CN115737511A - Method for obtaining aloe flower extract, aloe flower emulsion and device - Google Patents
Method for obtaining aloe flower extract, aloe flower emulsion and device Download PDFInfo
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- CN115737511A CN115737511A CN202211335870.5A CN202211335870A CN115737511A CN 115737511 A CN115737511 A CN 115737511A CN 202211335870 A CN202211335870 A CN 202211335870A CN 115737511 A CN115737511 A CN 115737511A
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- aloe
- flower
- aloe flower
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/361—Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides thereof
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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Abstract
The invention provides a method for obtaining aloe flower extract, aloe flower emulsion and a device, wherein the method comprises the following steps: placing aloe flower in an extraction tank, adding an extraction solvent, wherein the extraction solvent is aloe vera leaf water or aloe vera gel juice to obtain aloe flower crude extract; clarifying the aloe flower crude extract to obtain a clarified crude extract; carrying out microfiltration separation treatment on the clarified crude extract by using a microfiltration membrane to obtain microfiltration permeate; performing ultrafiltration on the microfiltration permeate by using an ultrafiltration membrane to obtain ultrafiltration permeate; filtering out pigment, salt and acid substances in the ultrafiltration permeate by using exchange resin to obtain an initial aloe flower extract; concentrating the initial aloe flower extractive solution with nanofiltration membrane to obtain aloe flower extractive solution. Can improve the extraction efficiency and purity of the aloe flower extract.
Description
Technical Field
The invention relates to the technical field of plant processing and refining, in particular to a method for obtaining an aloe flower extracting solution, an aloe flower emulsion and a device.
The application case is a divisional application of a patent application with the application number of 202210546394.5.
Background
The effective component polyphenol in aloe plant mainly exists in skin, root, leaf, flower and fruit of the plant, and has the functions of whitening, sun screening, resisting aging, moistening, astringing, resisting bacteria, resisting inflammation, relieving fever, protecting liver, resisting cancer, killing parasite, enhancing immunity, etc., so that the aloe plant has special medicinal effect, and can also be used for beautifying and beautifying. However, in the cosmetics, daily chemical products and the like on the market at present, the aloe leaves are used for extracting and processing the aloe leaves, compared with the aloe raw materials extracted and prepared from aloe flowers, the aloe flowers are few and few, and the research and development on the aspects of extraction, processing and application of the aloe flowers are relatively lacking.
Researches show that the total polyphenol content in the aloe flower is higher, but because the extraction process of the aloe flower is greatly different from that of the aloe leaf, the extraction of the aloe flower at present generally comprises the steps of adding a fresh or dry aloe flower product into a solvent, extracting and filtering at a certain temperature, and concentrating the filtrate to obtain the aloe flower extract, wherein the solvent is selected from water, glycerol and propylene glycol. However, in this method, water is used as a solvent, and the extraction efficiency of the aloe flower is low, while glycerin and propylene glycol are used as solvents, so that the obtained aloe flower extract contains the solvent and has low purity.
Disclosure of Invention
In view of this, the present invention aims to provide an aloe flower emulsion, which improves the extraction efficiency and purity of the aloe flower extract.
In a first aspect, an embodiment of the present invention provides a method for obtaining an aloe flower extract, including:
placing aloe flower in an extraction tank, adding an extraction solvent, wherein the extraction solvent is aloe vera leaf water or aloe vera gel juice to obtain aloe flower crude extract;
clarifying the aloe flower crude extract to obtain a clarified crude extract;
performing microfiltration separation treatment on the clarified crude extract by using a microfiltration membrane to obtain microfiltration permeating liquid;
performing ultrafiltration on the microfiltration permeating liquid by using an ultrafiltration membrane to obtain ultrafiltration permeating liquid;
filtering out pigment, salt and acid substances in the ultrafiltration permeate by using exchange resin to obtain an initial aloe flower extract;
concentrating the primary aloe flower extract by using a nanofiltration membrane to obtain an aloe flower extract.
With reference to the first aspect, an embodiment of the present invention provides a first possible implementation manner of the first aspect, wherein a liquid-to-material ratio of the extraction solvent to the aloe flower is 30 to 1 (v/w), a stirring temperature is 55 to 85 ℃, and a stirring time is 1 to 2 hours.
In combination with the first aspect, embodiments of the present invention provide a second possible implementation manner of the first aspect, wherein the aloe vera leaf water has a pH of 3.5 to 5.0, an O-acetyl group of 10mg/kg, an electrical conductivity of 50 μ s/cm or less, and the aloe vera gel juice has a pH of 3.5 to 5.0, and an O-acetyl group of 375mg/kg or more.
In combination with the first aspect, the present examples provide a third possible implementation manner of the first aspect, wherein the concentration of the clarifying agent solution for clarifying treatment is 1% to 3%, and the addition amount is 6% to 8% of the amount of aloe vera leaf water or the amount of aloe vera gel juice.
In combination with the third possible embodiment of the first aspect, the present example provides a fourth possible embodiment of the first aspect, wherein the clarifying agent solution is obtained by stirring a small amount of aloe vera leaf water or aloe vera gel juice to form a paste, adding the aloe vera leaf water or aloe vera gel juice, and stirring and swelling for 12 hours.
With reference to the first aspect, the present invention provides a fifth possible implementation manner of the first aspect, wherein the membrane pore size of the microfiltration membrane is 0.1 to 0.3 μm.
