CN110917238A - Millettia speciosa champ total-component extract and preparation method and application thereof - Google Patents
Millettia speciosa champ total-component extract and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a beautiful millettia root full-ingredient extract and a preparation method and application thereof, wherein the preparation method of the beautiful millettia root extract comprises the following steps: providing a beautiful millettia root raw material; crushing the beautiful millettia root raw material to obtain a beautiful millettia root crushed material; mixing the radix millettiae speciosae crushed material with water, emulsifying, stirring and cutting to obtain radix millettiae speciosae homogenate; carrying out solid-liquid separation on the millettia speciosa champ homogenate liquid to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag; mixing the millettia speciosa champ separation residues with an alcohol water solution, and extracting by adopting a low-temperature high-pressure-difference continuous extraction technology to obtain the millettia speciosa champ alcohol solution; the beautiful millettia root separating liquid and the beautiful millettia root alcohol solution are the beautiful millettia root extract. The preparation method of the beautiful millettia root extract can fully ensure the content of the effective components in the extract and realize standardized production.
Description
Technical Field
The invention relates to the technical field of natural plant extraction, in particular to a beautiful millettia root full-ingredient extract and a preparation method and application thereof.
Background
Beautiful MiLLettia root, also known as eriosema chinense, bellflower root and the like, is a dry root tuber of Millettia (Millettia speciosa champ) of Millettia of Leguminosae, is mainly distributed in Guangdong, Guangxi, Hainan, Yunnan and other places in China, is widely applied in two broad areas, is a famous plant for both medicine and food in the Lingnan area, and is commonly used as a raw material for making soup, medicated food, medicinal liquor and the like. According to the traditional Chinese medicine, the beautiful millettia root has sweet and mild nature and flavor, enters lung and kidney channels, and has the effects of tonifying deficiency, moistening lung, and strengthening tendons and activating collaterals. The research at home and abroad finds that the beautiful millettia root contains various chemical components such as triterpenoids, flavonoids, polysaccharides, phytosterol and the like, has the effects of protecting the liver, enhancing the immunity, resisting fatigue, eliminating phlegm and relieving cough and the like, is a plant resource with a certain health-care effect, and is worthy of deep research and wide popularization. Along with the endangered extinction of wild beautiful millettia root, the industrialized development of the beautiful millettia root can meet the market demand, so the research of a process route for efficiently extracting the functional components of the beautiful millettia root is urgent.
At present, beautiful millettia root is often used as soup cooking and health care wine in folks, the industrial beautiful millettia root extraction process usually adopts an extraction mode of high energy consumption and low efficiency of thermal reflux, and the laboratory research beautiful millettia root extraction process usually adopts an ultrasonic and thermal reflux mode, so that the traditional extraction modes are long in time consumption, high in energy consumption and low in extraction rate, and the development of related functional products of beautiful millettia root is limited. Therefore, the development of a preparation method of the beautiful millettia root extract, which can fully ensure the content of the effective components in the extract and can realize standardized production, is urgently needed.
Disclosure of Invention
Therefore, the full-ingredient extract of the beautiful millettia root, the preparation method and the application thereof are needed to be provided. The preparation method of the beautiful millettia root extract can fully ensure the content of the effective components in the extract and realize standardized production.
A preparation method of a beautiful millettia root extract comprises the following steps:
providing a beautiful millettia root raw material;
crushing the beautiful millettia root raw material to obtain a beautiful millettia root crushed material;
mixing the beautiful millettia root crushed material with water, emulsifying, stirring and cutting to obtain beautiful millettia root homogenate;
carrying out solid-liquid separation on the millettia speciosa champ homogenate liquid to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag;
mixing the millettia speciosa champ separation residues with an alcohol water solution, and extracting by adopting a low-temperature high-pressure-difference continuous extraction technology to obtain a millettia speciosa champ alcohol solution;
the beautiful millettia root separating solution and the beautiful millettia root alcoholic solution are the beautiful millettia root extract.
In one embodiment, the step of crushing the beautiful millettia root raw material to obtain the beautiful millettia root crushed material comprises the following steps:
crushing the beautiful millettia root raw material for the first time to obtain a first crushed object;
mixing the first crushed material with water according to the mass ratio of 1 (4-10) to obtain first fine crushed pulp and first fine crushed slag deposited at the bottom of the water;
adding water into the first fine crushed slag to perform secondary crushing to obtain second fine crushed pulp and second fine crushed slag precipitated at the bottom of the water;
circulating for n times to obtain n-th fine slurry, wherein n is an integer greater than or equal to 1;
and combining the fine crushed pulp obtained in each step to obtain the beautiful millettia root crushed material.
