CN112007087A - Method for extracting fresh rehmannia root, fresh rehmannia root extract, fresh rehmannia root granules and composition - Google Patents
Method for extracting fresh rehmannia root, fresh rehmannia root extract, fresh rehmannia root granules and composition Download PDFInfo
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Abstract
The invention provides a fresh rehmannia root extraction method, a fresh rehmannia root extracting solution, fresh rehmannia root granules and a composition, wherein the fresh rehmannia root extraction method comprises the following steps: taking a fresh rehmannia root plant for ultraviolet sterilization; crushing and homogenizing ultraviolet sterilized fresh rehmannia root to obtain juice and dregs; carrying out ultrahigh-temperature instantaneous sterilization on the juice to obtain first medicinal juice; decocting the dregs to obtain a second medicinal liquid; mixing the first and second medicinal juices to obtain fresh rehmanniae radix extractive solution. The method can obtain fresh rehmanniae radix preparation with high microorganism qualification rate and comprehensive effective components.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, and particularly relates to a method for extracting fresh rehmannia, a fresh rehmannia extracting solution, fresh rehmannia granules and a composition.
Background
The fresh Rehmannia root is fresh root tuber of Rehmannia Rehmannia glutamosa Libosch of Scrophulariaceae, is sweet, bitter and cold in taste, has the effects of clearing heat, promoting fluid, cooling blood and stopping bleeding, is used for treating fever yin impairment, crimson tongue, polydipsia, toxic heat, macula, hematemesis, epistaxis and swollen sore throat, is a common fresh medicinal material in traditional Chinese medicine, and has been applied for more than 2000 years in China. Bai He Di Huang Tang recorded in jin Kui Yao L ü e is prepared from Bai He and fresh Di Huang juice, and is indicated for lily diseases with symptoms similar to those of the first disease without vomiting and sweating. In the formula of the JI YUAN ZHI JI FANG, fresh rehmannia root is decocted in water for oral administration, and can be used for treating typhoid fever, seasonal febrile disease, headache, and strong fever with large pulse. Therefore, the fresh rehmannia root is clinically used for treating certain diseases in the traditional Chinese medicine, and has special curative effect.
Because the original fresh medicine supply mode of 'front shop and back shop' is not suitable for the requirements of modern society, the fresh rehmannia has the problems of difficult fresh-keeping and storage, single supply channel, deficient variety of fresh medicine preparations, inconvenient clinical dispensing and use and the like, so the fresh rehmannia is often replaced by the fresh rehmannia in clinical application. However, the difference between Sheng Di Huang and Xian Di Huang is large in terms of chemical composition, pharmacological efficacy and usage and dosage, which will affect the curative effect of Sheng Di Huang on some diseases.
In the modern technology, the fresh rehmannia slices are quickly dried at the temperature of below 100 ℃, the method solves the storage problem of the fresh rehmannia to a certain extent, but the fresh rehmannia is baked, dehydrated and dried for 4 to 12 hours and basically consistent with the process of slowly baking the fresh rehmannia to be about eight dry raw rehmannia, so that the fresh rehmannia characteristic is lost, partial active components are inactivated, and the medicinal value is reduced. Although the characteristic of 'freshness' of the fresh medicine can be kept by adopting the traditional Chinese medicine decoction method, the method has low extraction efficiency and single efficacy component, and the fresh medicine preparation has a serious problem that microorganisms are extremely easy to fail, and the problem is one of important problems which hinder the development of the fresh medicine preparation.
Disclosure of Invention
Based on the above, there is a need for a fresh rehmannia root extraction method, a fresh rehmannia root extract, a fresh rehmannia root granule and a composition, wherein the fresh rehmannia root extraction method can obtain a fresh medicinal preparation with high microbial qualification rate and comprehensive efficacy components.
A method for extracting fresh rehmannia comprises the following steps:
taking a fresh rehmannia root plant for ultraviolet sterilization;
crushing and homogenizing ultraviolet sterilized fresh rehmannia root to obtain juice and dregs;
carrying out ultrahigh-temperature instantaneous sterilization on the juice to obtain first medicinal juice;
decocting the dregs to obtain a second medicinal juice;
and combining the first medicinal juice and the second medicinal juice to obtain the fresh rehmannia root extracting solution.
In one embodiment, in the step of performing ultraviolet sterilization on the fresh rehmannia glutinosa Libosch plant, the ultraviolet wavelength is 253.7nm, and the ultraviolet intensity is greater than 90 μ W/cm2The sterilization time is 0.5-2 h.
In one embodiment, the step of crushing and homogenizing the uv-sterilized fresh rehmannia comprises the steps of:
crushing the ultraviolet sterilized fresh rehmannia to obtain crushed fresh rehmannia;
mixing the crushed fresh rehmannia root and water, and homogenizing at 0-30 ℃ for 10-60min, wherein the feeding amount of the water is 1-5 times of the weight of the crushed fresh rehmannia root.
