CN110923053A - Method for extracting tea oil with high freezing resistance - Google Patents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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- C11B1/04—Pretreatment of vegetable raw material
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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Abstract
The invention relates to the technical field of tea oil extraction, in particular to a method for extracting tea oil with high freezing resistance, which comprises the following steps: (1) activating camellia seeds; (2) performing water enzyme treatment; (3) slurry blasting; (4) preparation of crude oil; (5) performing supercritical extraction; the tea oil obtained by the method has the advantages of good quality, good quality stability and frost resistance, and contains abundant nutrient components such as vitamin E and vitamin B.
Description
Technical Field
The invention relates to the technical field of tea oil extraction, in particular to a method for extracting tea oil with high freezing resistance.
Background
The tea oil is a vegetable oil obtained by processing and refining camellia seeds, the content of unsaturated fatty acid in the tea oil is more than 80%, the fatty acid composition is similar to that of olive oil and is known as 'eastern olive oil', the tea oil is natural and mild, has strong permeability and is not easy to oxidize and deteriorate, and has the effects of preventing cardiovascular diseases, resisting tumors, protecting liver, cooling blood, resisting oxidation, regulating immunity, delaying organism aging and removing wrinkles and ageing.
The crude oil of the camellia seeds is dark in color and has astringent bitter taste, which is related to the fact that the oil contains a small amount of tea saponin and other impurities, and the crude oil is high in acid value, so the crude oil is applicable to various industries such as food, cosmetics and medicines only through refining processing, but the refined tea oil is low in freezing resistance, precipitates, turbidity and even freezing of the tea oil can occur below zero, the quality of the tea oil is not ideal, and the popularization and the application of the tea oil are not facilitated.
Patent No. CN201110247402.8 discloses an efficient method for producing high-quality antifreeze tea oil, the key of the scheme is that saturated fat is added as a seed crystal in the crystallization process of tea oil to realize rapid crystallization, and the antifreeze tea oil is obtained after filtration and separation.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides an extraction method of tea oil with high freezing resistance, which comprises the following steps:
a method for extracting tea oil with high freezing resistance comprises the following steps:
(1) activation of camellia seeds: treating camellia seeds with the plant disinfectant for 10-20s in a constant-voltage electric field with the voltage of 1-3V, wherein the mass ratio of the camellia seeds to the plant disinfectant is 1: (3-7), adding a crystal modifier with the mass of 1-5 per mill of the plant disinfectant, raising the voltage, treating for 10-20s under the condition of 15-20V, taking out camellia seeds, and draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: (1.5-2), treating for 20-30min at 30-35 ℃, and taking out the camellia seeds for enzymolysis;
(3) slurry blasting: maintaining the enzymolysis camellia seed under 1-1.8MPa for 60-90s, and then performing slurry explosion to obtain slurry;
(4) crude oil preparation: sending the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2-2.5Pa, maintaining the pressure for 120-;
(5) supercritical extraction: and (4) feeding the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain the finished product of the tea oil.
The preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 40-50 deg.C for 10-20 min; treating folium Artemisiae Argyi in 150 deg.C steam at 130-; mixing the prepared quinoa shell powder and folium Artemisiae Argyi, adding purified water 20-30 times of the mixture, and extracting at 70-90 deg.C for 1-3 hr.
The crystal transformation agent comprises the following components in parts by weight: 2.3-2.9 parts of sodium citrate and 11-15 parts of betaine.
The enzymolysis liquid is prepared by mixing citric acid solution with mass concentration of 40-50% and soybean protein powder according to the mass ratio of 1 (0.2-0.6) to prepare soybean protein solution, then heating to 92-95 ℃, preserving heat for 10-15min, then cooling the swollen soybean protein solution to 15-20 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution for enzymolysis, and obtaining the enzymolysis liquid.
The mixing proportion of the soybean protein solution, β -mannase, xylanase, protease and water is that β -mannase 200-.