In one embodiment, in the step of mixing the millettia speciosa champ crushed material with water and performing emulsification and stirring cutting, the mass ratio of the millettia speciosa champ raw material to the water is 1: (10-17);
the circulating pressure of the emulsification and stirring cutting is 0.1-0.2 Mpa.
In one embodiment, the separation is performed by centrifugation at 3800-.
In one embodiment, the extraction step is carried out by adopting a low-temperature high-pressure-difference continuous extraction technology, wherein the extraction temperature is 5-45 ℃, and the extraction pressure is 20-60 MPa.
In one embodiment, the mass ratio of the beautiful millettia root separation residue to the alcohol-water solution is 1: (8-15); the alcohol aqueous solution is an ethanol aqueous solution, wherein the volume percentage content of ethanol is 50-60%.
In one embodiment, after the step of obtaining the beautiful millettia root alcohol solution and/or the beautiful millettia root separation solution, the method further comprises the step of performing microfiltration on the beautiful millettia root alcohol solution and/or the beautiful millettia root separation solution by using a microfiltration membrane with the size of 300nm-600 nm.
In one embodiment, the step of obtaining the solution and/or the separated liquid of beautiful millettia root further comprises the following steps:
concentrating the beautiful millettia root alcohol solution by adopting a reverse osmosis concentration method to obtain a beautiful millettia root alcohol extract with the solid content of 5-20 percent; and/or
Concentrating the beautiful millettia root separating solution by adopting a reverse osmosis concentration method to obtain a beautiful millettia root water extract with the solid content of 5-20%.
In one embodiment, the obtaining of the beautiful millettia root extract further comprises the following steps:
performing sterilization by adopting a plate-frame filtration and/or instantaneous high-temperature sterilization method;
and filling by adopting a hot filling method.
The beautiful millettia root extract prepared by the preparation method.
The application of the beautiful millettia root extract in preparing drinks, foods or medicines.
The preparation method of the beautiful millettia root extract innovatively adopts the emulsification and stirring cutting method to carry out emulsification and homogenization, realizes the fine shearing of beautiful millettia root fibers, and then adopts the low-temperature high-pressure-difference continuous extraction technology to extract centrifugal slag, so that the centrifugal slag penetrates into the interior of the material to be crushed and extracted, and the extraction rate of effective components is greatly improved. And the combination of the two methods not only can greatly improve the extraction rate of active ingredients in the beautiful millettia root raw material, but also can be carried out at normal temperature, so that effective substances in the raw material are greatly reserved, and an important guarantee is provided for the development of subsequent functional products of the beautiful millettia root.
In addition, the preparation method of the beautiful millettia root extract adopts proper solvents according to a specific extraction method, and enriches different polar components in sections, so that the beautiful millettia root full-component extract can be obtained, compared with the traditional method, the component types in the extract are expanded, and raw materials with good flavor and good effect are provided for the development of beautiful millettia root related products. And the method has simple operation of each step, controllable process, and capability of realizing standardized production and being beneficial to the quality control of industrial production.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The preparation method of the beautiful millettia root extract comprises the following steps:
s101: provides a beautiful millettia root raw material.
Understandably, the beautiful millettia root raw material comprises fresh plants and also comprises treated Chinese herbal medicines. And the step S101 may further include a pretreatment step such as washing, slicing, etc., which should be understood to be within the scope of the present invention. For example: the beautiful millettia root raw material can be cut into about 0.5-2cm in advance, so as to be beneficial to the subsequent steps.
S102: crushing the beautiful millettia root raw material to obtain a beautiful millettia root crushed material.
The pulverization can be carried out by a conventional method, and is not particularly limited herein; further, preferably, the ground millettia speciosa champ is sieved by a sieve with the diameter of 1mm-2 mm; further, it is preferable to pass the ground Millettia speciosa champ through a sieve of 1.2 mm. Still further, step S102 preferably includes the steps of:
s1021: crushing a beautiful millettia root raw material for the first time to obtain a first crushed object;
s1022: mixing the first crushed material with water according to the mass ratio of 1 (4-10) to obtain first fine crushed pulp and first fine crushed slag deposited at the bottom of the water;
s1023: adding water into the first fine crushed slag to perform secondary crushing to obtain second fine crushed pulp and second fine crushed slag;
s1024: and (3) circulating for n times to obtain n-th fine crushed slurry, wherein n is an integer greater than or equal to 1, and combining the fine crushed slurry obtained in each step to obtain the beautiful millettia root crushed material.