In combination with the fifth possible embodiment of the first aspect, the present examples provide a sixth possible embodiment of the first aspect, wherein the microfiltration membrane comprises: inorganic ceramic membrane, organic microfiltration membrane.
With reference to the first aspect and any one of the first to sixth possible implementation manners of the first aspect, an embodiment of the present invention provides a seventh possible implementation manner of the first aspect, wherein the filtering, by using an exchange resin, pigments, salts, and acids in the ultrafiltration permeate includes:
according to the ultrafiltration permeation liquid: the strong-acid styrene cation exchange resin is 10-20: 1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-50 min to obtain a first extract;
according to the first extracting solution: 10-20 parts of macroporous strongly basic styrene anion exchange resin: 1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-50 min to obtain a second extracting solution;
according to the second extracting solution: 10-20% of macroporous weakly basic acrylic acid anion exchange resin: 1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-50 min to obtain the initial aloe flower extracting solution.
In a second aspect, embodiments of the present invention also provide an aloe flower emulsion comprising:
caprylic acid, accounting for 5% of the total amount;
the shea butter accounts for 2 percent of the total amount;
hydrogenated poly-decene, accounting for 2% of the total amount;
oleic acid erucic acid ester accounting for 2% of the total amount;
cetearyl alcohol, accounting for 2.5% of the total;
glycerol stearate accounting for 1.5 percent of the total amount;
350CST dimethyl silicone oil accounting for 0.5 percent of the total amount;
propyl hydroxybenzoate accounting for 0.1% of the total amount;
TEGO CARE CG 90, accounting for 1.5% of the total amount;
allantoin, accounting for 0.2% of the total amount;
methyl hydroxybenzoate accounting for 0.2% of the total amount;
glycerol accounting for 8% of the total amount;
EDTA-2NA, accounting for 0.05% of the total amount;
xanthan gum, accounting for 0.1% of the total amount;
carbomer 940 accounting for 0.35 percent of the total amount;
deionized water, adjusting the total amount to 100%;
triethanolamine, in an appropriate amount;
the aloe flower extract accounts for 3 percent of the total amount;
a proper amount of preservative;
and (4) proper amount of essence.
In a third aspect, an embodiment of the present application provides an apparatus for obtaining an aloe flower extract, including: a crusher, an extraction tank, a microfiltration membrane tube, an ultrafiltration membrane tube, a resin exchanger and a nanofiltration membrane tube, wherein,
the crusher is positioned above the extraction tank, and the outlet of the crusher is communicated with the first inlet of the extraction tank;
a solvent tube marked with transparent volume scales is arranged on one side above the extraction tank, and the lower end of the solvent tube is provided with a switch and is communicated with the inner cavity of the extraction tank through the switch;
a clarifying agent solution marked with transparent volume scales is arranged on the other side above the extraction tank, and a switch is arranged at the lower end of the clarifying agent solution and communicated with the inner cavity of the extraction tank through the switch;
a heater is arranged around the bottom of the extraction tank, a heating control button is arranged on the side surface of the extraction tank, the heating control button is connected to the heater through a circuit, a graduated scale marked with a transparent volume is arranged from the bottom to the top of the extraction tank, and a stirrer is arranged in an inner cavity of the extraction tank;
a coarse extract outlet controlled by a switch is arranged at the center of the bottom of the extraction tank, and a vibrating screen is arranged in the middle of the coarse extract outlet;
the microfiltration membrane tube is internally provided with a one-stage or multi-stage microfiltration membrane, the inlet of the microfiltration membrane tube is connected to the crude extract outlet of the extraction tank, the microfiltration membrane tube is internally provided with a temperature controller and a pressure controller, and the outer wall of the microfiltration membrane tube is provided with a heating control button and a pressure control button which are respectively connected to the temperature controller and the pressure controller through corresponding circuits;
the inlet of the ultrafiltration membrane tube is communicated with the outlet of the microfiltration membrane tube, and the outlet of the ultrafiltration membrane tube is communicated with the inlet of the resin exchanger;
the resin exchanger is a layered tube which is connected in sequence, the uppermost layer is a cation exchange resin tube, the middle layer is a strong-base anion exchange resin tube, the lower layer is a weak-base anion exchange resin tube, the ends of the tubes are communicated, and the cation exchange resin tube is connected with the ultrafiltration membrane tube;
the inlet of the nanofiltration membrane pipe is connected with the outlet of the resin exchanger, the inside of the nanofiltration membrane pipe is provided with a temperature controller and a pressure controller, and the outer wall of the nanofiltration membrane pipe is provided with a heating control button and a pressure control button which are respectively connected to the temperature controller and the pressure controller through corresponding circuits.
In a fourth aspect, an embodiment of the present application provides a computer device, which includes a memory, a processor, and a computer program stored in the memory and executable on the processor, where the processor implements the steps of the method when executing the computer program.
In a fifth aspect, the present application provides a computer-readable storage medium, on which a computer program is stored, where the computer program is executed by a processor to perform the steps of the above method.