The enzymolysis increases the temperature from the cooled temperature to 27-35 ℃, after 30-40min of enzymolysis, increases the temperature to 42-46 ℃, carries out enzymolysis for 20-30min, and then reduces the temperature to 15-20 ℃ according to the speed of 1-3 ℃/min.
The heating rate is 1-2 ℃ rising every 3-5 min.
The modified sodium carboxymethylcellulose powder is prepared by mixing the following components in percentage by weight of 1: (0.3-1.7): (13-17) mixing for 10-15min at the temperature of 80-90 ℃, and then performing microwave treatment for 200-240s at the microwave frequency of 48-62MHz and the power of 500-800W.
The extraction adopts a continuous pressurization mode, takes 4-5MPa as initial pressure, increases the pressure to 11-12MPa at the speed of 0.1-0.3MPa/min, and then maintains the pressure for 20-25 min.
Compared with the prior art, the invention has the following beneficial effects:
the tea oil obtained by the application has good quality, good quality stability and frost resistance, contains abundant nutrient components such as vitamin E and vitamin B, and the applicant detects the vitamin E and the vitamin B according to the traditional high-efficiency chromatography and discovers that: compared with the tea oil sold in the market, the content of the vitamin E and the content of the vitamin B in the tea oil obtained by the method are respectively 5-8% and 3-4%.
The application utilizes vegetal disinfectant and voltage treatment, kills microorganisms of camellia seeds, prevents decomposition and conversion of effective components, utilizes quinoa wheat husks and folium artemisiae argyi as the disinfectant, has the functions of bacteriostasis and sterilization, has abundant nutrient substances, can enable the effective components such as vitamin B and polysaccharide to have magnetism through the voltage treatment, can form viscosity with fatty substances after adding the crystal modifier, and can enable the components to permeate the camellia seeds under the treatment of 15-20V voltage.
According to the method, β -mannase, xylanase and protease are used for degrading soybean protein powder, so that an enzyme system is enriched, the activated camellia seed is high in cell membrane permeability and beneficial to oil production, an organic calcium source is released, oil and fat components in the activated camellia seed can permeate into the activated camellia seed to be combined, and the freezing resistance of the tea oil is improved.
The method effectively reduces the oxygen content and the water content by filling the inert gas, thereby preventing the generation of trans-fatty acid; and then high-speed dispersion shearing is combined to effectively separate the grease, the grease in the emulsion layer is dissolved out by adding the modified sodium carboxymethyl cellulose into the emulsion layer, and the trehalose embedded in the pinonic acid modified sodium carboxymethyl cellulose is separated by utilizing the high frequency and the volatility of microwaves and is mutually combined with the grease components, and then the grease is separated by utilizing high-speed dispersion.
The application utilizes the extraction mode of continuous pressurization, has prevented the formation of trans fatty acid, makes components such as trehalose, organic calcium, vitamin can disperse in the tea-seed oil and disperse evenly simultaneously, has effectively improved the antioxidant property and the freezing resistance of tea-seed oil.