It can be understood that when n is 1, the first crushed material is subjected to primary crushing to obtain first fine crushed pulp and first fine crushed slag, and the first fine crushed pulp is collected to be the beautiful millettia root crushed material; when n is 2, the first crushed material is crushed twice, namely, the first crushed material is firstly crushed for the first time to obtain first fine crushed pulp and first fine crushed slag, then the second fine crushed slag is crushed by adding water to obtain first fine crushed pulp and second fine crushed slag, and the first fine crushed pulp and the second fine crushed pulp are combined to obtain the beautiful millettia root crushed material; when n is 3, the first pulverized material is pulverized three times, and the specific operation is as described above and will not be described herein again. In one embodiment, n is 1 or 2.
Through carrying out primary crushing with beautiful millettia root raw materials earlier, then mix first crushing thing and the water of specific mass ratio, so, the less fine crushing thing suspension of particle diameter in aqueous, and the great raw materials of particle diameter (promptly beautiful millettia root fine crushing sediment) is settled down, so circulate, can reduce and smash the degree of difficulty, practice thrift the energy consumption.
S103, mixing the radix millettiae speciosae crushed material with water, emulsifying, stirring and cutting to obtain radix millettiae speciosae homogenate.
Through a large number of experiments, technicians of the invention find that the emulsifying, stirring and cutting method is firstly adopted for emulsifying and homogenizing, so that the fibers of the beautiful millettia root are refined, the water extraction effect can be enhanced, and the emulsifying, stirring and cutting are carried out at normal temperature, so that the inactivation of active components caused by high-temperature extraction can be effectively avoided, and the obtained extract is ensured to be rich and comprehensive in nutritional components.
Further, the mass ratio of the beautiful millettia root raw material to the water is 1: (10-17). It can be understood that when the pulverization is performed by the steps S1021 to S1024, the obtained fine pulverized millettia speciosa champ pulp contains water, and then the corresponding water can be continuously added on the basis.
Furthermore, the circulating pressure of the emulsification and stirring cutting is 0.1-0.2Mpa, so as to improve the content of active components in the millettia speciosa champ homogenate.
S104, carrying out solid-liquid separation on the millettia speciosa champ homogenate liquid to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag.
The separation can be carried out using existing centrifuges, such as horizontal centrifuges, tubular centrifuges, or a combination of both. Further, it is preferable to centrifuge the Millettia speciosa homogenate at 3800-.
S105: mixing the millettia speciosa champ separation residues with an alcohol water solution, and extracting by adopting a low-temperature high-pressure-difference continuous extraction technology to obtain the millettia speciosa champ alcohol solution.
The millettia speciosa champ separation residue is further extracted by adopting a low-temperature high-pressure-difference continuous extraction technology, and an alcohol-water solvent is adopted, so that active components with poor water solubility can be extracted, residual water-soluble components in centrifugal residues can be further extracted, and the millettia speciosa champ extract with comprehensive nutritional components can be obtained. Compared with the traditional heating reflux method, the low-temperature high-pressure difference continuous extraction technology can greatly reduce the inactivation of active components caused by high-temperature decoction, is a process of instantly transmitting pressure under the action of a liquid medium, and can be acted by consistent pressure no matter whether extracted is liquid or solid. And only non-covalent bonds can be affected under the pressure, but covalent bonds are not affected, so that the effective components are not damaged, and the content of active components in the beautiful millettia root extract is further improved.
Wherein, the low-temperature high-pressure difference continuous extractor can adopt the existing devices, such as: the device disclosed in zl200920304058.x, is not particularly limited herein.
Further, the mass ratio of the beautiful millettia root separation residue to the alcohol aqueous solution in the step S105 is 1: (8-15); further, the aqueous alcohol solution is an aqueous ethanol solution; furthermore, the alcohol water solution is 50-60% of alcohol solution by volume percentage; further, the alcohol aqueous solution is 55% by volume of an ethanol solution.
Further, in step S105, the extraction temperature is 5-45 ℃ and the extraction pressure is 20-60 MPa.