According to the method for obtaining the aloe flower extracting solution, the aloe flower emulsion and the device provided by the embodiment of the invention, the aloe flower is placed in the extracting tank, and the extracting solvent is added, wherein the extracting solvent is aloe vera leaf water or aloe vera gel juice to obtain the aloe flower crude extracting solution; clarifying the aloe flower crude extract to obtain a clarified crude extract; performing microfiltration separation treatment on the clarified crude extract by using a microfiltration membrane to obtain microfiltration permeating liquid; performing ultrafiltration on the microfiltration permeating liquid by using an ultrafiltration membrane to obtain ultrafiltration permeating liquid; filtering out pigment, salt and acid substances in the ultrafiltration permeate by using exchange resin to obtain an aloe flower extract primary solution; concentrating the primary aloe flower extract by using a nanofiltration membrane to obtain an aloe flower extract. Thus, since the aloe vera leaf water or aloe vera gel juice contains functional components similar to the aloe flower, the components in the aloe flower are more easily dissolved, and the extraction efficiency and purity of the aloe flower can be improved.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a schematic flow chart of a method for obtaining an aloe flower extract according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an apparatus for obtaining an aloe flower extract according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a computer device 300 according to an embodiment of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a method for obtaining aloe flower extract, aloe flower emulsion and a device, and is described by the embodiment.
FIG. 1 is a schematic flow chart of a method for obtaining an aloe flower extract according to an embodiment of the present invention. As shown in fig. 1, the method includes:
in the embodiment of the invention, in order to improve the extraction efficiency, the aloe powder is crushed, sieved and then placed in an extraction tank, and the aloe leaf water or aloe vera gel juice is used as an extraction solvent. In order to fully dissolve the active ingredients in the aloe flower and avoid damaging the active ingredients in the aloe flower by high temperature, as an optional example, the liquid-material ratio of the extraction solvent to the aloe flower is 30 to 1 (v/w), the stirring temperature is 55 to 85 ℃, and the stirring time is 1 to 2 hours. Preferably, it does not exceed 85 ℃.
In the embodiment of the invention, the aloe vera leaf water or the aloe vera gel juice is used as the extraction solvent, and as the main components of the aloe vera leaf water or the aloe vera gel juice are acidic substances such as polysaccharide, organic acid, amino acid, trace elements and the like and contain functional components similar to aloe flowers, the components in the aloe flowers are more easily dissolved, and the extraction efficiency of the aloe flowers is improved; further, the aloe vera leaf water or aloe vera gel juice contains functional ingredients, which can also increase the efficacy of aloe vera flower extract; moreover, the effective components of the extraction solvent are similar to those of aloe flower, and the extract obtained by extracting aloe leaf water or aloe vera gel juice has high purity of 100% of aloe vera flower extract.
In the embodiment of the invention, as an optional embodiment, the pH value of the aloe vera leaf water is 3.5-5.0, the O-acetyl group is 10mg/kg, the conductivity is less than or equal to 50 mu s/cm, the pH value of the aloe vera gel juice is 3.5-5.0, and the O-acetyl group is more than or equal to 375mg/kg.
in the embodiment of the invention, a clarifying agent solution with the concentration of 1-3% is slowly added into the aloe flower crude extract, and the addition amount of the clarifying agent is 6-8% of the amount of aloe vera leaf water or aloe vera gel juice, so that the clarifying effect can be optimal. Adding a clarifying agent, stirring for 5-10 min, stopping stirring, and filtering by using a vibrating screen (80-mesh screen) to obtain a clarified coarse extract. Washing the filter residue in the vibrating screen with aloe barbadensis leaf water, collecting the filtrate, filtering with a plate-and-frame filter, and adding into the clear crude extract.
In the embodiment of the invention, as the aloe flower crude extract also contains a large amount of particle suspended matters and mucilage components, the clarifying pretreatment is carried out by the clarifying agent, so that the efficiency of subsequent separation treatment can be improved, and the solubility of the aloe flower extract and the use of the aloe flower extract in cosmetics can be ensured.
In an embodiment of the present invention, as an alternative embodiment, a clarifier solution for clarifying treatment is prepared by: stirring a small amount of Aloe vera leaf water or Aloe vera gel juice with a clarifier to obtain a paste, adding Aloe vera leaf water or Aloe vera gel juice, stirring and swelling for 12h to obtain the final product.
103, performing microfiltration separation treatment on the clarified crude extract by using a microfiltration membrane to obtain microfiltration permeate;
in the embodiment of the invention, as an optional embodiment, the membrane aperture of the microfiltration membrane is 0.1-0.3 μm. Microfiltration membranes include, but are not limited to: inorganic ceramic membranes, organic microfiltration membranes. For the inorganic ceramic membrane, under a certain temperature range, the higher the temperature is, the higher the dialysate flux and the filtration speed are, which is beneficial to filtration, the inorganic ceramic membrane is high-pressure resistant, and the pressure is beneficial to the dialysate flux, so that the inorganic ceramic membrane is utilized to carry out microfiltration separation treatment at the temperature of 20-90 ℃ and the pressure of 1-5 bar; for organic micro-filtration membrane, the temperature is 20-45 ℃ and the pressure is 2-10 bar. Preferably, the inorganic ceramic membrane is selected as the microfiltration membrane because of the characteristics of acid and alkali resistance, high temperature resistance, large flux, convenient cleaning and the like.
In the embodiment of the invention, the microfiltration membrane has selective permeability, and is used as a separation medium for filtering according to the size of membrane pores. Thus, by performing microfiltration separation treatment on the clarified crude extract, the impurities such as colloid, tannin, protein and the like with relatively large molecular weight in the clarified crude extract can be removed while the active ingredients of the aloe flower are fully reserved.
104, performing ultrafiltration on the microfiltration permeate by using an ultrafiltration membrane to obtain ultrafiltration permeate;
in the embodiment of the invention, as an optional embodiment, the cut-off molecular weight of the ultrafiltration membrane is 6000 to 15000 daltons, preferably 8000 to 12000 daltons, the ultrafiltration temperature is 20 to 45 ℃, and the pressure is 4 to 10bar.