In one embodiment, in the step of performing ultrahigh-temperature instant sterilization on the juice, the temperature of the ultrahigh-temperature instant sterilization is 100-200 ℃ and the time is 5-60 seconds.
In one embodiment, the step of decocting the dregs comprises the following steps:
mixing the medicine residues with water, decocting for 0.5-2h, and filtering to obtain a second decoction, wherein the dosage of water is 5-20 times of the weight of the medicine residues.
In one embodiment, the method further comprises the step of concentrating the first medicinal juice and/or the second medicinal juice, and the relative density of the concentrated medicinal juice after concentration is 1.01-1.20.
In one embodiment, the step of concentrating the first and/or second juices comprises the steps of:
and (2) concentrating the first medicinal juice and/or the second medicinal juice under reduced pressure at 40-85 ℃ until the relative density is 1.01-1.2.
The fresh rehmannia root extract is prepared by the extraction method.
A granule of fresh rehmanniae radix is prepared from the above fresh rehmanniae radix extract.
A Chinese medicinal composition comprises the above fresh radix rehmanniae extractive solution and/or the above fresh radix rehmanniae granule.
According to the fresh rehmannia root extraction method, the fresh rehmannia root plants are subjected to ultraviolet sterilization at first, a large number of microorganisms on the surfaces of the plants are guaranteed to be eliminated, the problem that bacterial infection after wall breaking can be effectively avoided, and the problem that effective sterilization cannot be achieved is solved. By adopting the method of combining ultraviolet sterilization and ultrahigh-temperature instantaneous sterilization, on one hand, the sterilization strains can be enlarged, the purpose of comprehensive sterilization is achieved, the problem that microorganisms of the traditional fresh medicine preparation are easily unqualified is effectively solved, and the safety of the fresh medicine clinical medication is ensured; on the other hand, the time for ultrahigh temperature instantaneous sterilization can be greatly shortened, so that the inactivation of active components can be effectively avoided, and the medicinal value of the product is improved.
The method for extracting the fresh rehmannia root firstly adopts a homogenate method to obtain the juice and the dregs of a decoction, so as to retain the active components of the fresh rehmannia root to the maximum extent, keep the characteristics of the fresh rehmannia root, and further decoct the dregs of a decoction to fully decoct the active components, thereby not only improving the extraction efficiency, but also enabling the active components in the obtained extract to be more comprehensive, and effectively avoiding the problems of single component and low extraction efficiency in the traditional process.
Moreover, the fresh rehmannia root extraction method creatively carries out ultraviolet sterilization on fresh rehmannia root plants and then carries out subsequent extraction steps, so that on one hand, the sterilization efficiency is improved, on the other hand, the influence of the existence of microorganisms on active components in the extraction process can be effectively avoided, the extraction efficiency of the active components is further improved, and the medicinal value is improved.
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 invention provides a method for extracting fresh rehmannia, which comprises the following steps:
s101: taking fresh rehmannia root plants for ultraviolet sterilization.
The fresh Rehmannia glutinosa plant of step S101 is fresh root tuber of Rehmannia glutinosa Libosch of Scrophulariaceae family. Understandably, the fresh rehmannia can be pretreated, and particularly the pretreatment can comprise the following steps: cleaning to remove reed heads, fibrous roots, silt and the like, and draining.
Preferably, the ultraviolet sterilization conditions in step S101 are that the ultraviolet wavelength is 253.7nm and the ultraviolet intensity is more than 90 muW/cm2The sterilization time is 0.5-2h, and the plants can be rolled in the sterilization process so as to achieve comprehensive sterilization.
The inventor finds that the traditional method of extracting firstly and then sterilizing is difficult to achieve complete and effective sterilization in the research process, probably because the wall of a plant is broken in the extraction process, microorganisms permeate and contaminate, and further the comprehensive sterilization cannot be achieved, and particularly, the high-temperature resistant bacteria are difficult to remove. Therefore, the inventor creatively carries out ultraviolet sterilization on the plant firstly to realize comprehensive sterilization on the plant wall, and then carries out the subsequent extraction step, thereby solving the problems and greatly improving the sterilization effect. And the subsequent extraction step is carried out under the aseptic condition, the problem of active component decomposition caused by microorganisms in the extraction and storage processes can be avoided, and the efficacy and the stability of the obtained extract are further improved.
S102: crushing and homogenizing ultraviolet sterilized fresh rehmanniae radix to obtain juice and residue.
Specifically, step S102 may include the steps of:
s1021: crushing the ultraviolet sterilized fresh rehmannia to obtain the crushed fresh rehmannia.
The crushing method is not particularly limited, and methods and apparatuses commonly used in the art, such as a coarse crusher, can be used.