The beautiful millettia root separating solution obtained in the step S104 and the beautiful millettia root alcohol solution obtained in the step S105 are the needed beautiful millettia root extract. It is understood that the following steps S106-S108 can also be optionally performed according to the requirements of the dosage form and the like.
S106: and (3) carrying out microfiltration on the millettia speciosa champ alcohol solution and/or the millettia speciosa champ separation solution.
In particular, microfiltration is preferably performed by adopting a microfiltration membrane with the particle size of 300nm-600nm so as to improve the mouthfeel of the final product.
It is understood that the millettia speciosa champ alcohol solution and the millettia speciosa champ separation solution can be mixed and then treated, and can also be treated respectively, and are understood to be in the protection scope of the present invention.
S107: concentrating the millettia speciosa champ alcohol solution and/or the millettia speciosa champ separated solution to obtain the millettia speciosa champ alcohol extract and/or the millettia speciosa champ water extract.
Further, in step S107, the low-temperature vacuum concentration is preferably performed by a reverse osmosis concentration method, which can reduce the concentration temperature (65 ℃ C.) and avoid the inactivation of active components. Further, the temperature in the concentration step is less than or equal to 65 ℃; further, the reverse osmosis concentration in the step S107 is carried out at a temperature of 20 ℃ to 35 ℃ and the vacuum concentration is carried out at a temperature of 40 ℃ to 65 ℃.
It is understood that the millettia speciosa champ alcohol solution and the millettia speciosa champ separation solution can be mixed and then treated, and can also be treated respectively, and are understood to be in the protection scope of the present invention.
Further, concentrating the beautiful millettia root alcohol solution by adopting a reverse osmosis concentration method to obtain a beautiful millettia root alcohol extract with the solid content of 5-20 percent; and/or
Concentrating the beautiful millettia root separating solution by adopting a reverse osmosis concentration method to obtain a beautiful millettia root water extract with the solid content of 5-20 percent.
And S108, sterilizing and subpackaging.
Preferably, the sterilization is carried out by adopting a plate-frame filtration and/or instantaneous high-temperature sterilization method, the filling is carried out by adopting a hot filling method so as to further ensure the microbial qualification of the product, and the sterilization and the sub-packaging of the product are preferably carried out in a universal crystallization area so as to fully ensure the microbial qualification of the product.
The preparation method of the beautiful millettia root extract innovatively adopts the emulsification and stirring cutting method to carry out emulsification and homogenization, realizes the fine shearing of beautiful millettia root fibers, and then adopts the low-temperature high-pressure-difference continuous extraction technology to extract centrifugal slag, so that the centrifugal slag penetrates into the interior of the material to be crushed and extracted, and the extraction rate of effective components is greatly improved. And the combination of the two methods not only can greatly improve the extraction rate of active ingredients in the beautiful millettia root raw material, but also can be carried out at normal temperature, so that effective substances in the raw material are greatly reserved, and an important guarantee is provided for the development of subsequent functional products of the beautiful millettia root.
In addition, the preparation method of the beautiful millettia root extract adopts proper solvents according to a specific extraction method, and enriches different polar components in sections, so that the beautiful millettia root full-component extract can be obtained, compared with the traditional method, the component types in the extract are expanded, and raw materials with good flavor and good effect are provided for the development of beautiful millettia root related products. And the method has simple operation of each step, controllable process, and capability of realizing standardized production and being beneficial to the quality control of industrial production.
The present invention will be described below with reference to specific examples.
The following examples used the main equipment: traditional Chinese medicine slicing machine, high-efficiency turbine pulverizer, high-speed emulsifying equipment, stirring and mixing tank, and low-temperature high-pressure-difference continuous extractor (the specific structure is shown in ZL200920304058. X).