In the embodiment of the invention, the ultrafiltration membrane is used for selectively removing ineffective components such as macromolecular pigments, mucilaginous substances and the like, so that micromolecular active substances such as polyphenol and the like are separated by ultrafiltration.
105, filtering out pigments, salts and acid substances in the ultrafiltration permeate by using exchange resin to obtain an initial aloe flower extract;
in an embodiment of the present invention, as an optional embodiment, the filtering out pigments, salts and acids in the ultrafiltration permeate by using an exchange resin includes:
according to the ultrafiltration permeation liquid: the strong-acid styrene cation exchange resin is 10-20: 1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-50 min to obtain a first extract;
according to the first extracting solution: 10-20% of macroporous strongly basic styrene anion exchange resin: 1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-50 min to obtain a second extracting solution;
according to the second extracting solution: 10-20% of macroporous weakly basic acrylic acid anion exchange resin: 1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-50 min to obtain the initial aloe flower extracting solution.
In the embodiment of the invention, the ultrafiltration permeating liquid is subjected to resin exchange for three times, wherein the first resin exchange is to utilize strong-acid styrene cation exchange resin to perform resin gum exchange so as to remove pigments in the ultrafiltration permeating liquid; the second resin exchange is to use macroporous strongly basic styrene anion exchange resin to carry out resin exchange so as to remove part of salt substances in the ultrafiltration permeate; and the third resin exchange is to use macroporous weak-base acrylic acid anion exchange resin to remove part of acid substances in the ultrafiltration permeate.
And step 106, concentrating the primary aloe flower extract by using a nanofiltration membrane to obtain an aloe flower extract.
In the embodiment of the invention, the primary aloe flower extract is subjected to nanofiltration membrane concentration treatment to obtain the aloe flower extract. In order to improve the flux of the initial liquid of the aloe flower extraction and shorten the concentration period, as an optional embodiment, the concentration temperature is 20-45 ℃ and the pressure is 10-40 bar.
In the embodiment of the invention, the intercepted molecular weight of the nanofiltration membrane is less than or equal to 200 daltons, and the nanofiltration membrane is used for concentration and filtration, so that micromolecular active matters with the molecular weight of more than 200 daltons can be reserved, and redundant water and part of monovalent metal ions can be filtered.
In the embodiment of the invention, the aloe flower extract obtained by extraction through the treatment has the soluble solid content of 3-6%, the total polyphenol retention rate of not less than 75% and the total polyphenol concentration of 800-2500 mg/L.
In the embodiment of the invention, the aloe flower extract is stored for 28 days at the constant temperature of 45 ℃, the total polyphenol content and the soluble solid content are basically stable, and no obvious precipitate is generated.
In the embodiment of the invention, the method for extracting the aloe flower extract through crude extract preparation, clarification, microfiltration membrane precipitation removal, ultrafiltration membrane separation, decoloration and nanofiltration membrane concentration is convenient to operate, low in energy consumption, low in cost, ecological and environment-friendly and suitable for industrial production, the obtained aloe flower extract can furthest retain active substance polyphenol in aloe flowers, macromolecular impurity interference such as vegetative pituit is removed, the precipitate is less, the color is clear, other organic solvent components are not contained, the extracted aloe flower extract is safe and harmless to skin, high in purity, capable of effectively enhancing the stability of the aloe flower extract, and capable of improving the product quality and quality stability of the aloe flower extract, meanwhile, the aloe flower extract has the effects of better antioxidation function, anti-inflammation, allergy relief, irritation resistance, tyrosinase activity inhibition, whitening and skin brightening, and the like, and can be applied to cosmetics such as aging resistance, allergy resistance, whitening, moisturizing, astringency and the like. Wherein the cosmetic includes, but is not limited to: cream, essence, lotion, and aqua.
In the embodiment of the invention, the aloe vera leaf water or the aloe vera gel juice is used as the extraction solvent, compared with the organic solvent such as propylene glycol, the production process is green and environment-friendly, and the amount of the aloe leaves which can be dissolved by the aloe vera leaf water or the aloe vera gel juice is more, so that the extraction efficiency is improved; furthermore, the aloe vera leaf water or aloe vera gel juice contains certain functional components, so that the efficacy of the aloe flower extract can be increased, and the purity of the extracted aloe flower extract is 100% of the aloe effective components; moreover, a membrane with selective permeability is used as a separation medium, under the action of pressure difference, components with different molecular weights are intercepted through membrane pores or membrane pores according to the size of the membrane pore diameter, so that the purposes of separation and concentration are achieved, no phase change exists in the operation process, and no damage is caused to the structure of secondary metabolites of the aloe flower; in addition, the integrated membrane technology of combined application of microfiltration, ultrafiltration and nanofiltration is adopted, so that the color of the aloe flower extract can be obviously improved, the retention rate of total polyphenol in the obtained aloe flower extract is over 75 percent, and the product quality and the quality stability can be effectively improved.
