CN115316442A - Health-care camellia oil - Google Patents

Health-care camellia oil Download PDF

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CN115316442A
CN115316442A CN202210976600.6A CN202210976600A CN115316442A CN 115316442 A CN115316442 A CN 115316442A CN 202210976600 A CN202210976600 A CN 202210976600A CN 115316442 A CN115316442 A CN 115316442A
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camellia oil
oil
mass ratio
health
camellia
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李谨璇
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04—Working-up
    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/06—Production of fats or fatty oils from raw materials by pressing
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/10—Refining fats or fatty oils by adsorption
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/12—Refining fats or fatty oils by distillation
    • 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
    • C11B5/00—Preserving by using additives, e.g. anti-oxidants
    • C11B5/0085—Substances of natural origin of unknown constitution, f.i. plant extracts

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Botany (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses health-care camellia oil which comprises the following raw materials: refining oleum Camelliae Japonicae, oleum Lini, oleum Hippophae, and plant antioxidant compound. The health camellia oil disclosed by the invention is rich in nutrition and reasonable in proportion, and has health-care effects of reducing blood fat, resisting oxidation and the like.

Description

Health-care camellia oil
Technical Field
The invention relates to the technical field of edible oil, and particularly relates to health-care camellia oil.
Background
The camellia oil is traditional edible oil in China and is prepared by removing shells of seeds of camellia oleifera trees, drying in the sun, crushing, steaming, extracting oil and filtering. Camellia oil is rich in nutrition, and contains oleic acid, linoleic acid, camellin, tea polyphenols, saponin, tannin, squalene, etc. Wherein, the linolenic acid is a nutrient substance which is necessary for the human body but can not be synthesized by the human body. Chinese patent CN102504938A discloses a camellia oil cold pressing and physical refining process, which comprises the following steps: selecting mature camellia seeds, performing microwave vacuum drying, and conveying into a huller for hulling; cold pressing the shelled camellia seeds to obtain camellia oil; removing solid impurities from the pressed camellia oil by a plate-and-frame filter press; winterizing the camellia oil subjected to plate-and-frame filter pressing; removing free fatty acid, lipid peroxidation products, water and other low boiling point substances in the winterized camellia oil by molecular distillation; filtering the camellia oil subjected to molecular distillation with a mixture of clay, activated carbon and alumina as a filter medium to remove impurities and pigments. The camellia oil prepared by the process is environment-friendly and has high oil yield, but linoleic acid in the camellia oil is lost during cold pressing and refining, and the nutritional value of the camellia oil is influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides health-care camellia oil.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a health camellia oil comprises the following raw materials: refining camellia oil, linseed oil, sea buckthorn seed oil and plant antioxidant compound.
The mass ratio of the refined camellia oil to the linseed oil to the sea-buckthorn seed oil to the plant antioxidant compound is (8-10) to (0.5-1) to (0.05-0.1).
The preparation method of the plant antioxidant compound comprises the following steps: pulverizing cleaned and air-dried folium Ginkgo, herba Gnaphalii affinis leaf and folium Eucommiae, sieving with 100-300 mesh sieve, and mixing uniformly according to the mass ratio of (2-5) to (1-2) to obtain plant powder; adding plant powder into 70-85wt% edible alcohol according to a material-liquid ratio of 1g (8-15) mL, performing ultrasonic assisted extraction at 50-70 ℃ for 2-4h, filtering, concentrating the filtrate under reduced pressure to remove organic solvent, and freeze-drying to obtain the plant antioxidant compound.
According to the invention, three edible oils of refined camellia oil, linseed oil and sea-buckthorn seed oil are compounded, so that the health-care effect of the camellia oil is improved, and the blood fat of a human body can be effectively controlled after the camellia oil is eaten for a long time. In addition, the plant antioxidant compound is added as an additive, so that the camellia oil is green and healthy, and the antioxidant active substances can prevent the camellia oil from being oxidized in the storage process to cause quality deterioration while the nutritional ingredients of the camellia oil are enriched.