The application utilizes the effect of electric field heat on hydrogen bonds, hydrophobic bonds and van der waals force to redistribute the hydrogen bonds, thereby changing the internal structure of the camellia seeds, leading to cell rupture and being beneficial to subsequent blasting treatment. According to the application, the camellia seeds are subjected to pressure explosion, the biomembrane is damaged to the maximum extent in a short time, and the separation of grease from the lipid complex is facilitated.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
A method for extracting tea oil with high freezing resistance comprises the following steps:
(1) activation of camellia seeds: after camellia seeds are treated with the plant disinfectant for 20 seconds in a constant-voltage electric field with the voltage of 3V, the mass ratio of the camellia seeds to the plant disinfectant is 1: 7, adding a crystal transfer agent with the mass of 5 per mill of the plant disinfectant, raising the voltage, treating for 20s under the condition of 20V, taking out camellia seeds, draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: 2, treating for 30min at the temperature of 35 ℃, and taking out the camellia seeds for enzymolysis;
(3) slurry blasting: maintaining the enzymolyzed camellia seeds under the pressure of 1.8MPa for 90s, and then performing slurry blasting to obtain slurry;
(4) crude oil preparation: feeding the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2.5Pa, maintaining the pressure for 240s, shearing by using a high-speed disperser, performing centrifugal separation to obtain an oil layer, an emulsifying layer and residues, feeding the emulsifying layer into microwave treatment equipment, adding modified sodium carboxymethylcellulose powder with the mass of 0.5 per mill of the emulsifying layer, performing microwave treatment for 120s at the microwave frequency of 400MHz and the power of 400W, then placing the mixture into the high-speed disperser, shearing, performing centrifugal separation, and combining oil layers to obtain the crude tea oil;
(5) supercritical extraction: sending the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain finished tea oil;
the preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 50 deg.C for 20 min; treating folium Artemisiae Argyi in 150 deg.C steam for 15 min; mixing the prepared quinoa shell powder and folium artemisiae argyi, adding purified water with the mass being 30 times that of the mixture, and extracting for 3 hours at the temperature of 90 ℃;
the crystal transformation agent comprises the following components in parts by weight: 2.9 parts of sodium citrate and 15 parts of betaine;
mixing a citric acid solution with the mass concentration of 50% with soybean protein powder according to the mass ratio of 1: 0.6 to prepare a soybean protein solution, heating to 95 ℃, preserving heat for 15min, cooling the swollen soybean protein solution to 20 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution, and carrying out enzymolysis to obtain an enzymolysis solution;
the mixing proportion of the soybean protein solution, β -mannase, xylanase, protease and water is that each gram of soybean protein solution is added with β -mannase 300U, xylanase 400U, protease 3000U and water 300 mL;
the temperature is increased to 35 ℃ from the cooled temperature by the enzymolysis, the temperature is increased to 46 ℃ after the enzymolysis is carried out for 40min, the enzymolysis is carried out for 30min, and then the temperature is reduced to 20 ℃ according to the speed of 3 ℃/min;
the temperature rise rate is 2 ℃ rise every 5 min;
the modified sodium carboxymethylcellulose powder is prepared by mixing the following components in percentage by weight of 1: 1.7: 17, mixing for 15min at the temperature of 90 ℃, and then performing microwave treatment for 240s at the microwave frequency of 62MHz and the power of 800W;
the extraction adopts a continuous pressurization mode, takes 5MPa as initial pressure, increases the pressure to 12MPa at the speed of 0.3MPa/min, and then maintains the pressure for 25 min.
Example 2
A method for extracting tea oil with high freezing resistance comprises the following steps:
(1) activation of camellia seeds: after camellia seeds are treated by the plant disinfectant for 10 seconds in a constant-voltage electric field with the voltage of 1V, the mass ratio of the camellia seeds to the plant disinfectant is 1: 3, adding a crystal modifier with the mass of 1 per mill of the plant disinfectant, raising the voltage, treating for 10s under the condition of 15-20V, taking out camellia seeds, and draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: 1.5, treating at 30 deg.C for 20min, and taking out enzymolyzed camellia seed;
(3) slurry blasting: maintaining the enzymolysis camellia seeds under the pressure of 1MPa for 60s, and then performing slurry explosion to obtain slurry;
(4) crude oil preparation: feeding the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2Pa, maintaining the pressure for 120s, shearing by using a high-speed disperser, performing centrifugal separation to obtain an oil layer, an emulsifying layer and residues, feeding the emulsifying layer into microwave treatment equipment, adding modified sodium carboxymethylcellulose powder with the mass of 0.1 per mill of the emulsifying layer, performing microwave treatment for 60s at the microwave frequency of 300MHz and the power of 300W, placing the mixture into the high-speed disperser, shearing, performing centrifugal separation, and combining the oil layers to obtain the crude tea oil;