In an embodiment of the present invention, an aloe flower emulsion for cosmetics may be prepared based on the aloe flower extract extracted using the above method, wherein the aloe flower emulsion includes:
caprylic acid, accounting for 5 percent of the total amount;
the shea butter accounts for 2 percent of the total amount;
hydrogenated poly-decene, accounting for 2% of the total amount;
oleic acid erucic acid ester accounting for 2% of the total amount;
cetostearyl alcohol, 2.5% of the total;
glycerol stearate accounting for 1.5 percent of the total amount;
350CST dimethyl silicone oil accounting for 0.5 percent of the total amount;
propyl hydroxybenzoate accounting for 0.1% of the total amount;
TEGO CARE CG 90, accounting for 1.5% of the total amount;
allantoin accounting for 0.2 percent of the total amount;
methyl hydroxybenzoate accounting for 0.2% of the total amount;
glycerol, accounting for 8% of the total amount;
EDTA-2NA, accounting for 0.05% of the total amount;
xanthan gum, accounting for 0.1% of the total amount;
carbomer 940 accounting for 0.35 percent of the total amount;
deionized water, adjusting the total amount to 100%;
triethanolamine, in an appropriate amount;
the aloe flower extract accounts for 3 percent of the total amount;
a proper amount of preservative;
essence and proper amount.
In the embodiment of the invention, the ratio is volume ratio or mass ratio, caprylic acid can be replaced by capric triglyceride, TEGO CARE CG 90 is cetearyl dextran, and triethanolamine is TEA with the concentration of 20%. As an alternative example, the appropriate amount may be an amount of 0.1% or less of the total amount, for example, 0.01%, 0.05%, 0.08, etc.
Example one
(1) Preparation of aloe flower crude extract
Pulverizing 50kg of Aloe Vera powder, sieving, placing into an extraction tank, adding 1700L of Aloe Barbadensis Miller leaf water as extraction solvent, controlling the temperature in the extraction tank at 60 deg.C, and extracting for 2 hr under heat preservation.
(2) Clarifying the crude extract of Aloe flower
Slowly adding 110kg of 1% clarifier solution ZTC IIIA into the crude aloe flower extractive solution, stirring for 5min, filtering with a vibrating screen, washing the filter residue in the screen with appropriate amount of Aloe Barbadensis Miller leaf water, collecting the crude filtrate, and filtering with a plate frame to obtain 1300kg of the crude aloe flower extractive solution.
(3) Microfiltration membrane sedimentation removal
And (3) carrying out microfiltration separation treatment on the clarified extract by adopting an inorganic ceramic membrane with the membrane aperture of 0.1 mu m at the operation temperature of 45 ℃ and the operation pressure of 1bar to obtain microfiltration permeate.
(4) Separation with ultrafiltration membrane
And (3) performing ultrafiltration on the microfiltration permeating liquid by using an ultrafiltration membrane with the molecular weight cutoff of 8000 Dalton, wherein the operating temperature is 20-25 ℃, and the operating pressure is 5bar, so as to obtain 1250kg of ultrafiltration permeating liquid.
(5) Decolorizing
According to the ultrafiltration permeation liquid: the strong-acid styrene cation exchange resin is 15:1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-35 min to obtain a first extracting solution;
according to the first extracting solution: the macroporous strongly basic styrene anion exchange resin is 15:1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-35 min to obtain a second extracting solution;
according to the second extracting solution: the macroporous weakly basic acrylic acid anion exchange resin is 15:1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-35 min to obtain clear initial solution of aloe barbadensis flower extract.
(6) Nanofiltration membrane concentration
Concentrating the aloe flower extractive primary solution with nanofiltration membrane with molecular weight cutoff of 150 daltons, operating at 25 deg.C under 10bar, and concentrating the trapped solution to 1600L to obtain aloe flower extractive solution.
In the embodiment of the invention, the total polyphenol concentration in the feed liquid obtained in the steps (1) to (2) is respectively measured by adopting a forskolin-phenol method, and the absorbance of the feed liquid obtained in the steps (2) to (4) is detected by using an ultraviolet-visible spectrophotometer, and the result is shown in table 1.
In the embodiment of the invention, the coarse aloe flower extract is subjected to clarification pretreatment, the absorbance of a 10% aqueous solution is reduced to 0.769, and then the absorbance is sequentially reduced to 0.623 and 0.472 through microfiltration and ultrafiltration treatment, so that impurities in the coarse aloe flower extract are effectively removed. And after decoloring, reducing the absorbance to 0.385, finally obtaining the aloe flower extract after membrane concentration to be light brown transparent clear solution, measuring the content of soluble solids by using a portable refractometer to be 4.0 percent, wherein the concentration of total polyphenol is 867.5mg/L, and calculating the retention rate of the total polyphenol to be 83.6 percent in the membrane treatment process.
Example two
(1) Preparation of aloe flower crude extract
Pulverizing 50kg of aloe powder, sieving, placing into an extraction tank, adding 1500L of Aloe Barbadensis Miller leaf water as extraction solvent, controlling the temperature in the extraction tank at about 75 deg.C, and extracting for 1 hr under heat preservation.
(2) Clarifying the crude extract of Aloe flower
Slowly adding 112kg of 2% clarifier solution ZTC IIIA into the crude Aloe flower extractive solution, stirring for 10min, filtering with a vibrating screen, washing the filter residue in the screen with appropriate amount of Aloe Barbadensis leaf water, collecting the crude filtrate, and filtering with a plate frame to obtain 1100kg of crude extractive solution filtered with the plate frame.
(3) Microfiltration membrane sedimentation removal
And (3) performing microfiltration separation treatment on the centrifugally separated crude extract by adopting an inorganic ceramic membrane with the membrane aperture of 0.1 mu m, wherein the temperature of the microfiltration separation treatment is 40 ℃, and the pressure is 1bar, so as to obtain microfiltration permeating liquid.