The refined camellia oil is prepared by the following method:
p1, shelling: slowly parching semen Camelliae Japonicae at 55-60 deg.C under relative air pressure of 20-30kPa and stirring speed of 20-30rpm for 40-50min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130-140 ℃, the oil outlet temperature is 90-95 ℃ and the pressure is 40-42MPa, and then filtering to remove solid impurities;
p3 winterization: mixing the primary oil obtained in the step P2 and a coagulant aid at a mass ratio of 960-1100 (0.8-1.2) at 20-30 ℃, homogenizing at a rotation speed of 7000-8500rpm for 2-5min, then putting the mixture in an environment at the temperature of 0-3 ℃ for winterization treatment for 27-35h, filtering out solidified wax ester crystals to obtain winterized camellia oil;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 and the activated clay according to the mass ratio of (95-110) to (2-3), heating to 80-85 ℃, stirring at the rotating speed of 40-60rpm for 20-30min, and filtering to obtain decolorized camellia oil;
p5, deodorization: deodorizing the decolorized camellia oil obtained in step P4 for 20-25min at 165-170 deg.C and vacuum degree of 20-30Pa to obtain refined camellia oil.
It is known that unsaturated fatty acids have many beneficial effects on human body, such as lowering blood viscosity, improving blood microcirculation, maintaining the relative mobility of cell membranes to ensure the normal physiological function of cells, esterifying cholesterol to reduce cholesterol and triglyceride in blood, increasing the activity of brain cells, and enhancing memory and thinking ability.
The content of unsaturated fatty acid in the camellia oil is up to more than 90%, wherein the content of oleic acid and linoleic acid is extremely high, and particularly, the linolenic acid rich in the camellia oil is a nutrient substance which is necessary for a human body and cannot be synthesized by the human body.
In the traditional camellia oil production process, winterization treatment is usually adopted to reduce the solid fat content in the camellia oil, namely, wax such as glyceride with higher freezing point is crystallized and separated out by a low-temperature means, so that the content of saturated fatty acid ester in the biodiesel is reduced, and meanwhile, the content of unsaturated fatty acid ester including oleic acid and linolenic acid is improved, and the camellia oil with higher content of unsaturated fatty acid value is obtained. However, in the prior art, wax such as glyceride and the like which is not low in content still remains in the camellia oil after winterization treatment, the wax is not beneficial to human health, the content of beneficial unsaturated fatty acid is reduced, and the wax can separate out flocculent precipitate under the conditions of variable temperature and illumination, such as transportation, storage and selling, and the like, so that the appearance and the quality of the product are extremely influenced.
Therefore, the invention aims to provide a coagulant aid capable of further improving the crystallization precipitation efficiency of waxy materials such as glyceride with higher freezing point in the winterization treatment process, so as to improve the quality of the obtained camellia oil and the content of unsaturated fatty acid, and obtain the refined camellia oil which is rich in oleic acid and linoleic acid and has the effect of remarkably reducing blood fat.
The winterization process of the camellia oil comprises three steps of crystal nucleus formation, crystal growth and crystal separation of glyceride waxiness. Wherein, the nucleation and crystal growth are collectively called as the oil crystallization process, in the process, some triglyceride with higher freezing point in the oil is firstly crystallized and nucleated to form a plurality of fine crystal grains, and the fine crystal grains and the residual fine solid impurity particles in the camellia oil play the role of crystal nucleus in the crystallization process. The part of triglyceride which is not crystallized in the liquid oil continuously condenses on the surface of the crystal nuclei, so that the crystal nuclei continuously grow and finally grow into large-particle crystals which can be physically filtered and removed. Either nucleation or growth of the nuclei can be driven by the concentration difference of supersaturation of the solution. The crystallization phenomenon of triglyceride generally has polymorphism, namely a plurality of crystal phases, and the melting points, melting enthalpies, melting expansion rates and stability of the crystal phases are different, but the coagulant aid prepared by the specific method can achieve the purpose of promoting the nucleation and growth of glyceride by improving the surface free energy of a crystal nucleus attached growth environment, and simultaneously guide wax crystals to generate phase change towards the direction of more stable crystal forms, so that the phenomenon that metastable phase reverse reaction dissolution returns to a liquid phase is avoided, the precipitation crystallization separation efficiency of the waxes such as glyceride and the like is improved, the content of saturated fat in camellia oil is reduced, and the relative content of unsaturated fatty acid including oleic acid and linoleic acid is improved.