(5) supercritical extraction: sending the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain finished tea oil;
the preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 40 deg.C for 10 min; treating folium Artemisiae Argyi in 130 deg.C steam for 10 min; mixing the prepared quinoa shell powder and folium artemisiae argyi, adding purified water with the mass being 20 times that of the mixture, and extracting for 1h at the temperature of 70 ℃;
the crystal transformation agent comprises the following components in parts by weight: 2.3 parts of sodium citrate and 11 parts of betaine;
mixing citric acid solution with the mass concentration of 40% and soybean protein powder according to the mass ratio of 1: 0.2 to prepare soybean protein solution, heating to 92 ℃, preserving heat for 10min, cooling the swollen soybean protein solution to 15 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution, and carrying out enzymolysis to obtain enzymatic hydrolysate;
the mixing proportion of the soybean protein solution, β -mannase, xylanase, protease and water is that β -mannase 200U, xylanase 300U, protease 2000U and water 200mL are added into each gram of soybean protein solution;
the temperature is increased to 27 ℃ from the cooled temperature by the enzymolysis, the temperature is increased to 42 ℃ after the enzymolysis is carried out for 30min, the enzymolysis is carried out for 20-30min, and then the temperature is reduced to 15 ℃ according to the speed of 1 ℃/min;
the temperature rise rate is 1 ℃ rise every 3 min;
the modified sodium carboxymethylcellulose powder is prepared by mixing the following components in percentage by weight of 1: 0.3: 13, mixing for 10min at the temperature of 80 ℃, and then performing microwave treatment for 200s at the microwave frequency of 48MHz and the power of 500W;
the extraction adopts a continuous pressurization mode, takes 4MPa as initial pressure, increases the pressure to 11MPa at the speed of 0.1MPa/min, and then maintains the pressure for 20 min.
Example 3
A method for extracting tea oil with high freezing resistance comprises the following steps:
(1) activation of camellia seeds: after camellia seeds are treated by the plant disinfectant in a constant-voltage electric field with the voltage of 2V for 15s, the mass ratio of the camellia seeds to the plant disinfectant is 1: 5, adding a crystal transfer agent with the mass of 3 per mill of the plant disinfectant, raising the voltage, treating for 15s under the condition of 17V, taking out camellia seeds, and draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: 1.7, treating for 25min at 32 ℃, and taking out the camellia seeds subjected to enzymolysis;
(3) slurry blasting: maintaining the enzymolysis camellia seeds under the pressure of 1.5MPa for 75s, and then performing slurry explosion to obtain slurry;
(4) crude oil preparation: feeding the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2.2Pa, maintaining the pressure for 180s, shearing by using a high-speed disperser, performing centrifugal separation to obtain an oil layer, an emulsion layer and residues, feeding the emulsion layer into microwave treatment equipment, adding modified sodium carboxymethylcellulose powder with the mass of 0.3 per mill of the emulsion layer, performing microwave treatment for 90s at the microwave frequency of 350MHz and the power of 350W, then placing the mixture into the high-speed disperser, shearing, performing centrifugal separation, and combining oil layers to obtain the crude tea oil;
(5) supercritical extraction: sending the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain finished tea oil;
the preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 45 deg.C for 15 min; treating folium Artemisiae Argyi in 140 deg.C steam for 13 min; mixing the prepared quinoa shell powder and folium artemisiae argyi, adding purified water with the mass of 25 times of that of the mixture, and extracting for 2 hours at the temperature of 80 ℃;
the crystal transformation agent comprises the following components in parts by weight: 2.6 parts of sodium citrate and 13 parts of betaine;
mixing a citric acid solution with a mass concentration of 45% with soybean protein powder according to a mass ratio of 1: 0.4 to prepare a soybean protein solution, heating to 93 ℃, preserving heat for 12min, cooling the swollen soybean protein solution to 18 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution, and carrying out enzymolysis to obtain an enzymolysis solution;
the mixing proportion of the soybean protein solution, β -mannase, xylanase, protease and water is that β -mannase 250U, xylanase 350U, protease 2500U and water 250mL are added into each gram of the soybean protein solution;
the temperature is increased to 30 ℃ from the cooled temperature by the enzymolysis, the temperature is increased to 45 ℃ after the enzymolysis is carried out for 35min, the enzymolysis is carried out for 25min, and then the temperature is reduced to 16 ℃ according to the speed of 2 ℃/min;
the temperature rise rate is 1.5 ℃ rising every 4 min;
the modified sodium carboxymethylcellulose powder is prepared by mixing the following components in percentage by weight of 1: 1: 15) mixing for 12min at 85 ℃, and then performing microwave treatment for 210s at the microwave frequency of 55MHz and the power of 650W;
the extraction is carried out in a continuous pressurization mode, 4.5MPa is used as initial pressure, the pressure is increased to 11.5MPa at the speed of 0.2MPa/min, and then the pressure is maintained for 23 min.