(4) Separation with ultrafiltration membrane
And (3) performing ultrafiltration on the microfiltration permeate by using an ultrafiltration membrane with the molecular weight cutoff of 8000 Dalton, wherein the operating temperature is 20-25 ℃, and the operating pressure is 5bar, so as to obtain 1050kg of ultrafiltration permeate.
(5) Decolorizing
According to the ultrafiltration permeation liquid: strong acid styrene cation exchange resin =12:1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-35 min to obtain a first extract;
according to the first extracting solution: macroporous strongly basic styrene-based anion exchange resin =12:1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-35 min to obtain a second extracting solution;
according to the second extracting solution: macroporous weakly basic acrylic anion exchange resin =12:1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-35 min to obtain clear initial solution of aloe barbadensis flower extract.
(6) Nanofiltration membrane concentration
Concentrating the primary extractive solution of Aloe barbadensis Miller flower with nanofiltration membrane with cut-off molecular weight of 150 daltons at 25 deg.C under 10bar, and concentrating the cut-off solution to 1600L to obtain Aloe flower extractive solution.
In the embodiment of the invention, the total polyphenol concentration in the feed liquid obtained in the steps (1) to (2) is respectively measured by adopting a forskolin-phenol method, and the absorbance of the feed liquid obtained in the steps (2) to (4) is detected by using an ultraviolet-visible spectrophotometer, and the result is shown in table 1.
In the embodiment of the invention, the crude aloe flower extract is subjected to clarification pretreatment, the absorbance of a 10% aqueous solution is reduced to 0.874, then microfiltration and ultrafiltration treatment are carried out, the absorbance is sequentially reduced to 0.706 and 0.536, after decoloration treatment, the absorbance is reduced to 0.436, finally, the aloe flower extract obtained after membrane concentration is a light brown transparent clear solution, the soluble solid content is 5.0% measured by a portable refractometer, the total polyphenol concentration is 1060.4mg/L, and the total polyphenol retention rate in the membrane treatment process is calculated to be 84.7%.
EXAMPLE III
(1) Preparation of aloe flower crude extract
Pulverizing 50kg of Aloe Vera powder, sieving, placing into an extraction tank, adding 1600L of Aloe Barbadensis Miller gel juice as extraction solvent, controlling the temperature in the extraction tank at about 70 deg.C, and extracting for 2 hr under heat preservation.
(2) Clarifying the crude extract of Aloe flower
Slowly adding 95kg of 3% clarifier solution ZTC IIIA into the crude Aloe flower extractive solution, stirring for 10min, filtering with vibrating screen, washing the filter residue with appropriate amount of Aloe Barbadensis Miller gel juice, collecting the crude filtrate, and filtering with plate frame to obtain 1200kg of crude extractive solution filtered with plate frame.
(3) Microfiltration membrane sedimentation removal
And (3) carrying out microfiltration separation on the centrifugally separated crude extract by adopting an inorganic ceramic membrane with the membrane aperture of 0.1 mu m, wherein the operating temperature is 40 ℃, and the operating pressure is 1bar, so as to obtain microfiltration permeating liquid.
(4) Separation with ultrafiltration membrane
And (3) performing ultrafiltration on the microfiltration permeating liquid by using an ultrafiltration membrane with molecular weight cut-off of 8000 Dalton, wherein the operating temperature is 20-25 ℃, and the operating pressure is 5bar, so as to obtain 1130kg of ultrafiltration permeating liquid.
(5) Decolorizing
According to the ultrafiltration permeation liquid: strong acid styrene cation exchange resin =15:1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-35 min to obtain a first extracting solution;
according to the first extracting solution: macroporous strongly basic styrenic anion exchange resin =15:1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-35 min to obtain a second extracting solution;
according to the second extracting solution: macroporous weakly basic acrylic anion exchange resin =15:1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-35 min to obtain clear aloe barbadensis flower primary extracting solution.
(6) Nanofiltration membrane concentration
Concentrating the initial extract of Aloe barbadensis Miller flower with nanofiltration membrane with cut-off molecular weight of 150 daltons at 25 deg.C under 10bar, and concentrating the cut-off solution to 1600L to obtain Aloe flower extractive solution.
In the embodiment of the invention, the total polyphenol concentration in the feed liquid obtained in the steps (1) to (2) is respectively measured by adopting a forskolin-phenol method, and the absorbance of the feed liquid obtained in the steps (2) to (4) is detected by using an ultraviolet-visible spectrophotometer, and the result is shown in table 1.
In the embodiment of the invention, the crude aloe flower extract is subjected to clarification pretreatment, the absorbance of a 10% water solution is reduced to 0.735, then microfiltration and ultrafiltration treatment are carried out, the absorbance is sequentially reduced to 0.633 and 0.503, then decolorization treatment is carried out, the absorbance is reduced to 0.409, finally, the aloe flower extract obtained after membrane concentration is a light brown transparent clear solution, the content of soluble solids is 4.5% by using a portable refractometer, the concentration of total polyphenol is 904.7mg/L, and the retention rate of total polyphenol in the membrane treatment process is calculated to 85.9%.
Table 1 shows the total polyphenol concentration, absorbance (10% aqueous solution), and soluble solid content test results in the aloe flower extract, where in table 1, the total polyphenol concentration is mg/L, and the soluble solid content is%.