The preparation method of the coagulant aid comprises the following steps:
l1, mixing polyamide, a shiitake seed extract, cysteine and 50wt.% ethanol aqueous solution according to the mass ratio of (10-13) to (1-3) to (0.1-0.3) to (72-78), heating to 60-62 ℃, stirring at 1400-1600rpm for 50-60min, centrifuging at 7000-8000rpm for 5-8min, and filtering to obtain a bottom precipitate I;
l2 is prepared by using carbon dioxide as medium at 60-65 deg.C and gas flow rate of 4500-5000m 3 And/h, drying the precipitate I obtained in the step L1 for 40-45min by hot air to obtain the coagulant aid.
The polyamide is a good adsorbent which is safe, environment-friendly and non-toxic, the main chain of the polyamide contains a plurality of repeated acylamino groups, the acylamino groups can be subjected to cross-linking and condensation reactions with sitosterol and other substances in the stone flower seed extract, the obtained product can generate hydrogen bonds with wax including triglyceride and the like in the virgin camellia oil to attract each other, the wax is promoted to nucleate in a winterization environment and grow stable large-size grains, and the grains are filtered and removed, so that the content of unsaturated fatty acid including oleic acid and linoleic acid in the obtained camellia oil is increased.
The sulfhydryl group at a specific position contained in the cysteine can generate hydrogen bond with the polyamide and the shiitake seed extract, thereby enhancing the crosslinking degree of the polyamide and the shiitake seed extract and improving the conformation distribution between the molecular main chain and the branched chain of the product obtained by crosslinking the polyamide and the shiitake seed extract, so that the obtained coagulant aid has stronger adsorption and nucleation inducing capacity for waxes including triglyceride and the like.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the lithospermum seeds with 15-20wt.% ethanol water solution according to the mass ratio of 1 (5-7), and pressing for 15-25min under the pressure of 200-240MPa to obtain a lithospermum seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at the temperature of 20-30 ℃, stirring at the rotating speed of 120-200rpm for 40-60min, then centrifuging at the rotating speed of 6000-8000rpm for 3min, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is (65-70) to 1;
s3, freeze-drying the precipitate II obtained in the step S2 for 1-3h in an environment with the temperature of (-40) - (-35) DEG C, and then crushing to obtain the lithospermum seed extract.
The precipitation auxiliary agent is one or a mixture of two of calcium oleate and calcium lactate. Preferably, the precipitation auxiliary agent is a mixture of calcium oleate and calcium lactate in a mass ratio of (1-3) to (1-3). More preferably, the precipitation aid is a mixture of calcium oleate and calcium lactate in a mass ratio of 2:1.
The invention adopts the aqueous solution of ethanol as the extraction solvent of the lithospermum seeds, and besides providing necessary kinetic driving force for ultrahigh pressure treatment, the ultrahigh pressure treatment can promote the rupture and decomposition of cell structures such as cell walls and the like in the lithospermum seeds, thereby increasing the yield of the lithospermum seed extract and the yield of effective substances.
Calcium ions in calcium oleate and calcium lactate can be combined with organic acid in the extract of the lithospermum seeds to generate complex precipitation, so that the effective components in the extract of the lithospermum seeds are separated from the ultrahigh pressure extraction solvent. In addition, the unsaturated bond in the oleate and the hydroxyl group positioned on the specific point in the lactate have good compatibility with each other in polarity matching degree, so that the density of the active group on the molecular surface of the obtained coagulant aid is higher, the nucleation and growth rate of various waxes are further improved, the content of unsaturated fatty acids including oleic acid and linoleic acid is improved, and the quality of the obtained camellia oil is improved.
The preparation method of the health-care camellia oil comprises the following steps:
adding the refined camellia oil, the linseed oil, the sea-buckthorn seed oil and the plant antioxidant compound into a stirrer according to the mass ratio of (8-10): (0.5-1): (0.5-1): 0.05-0.1), and stirring for 30-50min at the stirring speed of 10-30rpm to obtain the health camellia oil.