Example 4
A method for extracting tea oil with high freezing resistance comprises the following steps:
(1) activation of camellia seeds: after camellia seeds are treated by the plant disinfectant under a constant voltage electric field with the voltage of 3V for 10, the mass ratio of the camellia seeds to the plant disinfectant is 1: 7, adding a crystal transfer agent with the mass of 5 per mill of the plant disinfectant, raising the voltage, treating for 20s under the condition of 15V, taking out camellia seeds, and draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: 1.9, treating for 25min at 33 ℃, and taking out the enzymolyzed camellia seeds;
(3) slurry blasting: maintaining the enzymolysis camellia seeds under the pressure of 1MPa for 90s, and then performing slurry explosion to obtain slurry;
(4) crude oil preparation: feeding the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2.3Pa, maintaining the pressure for 120s, shearing by using a high-speed disperser, centrifugally separating to obtain an oil layer, an emulsifying layer and residues, feeding the emulsifying layer into microwave treatment equipment, adding modified sodium carboxymethylcellulose powder with the mass of 0.4 per mill of the emulsifying layer, carrying out microwave treatment for 100s at the microwave frequency of 320MHz and the power of 370W, then placing the mixture into the high-speed disperser, shearing, centrifugally separating, and combining oil layers to obtain the crude tea oil;
(5) supercritical extraction: sending the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain finished tea oil;
the preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 40 deg.C for 20 min; treating folium Artemisiae Argyi in 150 deg.C steam for 15 min; mixing the prepared quinoa shell powder and folium artemisiae argyi, adding purified water with the mass being 20 times that of the mixture, and extracting for 1h at the temperature of 90 ℃;
the crystal transformation agent comprises the following components in parts by weight: 2.3 parts of sodium citrate and 12 parts of betaine;
mixing a citric acid solution with the mass concentration of 50% with soybean protein powder according to the mass ratio of 1: 0.5 to prepare a soybean protein solution, heating to 92 ℃, preserving heat for 10min, cooling the swollen soybean protein solution to 15 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution, and carrying out enzymolysis to obtain an enzymolysis solution;
the mixing proportion of the soybean protein solution, β -mannase, xylanase, protease and water is that β -mannase 200U, xylanase 400U, protease 3000U and water 200mL are added into each gram of the soybean protein solution;
the temperature is increased to 27 ℃ from the cooled temperature by the enzymolysis, the temperature is increased to 46 ℃ after the enzymolysis is carried out for 30min, and then the temperature is reduced to 15 ℃ according to the speed of 2 ℃/min;
the temperature rise rate is 1 ℃ rise every 5 min;
the modified sodium carboxymethylcellulose powder is prepared by mixing the following components in percentage by weight of 1: 0.6: 16, mixing for 10min at the temperature of 85 ℃, and then performing microwave treatment for 210s at the microwave frequency of 59MHz and the power of 730W;
the extraction is carried out in a continuous pressurization mode, 4.3MPa is used as initial pressure, the pressure is increased to 11.8MPa at the speed of 0.15MPa/min, and then the pressure is maintained for 21 min.