The main raw materials are as follows: fresh beautiful millettia root
Example 1
(1) Pretreatment of raw materials: cleaning fresh beautiful millettia root raw materials (sand washing away), and slicing (the diameter is about 0.5-2 cm) to obtain beautiful millettia root fine fragments;
(2) and (3) wet grinding: weighing a proper amount of beautiful millettia root fine crushed products, adding a certain amount (7 times) of purified water, and crushing for 2 times to obtain beautiful millettia root fine crushed pulp and beautiful millettia root fine crushed slag;
(3) emulsification (water extraction): adding water to the fine millettia speciosa champ pulp obtained in the step (2) to complement the amount of the fine millettia speciosa champ pulp to be 10 times of the extraction amount, carrying out high-speed stirring and cutting in an emulsification and homogenate tank, and collecting the millettia speciosa champ homogenate;
(4) centrifuging: centrifuging the millettia speciosa champ homogenate liquid obtained in the step (3) at the rotating speed of 3800r/min to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag;
(5) high-efficiency continuous extraction with high differential pressure and body temperature: adding 55% ethanol in a certain amount (10 times) into the millettia speciosa champ separation residue obtained in the step (4), carrying out high-efficiency high-pressure-difference low-temperature continuous extraction under the conditions of pressure of 25Mpa and temperature of 30 ℃, and centrifuging to obtain millettia speciosa champ alcohol solution;
(6) and (3) microfiltration: respectively carrying out microfiltration (membrane concentration/vacuum concentration (60 ℃) on the millettia speciosa champ separating solution obtained in the step (4) and the millettia speciosa champ alcohol solution obtained in the step (5) by adopting a microfiltration membrane of 500 nm;
(7) concentration and sterilization: respectively carrying out membrane concentration, vacuum concentration and plate-and-frame filtration on the millettia speciosa champ separation solution and the millettia speciosa champ alcohol solution subjected to microfiltration treatment in the step (6) to respectively obtain a millettia speciosa champ alcohol extract and a millettia speciosa champ water extract, and carrying out combined extraction on the millettia speciosa champ alcohol extract and the millettia speciosa champ water extract to prepare a millettia speci;
(8) subpackaging: filling the two parts of the bovine hero extract subjected to plate-and-frame filtration sterilization in a universal clean area.
Example 2
(1) Pretreatment of raw materials: cleaning fresh beautiful millettia root raw materials (sand washing away), and slicing (the diameter is about 0.5-2 cm) to obtain beautiful millettia root fine fragments;
(2) and (3) wet grinding: weighing a proper amount of beautiful millettia root fine crushed products, adding purified water with a certain amount (7 times) of the amount, and crushing to obtain beautiful millettia root fine crushed pulp and beautiful millettia root fine crushed slag;
(3) emulsification (water extraction): adding water to the fine millettia speciosa champ pulp obtained in the step (2) to complement the amount of the fine millettia speciosa champ pulp to be 3 times of the amount of the fine millettia speciosa champ pulp, stirring and cutting the fine millettia speciosa champ pulp in an emulsification and homogenization tank at a high speed, and collecting the fine millettia speci;
(4) centrifuging: centrifuging the millettia speciosa champ homogenate liquid obtained in the step (3) at the rotating speed of 3800r/min to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag;
(5) high-efficiency continuous extraction with high differential pressure and body temperature: adding 55% ethanol in a certain amount (8 times) to the millettia speciosa champ separation residue obtained in the step (4), carrying out high-efficiency high-pressure-difference low-temperature continuous extraction under the conditions of pressure of 25Mpa and temperature of 30 ℃, and centrifuging to obtain millettia speciosa champ alcohol solution;
(6) and (3) microfiltration: respectively carrying out microfiltration (membrane concentration/vacuum concentration (60 ℃) on the millettia speciosa champ separating solution obtained in the step (4) and the millettia speciosa champ alcohol solution obtained in the step (5) by adopting a microfiltration membrane of 500 nm;
(7) concentration, sterilization: respectively carrying out membrane concentration, vacuum concentration and plate-and-frame filtration on the millettia speciosa champ separation solution and the millettia speciosa champ alcohol solution subjected to microfiltration treatment in the step (6) in sequence to respectively obtain a millettia speciosa champ alcohol extract and a millettia speciosa champ water extract, and carrying out combined extraction on the millettia speciosa champ alcohol extract and the millettia speciosa champ water extract to prepare a millett;
(8) subpackaging: filling the two parts of the bovine hero extract subjected to plate-and-frame filtration sterilization in a universal clean area.