The invention has the beneficial effects that: the health camellia oil disclosed by the invention is rich in nutrition and reasonable in proportion, and has health-care effects of reducing blood fat, resisting oxidation and the like. The refined camellia oil is obtained by the steps of shelling, squeezing, winterization, decoloration, deodorization and the like, and a specific coagulant aid is adopted for auxiliary treatment in the winterization treatment, so that nutritional ingredients such as linoleic acid and the like are retained to the maximum extent.
Detailed Description
The foregoing summary of the invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above-described subject matter of the present invention is limited only by the following examples.
Introduction of some raw materials in this application:
camellia seeds: camellia seed, wanglong planting specialty cooperative, qiyang county, variety: cen xi Soft No. 2.
Activated clay, CAS:70131-50-9, hong environmental protection science and technology limited of Henan Qing, particle size: 220 meshes, specification grade: and (4) food grade.
Polyamide, CAS:5892-11-5, suzhou Huidao plastification import & export Co., ltd, brand: PA66, du pont usa, trade mark: FG133F1, specification grade: and (4) food grade.
Dan Huazi: nicandra physiaoides (L) gartn, bachuanbao grocery store, cat #: 002.
example 1
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: homogenizing the primary oil obtained in the step P2 at 22 deg.C at 8000rpm for 3min, winterizing at 2 deg.C for 30h, filtering out solidified wax ester crystal to obtain winterized camellia oil;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to a mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
Example 2
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to a mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, cysteine, 50wt.% ethanol aqueous solution in mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
Example 3
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to the mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, a shiitake seed extract, and a 50wt.% ethanol aqueous solution are mixed in a mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the shiitake seeds with 20wt.% ethanol water solution according to a mass ratio of 1:6, feeding the mixture into a reaction kettle, and pressing the mixture for 20min under the pressure of 220MPa to obtain a shiitake seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at 22 ℃, stirring for 40min at the rotating speed of 200rpm, then centrifuging for 3min at the rotating speed of 8000rpm, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is 70; the precipitation auxiliary agent is calcium oleate;
s3, freeze-drying the precipitate II obtained in the step S2 in an environment with the temperature of-35 ℃ for 2 hours, and then crushing to obtain the stone flower seed extract.
Example 4
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to the mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, shiitake seed extract, cysteine, 50wt.% ethanol aqueous solution, are mixed at a mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the shiitake seeds with an ethanol aqueous solution with the concentration of 20wt.% according to the mass ratio of 1:6, and treating for 5min by using microwaves with the power of 700W and the frequency of 500MHz to obtain a shiitake seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at 22 ℃, stirring for 40min at the rotating speed of 200rpm, then centrifuging for 3min at the rotating speed of 8000rpm, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is 70; the precipitation auxiliary agent is calcium oleate;
s3, freeze-drying the precipitate II obtained in the step S2 in an environment with the temperature of-35 ℃ for 2 hours, and then crushing to obtain the stone flower seed extract.
Example 5
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to the mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min at 170 ℃ and vacuum degree of 20Pa to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, shiitake seed extract, cysteine, 50wt.% aqueous ethanol solution, are mixed at a mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the shiitake seeds with 20wt.% ethanol water solution according to a mass ratio of 1:6, feeding the mixture into a reaction kettle, and pressing the mixture for 20min under the pressure of 220MPa to obtain a shiitake seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at 22 ℃, stirring for 40min at the rotating speed of 200rpm, then centrifuging for 3min at the rotating speed of 8000rpm, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is 70; the precipitation auxiliary agent is calcium lactate;
s3, freeze-drying the precipitate II obtained in the step S2 in an environment with the temperature of-35 ℃ for 2 hours, and then crushing to obtain the stone flower seed extract.
Example 6
The refined camellia oil is prepared by the following method:
p1, shelling: parching semen Camelliae Japonicae at 60 deg.C under relative air pressure of 20kPa and stirring speed of 20rpm for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to the mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, shiitake seed extract, cysteine, 50wt.% aqueous ethanol solution, are mixed at a mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the shiitake seeds with 20wt.% ethanol water solution according to a mass ratio of 1:6, feeding the mixture into a reaction kettle, and pressing the mixture for 20min under the pressure of 220MPa to obtain a shiitake seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at 22 ℃, stirring at the rotating speed of 200rpm for 40min, then centrifuging at the rotating speed of 8000rpm for 3min, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is 70; the precipitation auxiliary agent is calcium oleate;
s3, freeze-drying the precipitate II obtained in the step S2 in an environment with the temperature of-35 ℃ for 2 hours, and then crushing to obtain the stone flower seed extract.
