step to recover carbon dioxide and subcritical extraction solvent separated each time, and purifying and reusing the carbon dioxide and subcritical extraction solvent;
(3) and (3) performing thin-film evaporation treatment on the haematococcus pluvialis supercritical extract in the step (2) at the temperature of 90 ℃ for 5s to further remove residual solvent, and finally obtaining the haematococcus pluvialis extract.
Example 6
A preparation method of Haematococcus pluvialis extract comprises the following steps:
(1) extracting by using a CBE-150L X2 subcritical fluid extraction device, mixing 1kg of haematococcus pluvialis powder with 5L of butane, performing continuous subcritical butane extraction, performing continuous extraction at an extraction pressure of 10MPa, an extraction temperature of 50 ℃ and a separation temperature of 30 ℃, wherein the extraction time is 4 times, each extraction time is 1.5 hours, collecting the haematococcus pluvialis subcritical extract obtained by each extraction after the extraction is finished, and recovering the butane;
(2) adopting 2 x 5+1L/60MPa-IIA type supercritical extraction equipment to perform continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract, wherein the continuous supercritical carbon dioxide extraction treatment process comprises the following steps:
first, the flow rate of carbon dioxide is 0.6cm3S, extraction pressurePerforming supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 30min under the conditions of 20MPa and the extraction temperature of 70 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation condition of the separation kettle I is that the temperature is 55 ℃ and the pressure is 7.5MPa, and the separation condition of the separation kettle II is that the temperature is 40 ℃ and the pressure is 3.5MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 3 times according to the first step and the second step to recover carbon dioxide and subcritical extraction solvent separated each time, and purifying and reusing the carbon dioxide and subcritical extraction solvent;
(3) and (3) performing thin-film evaporation treatment on the haematococcus pluvialis supercritical extract in the step (2) at the temperature of 80 ℃ for 3s to further remove residual solvent, and finally obtaining the haematococcus pluvialis extract.
Comparative example 1
This comparative example is the same as the process of example 3, except only a subcritical butane extraction was performed.
Comparative example 2
This comparative example is the same as example 4, except that step (2) and step (3) are exchanged, i.e., the technical solution of this comparative example is to perform subcritical butane extraction first, perform thin film evaporation to remove the solvent, and finally perform supercritical carbon dioxide to further remove the solvent.
The product yield of the haematococcus pluvialis fat-soluble extract prepared by the method is calculated, and the residual quantity of butane (including n-butane and isobutane) in the product and the astaxanthin content in the product are detected by adopting a headspace gas chromatography (the content of all-trans astaxanthin is determined according to a determination method of Chinese patent 201110437754. X), and the specific data are shown in table 1.
TABLE 1 indices of Haematococcus pluvialis oil in examples and comparative examples
As can be seen from Table 1, in comparative example 1, after only subcritical butane extraction, the butane residue was 425.07mg/kg, the astaxanthin content was 6.83%, and the solvent residue was high, in example 3, after subcritical butane extraction, continuous supercritical carbon dioxide desolvation was performed, so that the butane residue in the Haematococcus pluvialis extract was 0.51mg/kg, that is, the butane residue was less than 1ppm, it can be seen that supercritical carbon dioxide has a very significant solvent removal effect, and the solvent removal was complete, and in addition, continuous supercritical carbon dioxide desolvation was performed, the astaxanthin content in the extract can be effectively increased, and the increase of the astaxanthin content was at least 25.9%; in order to further remove the residual solvent, after the subcritical extraction and the supercritical desolventization, the membrane evaporation is further performed in examples 4 to 6 to remove the residual solvent, so that the residual solvent content in the haematococcus pluvialis extract is 0.08mg/kg to 0.35mg/kg, namely the residual butane content is less than 0.5ppm, but the astaxanthin content in the extract is slightly reduced due to the higher temperature during the membrane evaporation.
Claims (6)
1. A preparation method of haematococcus pluvialis extract is characterized by comprising the following steps:
(1) mixing haematococcus pluvialis powder with a subcritical extraction solvent, carrying out continuous subcritical extraction, obtaining a haematococcus pluvialis subcritical extract after extraction is finished, and collecting the subcritical extract;
the continuous subcritical extraction process comprises the following steps: adopting a subcritical fluid extraction device to perform continuous extraction at an extraction pressure of 8 MPa-12 MPa, an extraction temperature of 30-60 ℃ and a separation temperature of 25-40 ℃, wherein the extraction frequency is 3-6 times, and the extraction time is 1-2 h each time, and collecting the extract obtained by each extraction;
(2) carrying out continuous supercritical carbon dioxide extraction treatment on the subcritical extract to remove residual solvent in the extract to obtain haematococcus pluvialis extract;
the process of the continuous supercritical carbon dioxide extraction treatment comprises the following steps:
in supercritical extraction equipment, the flow rate of carbon dioxide is 0.4cm3/s～0.8cm3Performing supercritical carbon dioxide extraction on the haematococcus pluvialis extract for 20-60 min under the conditions of extraction pressure of 15-25 MPa and extraction temperature of 60-80 ℃;
secondly, separating out supercritical fluid carbon dioxide through a separation kettle I, and separating out the residual subcritical extraction solvent in the haematococcus pluvialis extract through a separation kettle II, wherein the separation conditions of the separation kettle I are that the temperature is 50-60 ℃ and the pressure is 7-8 MPa, the separation conditions of the separation kettle II are that the temperature is 30-50 ℃ and the pressure is 3-4 MPa, so as to obtain the haematococcus pluvialis supercritical extract;
thirdly, continuously and repeatedly treating the haematococcus pluvialis supercritical extract for 2-5 times according to the first step and the second step, recovering carbon dioxide and a subcritical extraction solvent separated each time, and purifying for reuse;
further comprising performing thin film evaporation treatment after the supercritical carbon dioxide extraction treatment, wherein the conditions of the thin film evaporation treatment are as follows: treating at 70-90 deg.c for 2-5 sec.
2. The method of claim 1, wherein the subcritical extraction solvent is butane; the mass volume ratio of the haematococcus pluvialis powder to the subcritical extraction solvent is 1kg (4-8) L.
3. The method of claim 1, wherein the continuous subcritical extraction comprises: the continuous extraction is carried out under the extraction pressure of 10MPa, the extraction temperature of 50 ℃ and the separation temperature of 30 ℃, the extraction times are 4 times, and the extraction time is 1.5h each time.
4. The method for preparing Haematococcus pluvialis extract according to claim 1, wherein the supercritical carbon dioxide extraction conditions of step (i) are as follows: carbon dioxide flow rate 0.6cm3The extraction pressure is 20MPa, the extraction temperature is 70 ℃, and the extraction time is 30 min; the separation condition of the separation kettle I is that the temperature is 55 ℃ and the pressure is 7.5Mpa,the separation condition of the separation kettle II is that the temperature is 40 ℃ and the pressure is 3.5 Mpa; step (ii) of
And the repeated treatment is carried out for 3 times.
5. The method of claim 1, wherein the conditions of the thin film evaporation treatment are as follows: the conditions of the film evaporation treatment are as follows: the treatment was carried out at 80 ℃ for 3 s.
6. A Haematococcus pluvialis extract prepared by the method of any one of claims 1-5, wherein the extract has an astaxanthin content of >8 wt% and a butane residue of < 0.5 ppm.
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