Comparative example 1
The comparative example omits the step of emulsification, stirring and cutting, and directly adopts water as an extraction medium to carry out high-efficiency high-pressure-difference low-temperature extraction; specifically, the method comprises the following steps:
(1) pretreatment of raw materials: cleaning fresh beautiful millettia root raw materials (sand washing away), and slicing (the diameter is about 0.5-2 cm) to obtain beautiful millettia root fine fragments;
(2) and (3) wet grinding: weighing a proper amount of beautiful millettia root fine crushed products, adding purified water with a certain amount (7 times) of the amount of beautiful millettia root fine crushed products, and crushing to obtain beautiful millettia root fine crushed pulp and fine crushed slag;
(3) low-temperature high-pressure-difference continuous extraction: adding water to the fine millettia speciosa champ pulp obtained in the step (2) to complement to a certain amount (3 times), carrying out high-efficiency high-pressure-difference low-temperature continuous extraction under the conditions of pressure of 25Mpa and temperature of 30 ℃, and centrifuging to obtain a millettia speciosa champ separation liquid and millettia speciosa champ separation slag; adding a certain amount (8 times) of purified water into the millettia speciosa champ separated slag obtained in the step (3), continuously extracting at low temperature under high pressure difference under the same condition, and centrifuging to obtain millettia speciosa champ aqueous solution
(4) And (3) microfiltration: carrying out microfiltration (membrane concentration/vacuum concentration (60 ℃) on the millettia speciosa champ aqueous solution (separation solution and aqueous solution are combined) obtained in the step (3) by adopting a microfiltration membrane of 500 nm;
(5) concentration, drying and sterilization: respectively carrying out membrane concentration, vacuum concentration and plate-and-frame filtration on the millettia speciosa champ aqueous solution subjected to microfiltration treatment in the step (4) to respectively obtain millettia speciosa champ aqueous extracts;
(6) subpackaging: and (3) filling the millettia speciosa champ aqueous extract subjected to plate-and-frame filtration sterilization in a universal clean area.
Comparative example 2
In the comparative example, water is used as a medium, and a traditional hot reflux extraction method is adopted for extraction, specifically:
(1) pretreatment of raw materials: cleaning fresh beautiful millettia root raw materials (sand washing away), and slicing (the diameter is about 0.5-2 cm) to obtain beautiful millettia root fine fragments;
(2) traditional heating extraction: weighing a proper amount of beautiful millettia root fine crushed products and a certain amount (10 times) of purified water into an extraction tank, and heating and refluxing for 1h for extraction to obtain a beautiful millettia root primary water extract and extraction residues;
(3) centrifuging: centrifuging the Millettia speciosa champ water extract obtained in the step (2) at the rotating speed of 3800r/min to obtain a Millettia speciosa champ primary water solution separation solution;
(4) secondary thermal reflux: adding a certain amount (8 times) of purified water into the extraction residue obtained in the step (2), heating and refluxing for 1h for extraction, and centrifuging to obtain a secondary water extract of the beautiful millettia root;
(5) and (3) microfiltration: combining the primary millettia speciosa champ water extract obtained in the step (3) and the secondary millettia speciosa champ water extract obtained in the step (4) by adopting a microfiltration membrane of 500nm, and then carrying out microfiltration (membrane concentration/vacuum concentration (60 ℃);
(6) concentration and sterilization: respectively sequentially carrying out membrane concentration, vacuum concentration and plate-and-frame filtration on the millettia speciosa champ aqueous solution subjected to microfiltration treatment in the step (5) to obtain the millettia speciosa champ aqueous extract;
(7) subpackaging: and (3) filling the millettia speciosa champ aqueous extract subjected to plate-and-frame filtration sterilization in a universal clean area.
Comparative example 3
The comparative example uses water as an extraction medium, and adopts an emulsification and high-efficiency high-pressure-difference low-temperature combined extraction method for extraction, and specifically comprises the following steps:
(1) pretreatment of raw materials: cleaning fresh beautiful millettia root raw materials (sand washing away), and slicing (the diameter is about 0.5-2 cm) to obtain beautiful millettia root fine fragments;
(2) and (3) wet grinding: weighing a proper amount of beautiful millettia root fine crushed products, adding a certain amount (7 times) of purified water, and crushing twice to obtain beautiful millettia root fine crushed pulp and beautiful millettia root fine crushed slag;
(3) emulsification (water extraction): adding water to the fine millettia speciosa champ pulp obtained in the step (2) to complement the amount of the fine millettia speciosa champ pulp to be 3 times of the amount of the fine millettia speciosa champ pulp, stirring and cutting the fine millettia speciosa champ pulp in an emulsification and homogenization tank at a high speed, and collecting the fine millettia speci;
(4) centrifuging: centrifuging the millettia speciosa champ homogenate liquid obtained in the step (3) at the rotating speed of 3800r/min to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag;
(5) high-efficiency continuous extraction with high differential pressure and body temperature: adding a certain amount (8 times) of purified water into the millettia speciosa champ separation residue obtained in the step (4), carrying out high-efficiency high-pressure-difference low-temperature continuous extraction under the conditions of pressure of 25Mpa and temperature of 30 ℃, and centrifuging to obtain a millettia speciosa champ aqueous solution;
(6) and (3) microfiltration: combining the Millettia speciosa champ separation liquid obtained in the step (4) and the Millettia speciosa champ aqueous solution obtained in the step (5) by adopting a microfiltration membrane of 500nm, and then carrying out microfiltration (membrane concentration/vacuum concentration (60 ℃);
(7) concentration and sterilization: respectively carrying out membrane concentration, vacuum concentration and plate-and-frame filtration on the Millettia speciosa champ separation solution and the Millettia speciosa champ alcohol solution subjected to microfiltration treatment in the step (6) in sequence to obtain a Millettia speciosa champ aqueous extract;
(8) subpackaging: and (3) filling the bovine heroic extract subjected to plate-and-frame filtration sterilization in a universal clean area.