Example 7
The refined camellia oil is prepared by the following method:
p1, shelling: slowly baking camellia seeds at a low temperature of 60 ℃, under a relative air pressure of 20kPa and a stirring speed of 20rpm, and removing the shells for 40min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a barrel is 130 ℃, the temperature of oil extraction is 90 ℃ and the pressure is 40MPa, and then filtering to remove solid impurities in the primary oil;
p3 winterization: mixing the primary oil obtained in the step P2 with a coagulant aid according to a mass ratio of 1000;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 with activated clay according to the mass ratio of 100;
p5, deodorization: deodorizing the decolorized camellia oil obtained in the step P4 for 20min under the conditions that the temperature is 170 ℃ and the vacuum degree is 20Pa, so as to obtain the refined camellia oil.
The preparation method of the coagulant aid comprises the following steps:
l1 polyamide, shiitake seed extract, cysteine, 50wt.% aqueous ethanol solution, are mixed at a mass ratio of 11;
l2 is carbon dioxide as medium, at 65 deg.C and gas flow rate of 5000m 3 And/h, drying the precipitate I obtained in the step L1 for 45min by hot air to obtain the coagulant aid.
The preparation method of the Dan Huazi extract comprises the following steps:
s1, mixing the shiitake seeds with 20wt.% ethanol water solution according to a mass ratio of 1:6, feeding the mixture into a reaction kettle, and pressing the mixture for 20min under the pressure of 220MPa to obtain a shiitake seed extracting solution;
s2, adding a precipitation auxiliary agent into the shiitake seed extracting solution obtained in the step S1 at 22 ℃, stirring for 40min at the rotating speed of 200rpm, then centrifuging for 3min at the rotating speed of 8000rpm, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is 70; the precipitation auxiliary agent is a mixture of calcium oleate and calcium lactate in a mass ratio of 2:1;
s3, freeze-drying the precipitate II obtained in the step S2 in an environment with the temperature of-35 ℃ for 2 hours, and then crushing to obtain the stone flower seed extract.
Example 8
A health camellia oil is prepared by the following steps:
adding the refined camellia oil, the linseed oil, the sea buckthorn seed oil and the plant antioxidant compound obtained in the example 7 into a stirrer according to a mass ratio of 9.
The preparation method of the plant antioxidant compound comprises the following steps: crushing and sieving cleaned and dried ginkgo leaves, twisted leaves and eucommia leaves through a 200-mesh sieve, and uniformly mixing according to a mass ratio of 3; adding plant powder into 78wt% edible alcohol according to the material-liquid ratio of 1g, 10mL, performing ultrasonic-assisted extraction at 65 ℃ for 3.5h, filtering, concentrating the filtrate under reduced pressure to remove an organic solvent, and freeze-drying to obtain the plant antioxidant compound.
Test example 1
Oleic acid and linoleic acid content testing: the contents of oleic acid and linoleic acid in the refined camellia oil obtained in the embodiments 1 to 7 of the present invention were determined according to NY/T3299-2018, determination of oleic acid and linoleic acid in vegetable oil by near infrared spectroscopy. The temperature of the test environment was 23 ℃ and the relative humidity was 60%. Each example tested 5 different samples and the test results were averaged. The test results are shown in table 1.