Example four
The clarified treated solution, the ultrafiltrate, the decolorized solution and the nanofiltration concentrate obtained in the first example were taken and packaged into 2 parts each of 100g by using a transparent PE bag, and the resulting product was sterilized and then left at a constant temperature of 45 ℃. The appearance of the sample was observed periodically for 1 month, and the results are shown in Table 2.
TABLE 2 stability of Aloe Vera solution obtained by different treatment methods
In Table 2, the feed liquid which is only subjected to clarification treatment but not subjected to microfiltration, ultrafiltration and decoloration is placed at 45 ℃ for 7 days, and then a small amount of precipitate is generated; the decolored feed liquid and the nano-filtered concentrated feed liquid have light color, no precipitate and more stable shape than the undeloured feed liquid.
Fig. 2 is a schematic structural diagram of a device for obtaining an aloe flower extract according to an embodiment of the present invention. As shown in fig. 2, the apparatus includes: a pulverizer 201, an extraction tank 202, a microfiltration membrane pipe 203, an ultrafiltration membrane pipe 204, a resin exchanger 205, and a nanofiltration membrane pipe 206, wherein,
the crusher 201 is positioned above the extraction tank 202, and the outlet of the crusher 201 is communicated with the first inlet of the extraction tank 202;
a solvent tube marked with transparent volume scales is arranged on one side above the extraction tank 202, and a switch is arranged at the lower end of the solvent tube and communicated with the inner cavity of the extraction tank 202 through the switch;
a clarifier solution pipe marked with transparent volume scales is arranged at the other side above the extraction tank 202, and the lower end of the clarifier solution pipe is provided with a switch and is communicated with the inner cavity of the extraction tank 202 through the switch;
a heater is arranged around the bottom of the extraction tank 202, a heating control button is arranged on the side surface of the extraction tank, the heating control button is connected to the heater through a circuit, a graduated scale marked with a transparent volume is arranged from the bottom to the top of the extraction tank, and a stirrer is arranged in an inner cavity of the extraction tank 202;
a coarse extract outlet controlled by a switch is arranged at the center of the bottom of the extraction tank 202, and a vibrating screen is arranged in the middle of the coarse extract outlet;
the microfiltration membrane tube 203 is internally provided with one-stage or multi-stage microfiltration membranes, the inlet of the microfiltration membrane tube is connected to the crude extract outlet of the extraction tank, the microfiltration membrane tube 203 is internally provided with a temperature controller and a pressure controller, and the outer wall of the microfiltration membrane tube 203 is provided with a heating control button and a pressure control button which are respectively connected to the temperature controller and the pressure controller through corresponding circuits;
an inlet of the ultrafiltration membrane pipe 204 is communicated with an outlet of the microfiltration membrane pipe 203, and an outlet is communicated with an inlet of the resin exchanger 205;
the resin exchanger 205 is a layered tube which is connected in sequence, the uppermost layer is a cation exchange resin tube, the middle layer is a strong-base anion exchange resin tube, the lower layer is a weak-base anion exchange resin tube, the ends are communicated, and the cation exchange resin tube is connected to the ultrafiltration membrane tube 204;
the inlet of the nanofiltration membrane pipe 206 is connected to the outlet of the resin exchanger 205, a temperature controller and a pressure controller are arranged in the nanofiltration membrane pipe, and a heating control button and a pressure control button are arranged on the outer wall of the nanofiltration membrane pipe and are respectively connected to the temperature controller and the pressure controller through corresponding circuits.
In the embodiment of the present invention, as an optional embodiment, the microfiltration membrane tube 203 is a double-volume tube with a sealed and isolated middle, and comprises: the micro-liquid tube comprises a micro-liquid tube and a micro-filtration tube, wherein an inlet of the micro-liquid tube is connected to a coarse extract outlet of the extraction tank, a temperature controller and a pressure controller are arranged in the micro-liquid tube, multi-stage openings are formed in the micro-liquid tube at different heights, each opening is provided with a corresponding micro-filtration membrane, and the opening provided with the micro-filtration membrane is communicated with the inlet of the micro-filtration tube after extending.
As shown in fig. 3, an embodiment of the present application provides a computer device 300 for executing the method for obtaining aloe flower extract in fig. 1, the device includes a memory 301, a processor 302 and a computer program stored on the memory 301 and executable on the processor 302, wherein the processor 302 implements the steps of the method for obtaining aloe flower extract when executing the computer program.
Specifically, the memory 301 and the processor 302 can be general-purpose memory and processor, and are not limited in particular, and when the processor 302 runs the computer program stored in the memory 301, the method for obtaining the aloe flower extract can be performed.
Corresponding to the method for obtaining aloe flower extract liquid in fig. 1, the present application further provides a computer readable storage medium, on which a computer program is stored, and the computer program is executed by a processor to perform the steps of the method for obtaining aloe flower extract liquid.
In particular, the storage medium can be a general-purpose storage medium, such as a removable disk, a hard disk, etc., and when the computer program on the storage medium is executed, the method for obtaining the aloe flower extract can be executed.
In the embodiments provided in the present application, it should be understood that the disclosed system and method may be implemented in other ways. The above-described system embodiments are merely illustrative, and for example, the division of the units is only one logical functional division, and there may be other divisions in actual implementation, and for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed mutual coupling or direct coupling or communication connection may be an indirect coupling or communication connection of systems or units through some communication interfaces, and may be in an electrical, mechanical or other form.
The units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, functional units in the embodiments provided in the present application may be integrated into one processing unit, or each unit may exist alone physically, or two or more units are integrated into one unit.