Effect testing experiment
The beautiful millettia root extracts of example 1 and comparative examples 1 to 2 were measured for polysaccharide extraction rate, index component content, and microbial condition, and the test results are shown in table 1 below;
the polysaccharide determination method comprises the following steps:
(1) sample preparation
Precisely weighing 2g of the sample in a 100mL triangular flask, adding 25mL of water, refluxing in boiling water for 2h, cooling to room temperature, and supplementing water. Shaking up, filtering to obtain continuous filtrate) and taking 5mL of continuous filtrate, adding 10mL of absolute ethyl alcohol into a 50mL centrifuge tube, mixing uniformly, centrifuging for 20min in a 4000r/min centrifuge, discarding the supernatant, adding 10mL of 80% ethanol, centrifuging for 20min, discarding the supernatant, adding 10mL of 80% ethanol, centrifuging for 20min, discarding the supernatant, diluting the residue to 10mL with water to constant volume, and shaking up to obtain the final product.
(2) Preparation of Standard Curve
Accurately sucking 100mg/L standard glucose solution 0, 0.30, 0.90, 1.20 and 1.50mL (equivalent to glucose 0, 0.03, 0.06, 0.09, 0.12 and 0.15mg) respectively and placing in a 25mL colorimetric tube, accurately supplementing water to 2.0mL by using a liquid transfer gun, adding 1mL of 5% phenol, uniformly mixing on a rotary mixer, carefully adding 10mL of concentrated sulfuric acid, carefully mixing on the rotary mixer, boiling in a boiling water bath for 2min, taking out cold water for cooling for 2min, using a spectrophotometer at 485nm wavelength and taking a reagent blank solution as a reference, and measuring an absorbance value by using a 1cm cuvette. And drawing a standard curve by taking the glucose concentration as an abscissa and the absorbance value as an ordinate.
(3) Measurement of
Precisely measuring 2mL of the preparation solution into a 25mL colorimetric tube, adding 1mL of 5% phenol, adding 10mL of concentrated sulfuric acid, uniformly mixing, carrying out water bath for 2min, cooling to room temperature with cold water, carrying out blank with a concomitant reagent, and measuring the light absorption value within half an hour.
The testing method of the index components comprises the following steps:
(1) the preparation conditions of the beautiful millettia root raw material test solution are as follows: adding 50% ethanol 1:10 times, ultrasonic extracting for 40min, volatilizing solvent, adding 2mL 50% ethanol for redissolving to obtain test solution;
(2) the method for measuring the content of beautiful sophora japonica essence in beautiful millettia root comprises the following steps:
the method for measuring the content of the Korean sophoricoside comprises the following steps: mobile phase: acetonitrile-water (0-10min, 15% acetonitrile; 10-25min, 15-45% acetonitrile; 25-40min, 45% acetonitrile), flow rate: 1.0mL/min, detection wavelength of 309nm (optimal wavelength of Korean sophoricine), column temperature: 35 deg.C
Method for measuring microbiological conditions: reference to non-sterile product microbial limit check: the microorganism counting method and the bacteria control inspection method (1105-1106 standard in the Chinese pharmacopoeia 2015).