TABLE 1 oleic acid, linoleic acid content of refined Camellia oil
Figure BDA0003798695420000121
Figure BDA0003798695420000131
In the traditional camellia oil production process, winterization treatment is usually adopted to reduce the solid fat content in the camellia oil, namely, wax such as glyceride with higher freezing point is crystallized and separated out by a low-temperature means, so that the content of saturated fatty acid ester in the biodiesel is reduced, and meanwhile, the content of unsaturated fatty acid ester including oleic acid and linolenic acid is improved, and the camellia oil with higher content of unsaturated fatty acid value is obtained. However, in the prior art, wax such as glyceride and the like which is not low in content still remains in the camellia oil after winterization treatment, the wax is not beneficial to human health, the content of beneficial unsaturated fatty acid is reduced, and the wax can separate out flocculent precipitate under the conditions of variable temperature and illumination, such as transportation, storage and selling, and the like, so that the appearance and the quality of the product are extremely influenced. Therefore, the invention aims to provide a coagulant aid capable of further improving the crystallization precipitation efficiency of waxy materials such as glyceride with higher freezing point in the winterization treatment process, so as to improve the quality of the obtained camellia oil and the content of unsaturated fatty acid, and obtain the refined camellia oil which is rich in oleic acid and linoleic acid and has the effect of remarkably reducing blood fat. The winterization process of the camellia oil comprises three steps of crystal nucleus formation, crystal growth and crystal separation of glyceride waxiness. Wherein, the nucleation and crystal growth are collectively called as the oil crystallization process, in the process, some triglyceride with higher freezing point in the oil is firstly crystallized and nucleated to form a plurality of fine crystal grains, and the fine crystal grains and the residual fine solid impurity particles in the camellia oil play the role of crystal nucleus in the crystallization process. The part of triglyceride which is not crystallized in the liquid oil continuously condenses on the surface of the crystal nuclei, so that the crystal nuclei continuously grow and finally grow into large-particle crystals which can be physically filtered and removed. Either nucleation or growth of the nuclei can be driven by the concentration difference of supersaturation of the solution. The crystallization phenomenon of triglyceride generally has polymorphism, namely a plurality of crystal phases, and the melting points, melting enthalpies, melting expansion rates and stability of the crystal phases are different, but the coagulant aid prepared by the specific method can achieve the purpose of promoting the nucleation and growth of glyceride by improving the surface free energy of a crystal nucleus attached growth environment, and simultaneously guide wax crystals to generate phase change towards the direction of more stable crystal forms, so that the phenomenon that metastable phase reverse reaction dissolution returns to a liquid phase is avoided, the precipitation crystallization separation efficiency of the waxes such as glyceride and the like is improved, the content of saturated fat in camellia oil is reduced, and the relative content of unsaturated fatty acid including oleic acid and linoleic acid is improved. The polyamide is a good adsorbent which is safe, environment-friendly and non-toxic, the main chain of the polyamide contains a plurality of repeated acylamino groups, the acylamino groups can be subjected to cross-linking and condensation reactions with sitosterol and other substances in the stone flower seed extract, the obtained product can generate hydrogen bonds with wax including triglyceride and the like in the virgin camellia oil to attract each other, the wax is promoted to nucleate in a winterization environment and grow stable large-size grains, and the grains are filtered and removed, so that the content of unsaturated fatty acid including oleic acid and linoleic acid in the obtained camellia oil is increased. The sulfydryl contained in the cysteine and positioned at a specific position can generate hydrogen bonds with the polyamide and the stone flower seed extract, so that the crosslinking degree of the polyamide and the stone flower seed extract is enhanced, the conformation distribution between the molecular main chain and the branched chain of the product obtained by crosslinking the polyamide and the stone flower seed extract is improved, and the obtained coagulant aid has stronger adsorption and nucleation-inducing capacity for waxes including triglyceride and the like. The invention adopts the aqueous solution of ethanol as the extraction solvent of the lithospermum seeds, and besides providing necessary kinetic driving force for ultrahigh pressure treatment, the ultrahigh pressure treatment can promote the rupture and decomposition of cell structures such as cell walls and the like in the lithospermum seeds, thereby increasing the yield of the lithospermum seed extract and the yield of effective substances. Calcium ions in calcium oleate and calcium lactate can be combined with organic acid in the extract of the lithospermum seeds to generate complex precipitation, so that the effective components in the extract of the lithospermum seeds are separated from the ultrahigh pressure extraction solvent. In addition, the unsaturated bond in the oleate and the hydroxyl group positioned on the specific point in the lactate have good compatibility with each other in polarity matching degree, so that the density of the active group on the molecular surface of the obtained coagulant aid is higher, the nucleation and growth rate of various waxes are further improved, the content of unsaturated fatty acids including oleic acid and linoleic acid is improved, and the quality of the obtained refined camellia oil is improved.