The functions, if implemented in the form of software functional units and sold or used as a stand-alone product, may be stored in a computer readable storage medium. Based on such understanding, the technical solution of the present application or portions thereof that substantially contribute to the prior art may be embodied in the form of a software product stored in a storage medium and including instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method according to the embodiments of the present application. And the aforementioned storage medium includes: various media capable of storing program codes, such as a usb disk, a removable hard disk, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk, or an optical disk.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus once an item is defined in one figure, it need not be further defined and explained in subsequent figures, and moreover, the terms "first", "second", "third", etc. are used merely to distinguish one description from another and are not to be construed as indicating or implying relative importance.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present application, and are used to illustrate the technical solutions of the present application, but not to limit the technical solutions, and the scope of the present application is not limited to the above-mentioned embodiments, although the present application is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: those skilled in the art can still make modifications or changes to the embodiments described in the foregoing embodiments, or make equivalent substitutions for some features, within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present application. Are intended to be covered by the scope of this application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (9)
1. An aloe flower emulsion comprising:
caprylic acid, accounting for 5% of the total amount;
butyrospermum parkii fruit resin accounting for 2 percent of the total amount;
hydrogenated poly-decene, accounting for 2% of the total amount;
oleic acid erucic acid ester accounting for 2% of the total amount;
cetostearyl alcohol, 2.5% of the total;
glycerol stearate accounting for 1.5 percent of the total amount;
350CST dimethyl silicone oil accounting for 0.5 percent of the total amount;
propyl hydroxybenzoate accounting for 0.1% of the total amount;
TEGO CARE CG 90, accounting for 1.5% of the total amount;
allantoin accounting for 0.2 percent of the total amount;
methyl hydroxybenzoate accounting for 0.2% of the total amount;
glycerol accounting for 8% of the total amount;
EDTA-2NA, accounting for 0.05% of the total amount;
xanthan gum, accounting for 0.1% of the total amount;
carbomer 940 accounting for 0.35 percent of the total amount;
deionized water, adjusting the total amount to 100%;
triethanolamine, in an appropriate amount;
the aloe flower extract accounts for 3 percent of the total amount;
a proper amount of preservative;
essence and proper amount.
2. The aloe flower emulsion according to claim 1, wherein the aloe flower extract is obtained by:
placing aloe flower in an extraction tank, adding an extraction solvent, wherein the extraction solvent is aloe vera leaf water or aloe vera gel juice to obtain aloe flower crude extract;
clarifying the aloe flower crude extract to obtain a clarified crude extract;
carrying out microfiltration separation treatment on the clarified crude extract by using a microfiltration membrane to obtain microfiltration permeate;
performing ultrafiltration on the microfiltration permeate by using an ultrafiltration membrane to obtain ultrafiltration permeate;
filtering out pigment, salt and acid substances in the ultrafiltration permeate by using exchange resin to obtain an aloe flower extract primary solution;
concentrating the initial aloe flower extractive solution with nanofiltration membrane to obtain aloe flower extractive solution.
3. The aloe flower emulsion according to claim 2, wherein the liquid-to-material ratio of the extraction solvent to the aloe flower is 30-35 (v/w), the stirring temperature is 55-85 ℃, and the stirring time is 1-2 hours.
4. The aloe flower emulsion according to claim 2, wherein the aloe vera leaf water has a pH of 3.5-5.0, an O-acetyl group of 10mg/kg, a conductivity of less than or equal to 50 μ s/cm, the aloe vera gel juice has a pH of 3.5-5.0, an O-acetyl group of greater than or equal to 375mg/kg.
5. The aloe flower emulsion according to claim 2, wherein the clarifying agent solution is 1-3% in concentration and 6-8% in addition to the amount of aloe vera leaf water or aloe vera gel juice.
6. The aloe flower emulsion according to claim 5, wherein the clarifying agent solution is obtained by stirring a small amount of aloe vera leaf water or aloe vera gel juice to form a paste, adding the aloe vera leaf water or aloe vera gel juice, and stirring for swelling for 12 hours.
7. The aloe flower emulsion according to claim 2, wherein the membrane pore size of the microfiltration membrane is 0.1 to 0.3 μm.
8. The aloe flower emulsion of claim 7, wherein the microfiltration membrane comprises: inorganic ceramic membranes, organic microfiltration membranes.
9. The aloe flower emulsion according to any one of claims 1 to 8, wherein the filtering of the pigments, salts and acids from the ultrafiltration permeate by means of an exchange resin comprises:
according to the ultrafiltration permeation liquid: the strong-acid styrene cation exchange resin is 10-20: 1, passing the ultrafiltration permeate through strong-acid styrene cation exchange resin, and controlling the contact time for 25-50 min to obtain a first extract;
according to the first extracting solution: 10-20 parts of macroporous strongly basic styrene anion exchange resin: 1, passing the first extracting solution through macroporous strongly basic styrene anion exchange resin, and controlling the contact time for 25-50 min to obtain a second extracting solution;
according to the second extracting solution: 10-20% of macroporous weakly basic acrylic acid anion exchange resin: 1, passing the second extracting solution through macroporous alkalescent acrylic acid anion exchange resin, and controlling the contact time for 25-50 min to obtain the initial aloe flower extracting solution.
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| CN108635301A (en) * | 2018-07-25 | 2018-10-12 | 云南万绿生物股份有限公司 | A kind of aloe flower extract and preparation method thereof |
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