TABLE 1
| Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Polysaccharide extraction ratio/%) | 62.45 | 34.01 | 54.27 | 65.18 |
| Percent of Korean sophoricone extraction | 35 | 0 | 0 | 0 |
| Microorganisms | Qualified | Qualified | Qualified | Qualified |
From the polysaccharide extraction rates in table 1, the polysaccharide extraction rate of comparative example 1, in which the emulsification and agitation cutting steps are omitted and the low-temperature high-pressure-difference continuous extraction method is directly used for extraction, is much lower than that of example 1, and the polysaccharide extraction rate of comparative example 2, in which the conventional thermal reflux is used, is also lower than that of example 1, which shows that the combination of emulsification and agitation cutting and the low-temperature high-pressure-difference continuous extraction method can improve the polysaccharide extraction rate. From the extraction rates of the robinin in table 1, the robinin component (flavonoid component) was not significantly extracted in any of the three extraction methods of comparative example 1, comparative example 2, and comparative example 3.
In addition, in the table, the embodiment 1 and the comparative example 3 are both high-efficiency high-pressure-difference low-temperature continuous extraction after emulsification, but the extraction media of the two are different, and as can be seen from the table 1, the extraction rate of the polysaccharides obtained by combining pure water with ethanol with a certain concentration is reduced by 2% -4%, while the content of the kukoff base is obviously increased, which indicates that the method can obtain the beautiful millettia root extract with rich active components and higher content.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the beautiful millettia root extract is characterized by comprising the following steps:
providing a beautiful millettia root raw material;
crushing the beautiful millettia root raw material to obtain a beautiful millettia root crushed material;
mixing the beautiful millettia root crushed material with water, emulsifying, stirring and cutting to obtain beautiful millettia root homogenate;
carrying out solid-liquid separation on the millettia speciosa champ homogenate liquid to obtain millettia speciosa champ separation liquid and millettia speciosa champ separation slag;
mixing the millettia speciosa champ separation residues with an alcohol water solution, and extracting by adopting a low-temperature high-pressure-difference continuous extraction technology to obtain a millettia speciosa champ alcohol solution;
the beautiful millettia root separating solution and the beautiful millettia root alcoholic solution are the beautiful millettia root extract.
2. The method according to claim 1, wherein the step of pulverizing the Millettia speciosa champ raw material to obtain a Millettia speciosa champ pulverized material comprises the steps of:
crushing the beautiful millettia root raw material for the first time to obtain a first crushed object;
mixing the first crushed material with water according to the mass ratio of 1 (4-10) to obtain first fine crushed pulp and first fine crushed slag deposited at the bottom of the water;
adding water into the first fine crushed slag to perform secondary crushing to obtain second fine crushed pulp and second fine crushed slag precipitated at the bottom of the water;
circulating for n times to obtain n-th fine slurry, wherein n is an integer greater than or equal to 1;
and combining the fine crushed pulp obtained in each step to obtain the beautiful millettia root crushed material.
3. The method according to claim 1, wherein in the step of mixing the Millettia speciosa champ crushed material with water and emulsifying and stirring the mixture, the mass ratio of the Millettia speciosa raw material to the water is 1: (10-17); and/or
The circulating pressure of the emulsification and stirring cutting is 0.1-0.2 MPa.
4. The method as claimed in claim 1, wherein the step of separating the Millettia speciosa homogenate comprises centrifuging at 3800-.
5. The method according to any one of claims 1 to 4, wherein the extraction is carried out by a low-temperature high-pressure-difference continuous extraction technique at a temperature of 5 ℃ to 45 ℃ and at a pressure of 20MPa to 60 MPa.
6. The preparation method according to claim 5, wherein the mass ratio of the Millettia speciosa champ separated slag to the alcohol aqueous solution is 1: (8-15); the alcohol aqueous solution is an ethanol aqueous solution, wherein the volume percentage content of ethanol is 50-60%.
7. The method according to claim 5, further comprising a step of microfiltration of the Millettia speciosa solution and/or the Millettia speciosa solution with a microfiltration membrane of 300nm to 600nm after the step of obtaining the Millettia speciosa solution and/or the Millettia speciosa solution.
8. The method of claim 7, further comprising the following steps after the step of obtaining the solution and/or the separated solution of Millettia speciosa:
concentrating the beautiful millettia root alcohol solution by adopting a reverse osmosis concentration method to obtain a beautiful millettia root alcohol extract with the solid content of 5-20 percent; and/or
Concentrating the millettia speciosa champ separation liquid by adopting a reverse osmosis concentration method to obtain a millettia speciosa champ aqueous extract with the solid content of 5-20%.
9. The beautiful millettia root extract prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the beautiful millettia root extract according to claim 9 for the production of foods, drinks or medicines.
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