Test example 2
Rat experiment:
(1) Preparing high-fat feed: mixing and sterilizing a basal feed, lard, egg yolk powder, white granulated sugar and cholesterol in a mass ratio of 66.
(2) Adapting to feeding: firstly, feeding 80 rats (with the weight range of 200-210 g) with the basic feed under the experimental environment (the temperature is 24 ℃, and the relative humidity is 60%), maintaining normal day-night circulation, providing free drinking water and food intake, and ensuring that the time for adapting to feeding is 7 days.
(3) Molding and feeding: rats that completed the acclimatization were randomly divided into 2 groups, of which: 60 patients in the hyperlipemia group are fed with high-fat feed; the group with normal blood lipid had 20 animals, and was continuously fed with basal diet. Both groups provided free access to drinking water. The time period of model breeding is 21d, then fasting is carried out for 12h, and then blood is collected in the tail vein. Four indexes of blood fat of rats, namely total cholesterol TC, triglyceride TG, low-density lipoprotein LDL-C and high-density lipoprotein HDL-C, are measured by a Hitachi 7180 full-automatic biochemical analyzer and an oxidase method. The four contents of blood fat of the rat with the hyperlipemia group are all obviously higher than that of the rat with the normal blood fat, which proves that the model building is successful.
(4) Blood fat reduction experiment: the rats of the hyperlipemia group successfully molded were randomly divided into 3 groups, and fed with a mixture of the refined camellia oil obtained in examples 1 and 7 of the present invention and the high-fat diet in a mass ratio of 1:7, respectively, and a hyperlipemia control group fed with only the high-fat diet without the refined camellia oil was set to maintain free intake of drinking water and normal day and night cycles. The duration of the blood fat reducing experiment is 28 days, then fasting is carried out for 12 hours, blood is collected in the tail vein, serum is prepared, and four indexes (TC, TG, LDL-C and HDL-C) of blood fat are measured.
(5) Data processing: SPSS software is adopted to carry out statistical analysis on experimental data, all data are represented in a form of x +/-s, t test is adopted among groups, P <0.05 is different, and the experimental result has statistical significance. The results of the experiment are shown in table 2.
TABLE 2 influence of refined Camellia oil on the blood lipid content of hyperlipidemic rat
Figure BDA0003798695420000151
From the experimental results in table 2, it is obvious that the refined camellia oil obtained by the specific method of the present invention has a significant effect of reducing blood lipid for rats cultured on high-fat diet.
It is known that unsaturated fatty acids have many beneficial effects on human body such as reducing blood viscosity, improving blood microcirculation, maintaining relative fluidity of cell membranes to ensure normal physiological functions of cells, esterifying cholesterol to reduce cholesterol and triglyceride in blood, increasing activity of brain cells, and enhancing memory and thinking ability. The content of unsaturated fatty acid in the camellia oil is up to more than 90%, wherein the content of oleic acid and linoleic acid is extremely high, and particularly, the linolenic acid rich in the camellia oil is a nutrient substance which is necessary for a human body and cannot be synthesized by the human body. The camellia oil contains a plurality of substances which participate in various specific physiological activities, such as tea polyphenol and camellin, can effectively improve cardiovascular and cerebrovascular diseases, reduce cholesterol and fasting blood sugar, inhibit the increase of triglyceride content, and has obvious effect on inhibiting cancer cells.

Claims (8)

1. The health camellia oil is characterized by comprising the following raw materials: refining oleum Camelliae Japonicae, oleum Lini, oleum Hippophae, and plant antioxidant compound.
2. The health camellia oil as claimed in claim 1, wherein the mass ratio of the refined camellia oil, the linseed oil, the sea buckthorn seed oil and the plant antioxidant compound is (8-10): (0.5-1): (0.05-0.1).
3. The health camellia oil as claimed in claim 1, wherein the plant antioxidant complex is prepared by the method comprising: crushing cleaned and dried ginkgo leaves, twisted leaves and eucommia leaves, and uniformly mixing the crushed ginkgo leaves, the twisted leaves and the eucommia leaves according to the mass ratio of (2-5) to (1-2) to obtain plant powder; adding plant powder into 70-85wt% edible alcohol according to a material-liquid ratio of 1g (8-15) mL, performing ultrasonic assisted extraction at 50-70 ℃ for 2-4h, filtering, concentrating the filtrate under reduced pressure to remove organic solvent, and freeze-drying to obtain the plant antioxidant compound.