Comparative example 1
The difference from example 3 is that: no crystal transformation agent was added.
Comparative example 2
The difference from example 3 is that: modified sodium carboxymethylcellulose was not added.
Comparative example 3
The difference from the example 3 is that the enzymolysis liquid consists of soybean protein solution, β -mannase, xylanase, protease and water, wherein each 250mL of enzymolysis liquid contains β -mannase 250U, xylanase 350U and protease 2500U.
Comparative example 4
The difference from example 3 is that: the extraction is carried out without adopting a continuous pressurization mode, the extraction pressure is 11.5MPa, and the extraction time is 60 min.
Comparative example 5
The difference from example 3 is that: extracting under constant pressure of 4.5MPa for 15min, and extracting under constant pressure of 11.5MPa for 15 min.
Comparative example 6
The difference from example 3 is that: the step (4) is not subjected to microwave treatment.
Test example 1
The tea oil obtained in examples and comparative examples was subjected to acid value measurement according to the method specified in GB 5009.229-2016 and peroxide value measurement according to the method specified in GB5009.227-2016, and the results are shown in Table 1:
TABLE 1
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Acid value (mg/g) | 1.24 | 1.36 | 1.08 | 1.16 | 5.62 |
| Peroxide number (mmol/kg) | 0.84 | 1.01 | 0.64 | 1.04 | 2.76 |
| Item | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
| Acid value (mg/g) | 3.34 | 2.12 | 2.49 | 3.01 | 1.73 |
| Peroxide number (mmol/kg) | 3.12 | 2.66 | 0.89 | 5.42 | 1.96 |
The transparency and the smell and the taste of the extracted tea oil are measured according to GB/T5525-2008 identification method for the transparency, the smell and the taste of the vegetable oil. The color of the tea oil is measured according to GB/T11765-2003 oil tea seed oil, and the result is shown in Table 2;
TABLE 2
Fatty acid component analysis
Fatty acid methyl esters of the extracted oil were prepared using a Fatty Acid Methylation (FAME) method. FAME was identified by Gas Chromatography (GC) using Agilent 6890N GC-FID equipped with a fused silica capillary column (30mm x 0.25 mm). The thickness of the polyethylene glycol coating film was 0.32 μm, and the ratio of 100: 1, injecting 1 mu L of n-hexane solution containing a methylated sample; the inlet temperature was 220 ℃, the detector temperature was 260 ℃, the initial oven temperature was 170 ℃, then increased to 240 ℃ at a rate of 5 ℃/min and held at 240 ℃ for 5 min. Nitrogen was used as a carrier gas at a flow rate of 1.4 mL/min. Qualitative and quantitative AME by comparison with standard FAME mixtures; the results are shown in Table 3;
TABLE 3
Respectively measuring 90mL of the tea oil of the comparative example by using a measuring cylinder, uniformly dividing each 90mL of the tea oil of the same group into 3 parts, respectively pouring each part into 100mL of freezing tubes, respectively numbering, clamping the freezing tubes filled with the tea oil by using test tubes, placing the freezing tubes in a constant-temperature water bath kettle, heating to 80 ℃, standing and cooling to room temperature, respectively placing the freezing tubes in a-15 ℃ medical low-temperature box, a-4 ℃ low-temperature constant-temperature tank and a 0 ℃ ice-water mixture (the ice-water mixture is placed in a refrigerator), and inspecting the time of precipitates of the tea oil at low temperature, wherein the results are shown in Table 4;
TABLE 4
Claims (9)
1. A method for extracting tea oil with high freezing resistance is characterized by comprising the following steps:
(1) activation of camellia seeds: treating camellia seeds with the plant disinfectant for 10-20s in a constant-voltage electric field with the voltage of 1-3V, wherein the mass ratio of the camellia seeds to the plant disinfectant is 1: (3-7), adding a crystal modifier with the mass of 1-5 per mill of the plant disinfectant, raising the voltage, treating for 10-20s under the condition of 15-20V, taking out camellia seeds, and draining to obtain activated camellia seeds;
(2) water enzyme treatment: mixing the activated camellia seeds and the enzymolysis solution according to the proportion of 1: (1.5-2), treating for 20-30min at 30-35 ℃, and taking out the camellia seeds for enzymolysis;
(3) slurry blasting: maintaining the enzymolysis camellia seed under 1-1.8MPa for 60-90s, and then performing slurry explosion to obtain slurry;
(4) crude oil preparation: sending the slurry into a pressure tank, vacuumizing, filling inert gas, keeping the pressure at 2-2.5Pa, maintaining the pressure for 120-;
(5) supercritical extraction: and (4) feeding the slurry into a supercritical CO2 device for extraction, and collecting raffinate to obtain the finished product of the tea oil.