4. The health camellia oil of claim 1, wherein the refined camellia oil is prepared by the method comprising:
p1, shelling: slowly parching semen Camelliae Japonicae at 55-60 deg.C under relative air pressure of 20-30kPa and stirring speed of 20-30rpm for 40-50min;
p2, squeezing: extracting primary oil from the camellia seeds obtained in the step P1 under the conditions that the temperature of a press chamber is 130-140 ℃, the oil outlet temperature is 90-95 ℃ and the pressure is 40-42MPa, and then filtering to remove solid impurities;
p3 winterization: mixing the primary oil obtained in the step P2 and a coagulant aid at a mass ratio of 960-1100 (0.8-1.2) at 20-30 ℃, homogenizing at a rotation speed of 7000-8500rpm for 2-5min, then putting the mixture in an environment at the temperature of 0-3 ℃ for winterization treatment for 27-35h, filtering out solidified wax ester crystals to obtain winterized camellia oil;
p4 decolorization: mixing the winterized camellia oil obtained in the step P3 and the activated clay according to the mass ratio of (95-110) to (2-3), heating to 80-85 ℃, stirring at the rotating speed of 40-60rpm for 20-30min, and filtering to obtain decolorized camellia oil;
p5, deodorization: deodorizing the decolorized camellia oil obtained in step P4 for 20-25min at 165-170 deg.C and vacuum degree of 20-30Pa to obtain refined camellia oil.
5. The health camellia oil of claim 4, wherein the coagulant aid is prepared by the steps of:
l1, mixing polyamide, a lithospermum seed extract, cysteine and 50wt.% ethanol aqueous solution according to the mass ratio of (10-13): 1-3): 0.1-0.3): 72-78, heating to 60-62 ℃, stirring at the rotating speed of 1400-1600rpm for 50-60min, then centrifuging at the rotating speed of 7000-8000rpm for 5-8min, and filtering to obtain a bottom precipitate I;
l2 is prepared by using carbon dioxide as medium at 60-65 deg.C and with gas flow rate of 4500-5000m 3 And/h, drying the precipitate I obtained in the step L1 for 40-45min by hot air to obtain the coagulant aid.
6. The health camellia oil of claim 5, wherein the Dan Huazi extract is prepared by the method comprising:
s1, mixing the lithospermum seeds with 15-20wt.% ethanol water solution according to the mass ratio of 1 (5-7), and pressing for 15-25min under the pressure of 200-240MPa to obtain a lithospermum seed extracting solution;
s2, adding a precipitation auxiliary agent into the stone flower seed extracting solution obtained in the step S1 at the temperature of 20-30 ℃, stirring at the rotating speed of 120-200rpm for 40-60min, then centrifuging at the rotating speed of 6000-8000rpm for 3min, and filtering to obtain a bottom precipitate II; the mass ratio of the shihua seed extracting solution to the precipitation auxiliary agent is (65-70) to 1;
s3, freeze-drying the precipitate II obtained in the step S2 for 1-3h in an environment with the temperature of (-40) - (-35) DEG C, and then crushing to obtain the lithospermum seed extract.
7. The health camellia oil of claim 6, wherein: the precipitation auxiliary agent is one or a mixture of two of calcium oleate and calcium lactate.
8. The method for preparing health camellia oil according to any one of claims 1-7, wherein: the method comprises the following steps:
adding the refined camellia oil, the linseed oil, the sea-buckthorn seed oil and the plant antioxidant compound into a stirrer according to the mass ratio of (8-10): (0.5-1): (0.5-1): 0.05-0.1), and stirring for 30-50min at the stirring speed of 10-30rpm to obtain the health camellia oil.
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Publication number Priority date Publication date Assignee Title
CN115778876A (en) * 2022-12-14 2023-03-14 怀化学院 Antioxidant camellia oil composition, shampoo and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115778876A (en) * 2022-12-14 2023-03-14 怀化学院 Antioxidant camellia oil composition, shampoo and preparation method thereof

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