2. The method for extracting the tea oil with high freezing resistance as claimed in claim 1, wherein the preparation method of the botanical disinfectant comprises the following steps: grinding quinoa shell to nanometer level, and parching in a frying pan at 40-50 deg.C for 10-20 min; treating folium Artemisiae Argyi in 150 deg.C steam at 130-; mixing the prepared quinoa shell powder and folium Artemisiae Argyi, adding purified water 20-30 times of the mixture, and extracting at 70-90 deg.C for 1-3 hr.
3. The method for extracting the tea oil with high freezing resistance according to claim 1, wherein the crystal modifier comprises the following components in parts by weight: 2.3-2.9 parts of sodium citrate and 11-15 parts of betaine.
4. The method for extracting tea oil with high freezing resistance as claimed in claim 1, wherein the enzymolysis solution is prepared by mixing citric acid solution with mass concentration of 40-50% and soybean protein powder according to the mass ratio of 1 (0.2-0.6) to obtain soybean protein solution, heating to 92-95 ℃, keeping the temperature for 10-15min, cooling the swollen soybean protein solution to 15-20 ℃, adding β -mannase, xylanase, protease and water into the soybean protein solution, and performing enzymolysis.
5. The method for extracting tea oil with high freezing resistance as claimed in claim 4, wherein the mixing ratio of the soy protein solution to β -mannase, xylanase, protease and water is β -mannase 200-.
6. The method for extracting tea oil with high freezing resistance according to claim 4, wherein the temperature is raised to 27-35 ℃ from the cooled temperature by enzymolysis, the temperature is raised to 42-46 ℃ after the enzymolysis is carried out for 30-40min, the enzymolysis is carried out for 20-30min, and then the temperature is reduced to 15-20 ℃ according to the speed of 1-3 ℃/min.
7. The method for extracting camellia oil with high freezing resistance as claimed in claim 6, wherein the temperature rise rate is 1-2 ℃ every 3-5 min.
8. The method for extracting tea oil with high freezing resistance according to claim 1, wherein the modified sodium carboxymethylcellulose powder is prepared by mixing the following components in a weight ratio of 1: (0.3-1.7): (13-17) mixing for 10-15min at the temperature of 80-90 ℃, and then performing microwave treatment for 200-240s at the microwave frequency of 48-62MHz and the power of 500-800W.
9. The method for extracting tea oil with high freezing resistance according to claim 1, wherein the extraction is performed by continuously pressurizing, using 4-5MPa as initial pressure, increasing the pressure to 11-12MPa at a rate of 0.1-0.3MPa/min, and then maintaining the pressure for 20-25 min.
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| CN114796028A (en) * | 2022-06-13 | 2022-07-29 | 广州大唐化妆品有限公司 | Hair care essence oil |
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