S1022: mixing crushed fresh rehmanniae radix with water, and homogenizing at 0-30 deg.C for 10-60min, wherein the amount of water is 1-5 times of the weight of the crushed fresh rehmanniae radix.
The active components of the fresh rehmannia can be retained to the maximum extent by adopting a homogenization method, the characteristics of the fresh rehmannia are kept, the temperature of the homogenate is controlled to be 0-30 ℃, and the active components can be prevented from being degraded due to high temperature.
Further, it is preferable that the temperature of the homogenate is 4 ℃ to 20 ℃ and the time of the homogenate is 20min to 40 min.
S103: and (4) carrying out ultrahigh-temperature instantaneous sterilization on the juice to obtain first medicinal juice.
The medicine juice produced in the production process can be sterilized by adopting ultra-high temperature instantaneous sterilization, and simultaneously, the sterilization bacteria can be expanded by combining with the ultraviolet sterilization in the step S101, so that the purpose of comprehensive sterilization is achieved, the problem that the traditional fresh medicine preparation microorganism is extremely easy to disqualify is effectively solved, and the safety of the fresh medicine clinical medication is ensured.
Because the whole fresh rehmannia root is sterilized and then extracted, the microorganism content in the whole process is low, the ultrahigh-temperature instant sterilization time can be greatly shortened, the decomposition of active components can be avoided, and the total content of the active components in the obtained extracting solution can be ensured.
Further, the temperature of high-temperature instant sterilization is preferably 100-200 ℃ and the time is preferably 5-60 s. Further, the sterilization time is preferably 10s to 30 s.
In addition, step S103 may further include a concentration step, specifically, the first juice is concentrated under reduced pressure at 40 ℃ to 85 ℃ to a desired relative density. Concentration is preferably carried out at 40 ℃ to 65 ℃ to ensure the activity of the active ingredient.
In one embodiment, the first juice has a relative density of 1.01 to 1.2.
S104: decocting the dregs to obtain a second medicinal liquid;
in the step S104, the medicine dregs are decocted, so that on one hand, the decoction in the decocting process can be sterilized by using the high temperature of the decoction, on the other hand, the active components can be fully decocted out, the extraction efficiency is improved, the active components in the obtained extract are more comprehensive, and the problems of single component and low extraction efficiency in the traditional process are effectively solved.
Specifically, step S104 may include the steps of:
mixing the decoction dregs and water, decocting for 0.5-2h, and filtering to obtain a second decoction, wherein the feed amount of the water is 5-20 times of the weight of the decoction dregs, preferably 10-15 times of the weight of the decoction dregs, and the use of the water with the same amount has higher extraction efficiency, can prevent waste caused by excessive water, reduce the difficulty of subsequent concentration and reduce the production cost.
In addition, step S104 may further include a step of concentrating the second decoction, specifically: and concentrating the second medicinal juice at 40-85 deg.C under reduced pressure to desired relative density. Concentration is preferably carried out at 40 ℃ to 65 ℃ to ensure the activity of the active ingredient.
In one embodiment, the relative density of the second juice is 1.01-1.2.
S105: mixing the first and second medicinal juices to obtain fresh rehmanniae radix extractive solution.
It is understood that the first and second juices can be concentrated to the desired relative densities and then mixed, or mixed and then concentrated, and are understood to be within the scope of the present invention.
The obtained fresh rehmanniae radix extractive solution contains high content of active components, has high microorganism qualification rate, and can be made into various preparations, such as: decoction, pill, paste, oral liquid, capsule, tablet, granule, etc., or can be mixed with other components to make into Chinese medicinal composition.
The invention also provides fresh rehmannia root granules prepared from the fresh rehmannia root extracting solution.
The prepared fresh rehmannia root granules have the advantages of no decoction, easy carrying, convenient taking and the like, solve the limitations of seasonal harvesting, fresh keeping, storage, transportation, clinical dispensing and the like of the fresh rehmannia root, and avoid the problem of reduced special efficacy caused by the loss of active ingredients in the process of processing the fresh rehmannia root into the fresh rehmannia root. It can also provide safe and effective fresh rehmannia root granules with controllable quality for clinical use, is convenient for clinical application based on syndrome differentiation, can be added or subtracted according to the syndrome and can be freely adjusted, so that the traditional classical prescription using fresh rehmannia root as a medicine can be inherited and applied.
The invention also provides a preparation method of the fresh rehmannia root granules, which comprises the following steps:
s201: providing a fresh rehmannia root extracting solution;
the method for extracting the fresh rehmannia root extract is as described in steps S101-S105, and is not described herein again.
S202, concentrating, drying and granulating the fresh rehmannia root extracting solution.
The drying method may adopt methods commonly used in the art, and is not particularly limited herein, including but not limited to: one or more of freeze drying, spray drying, belt drying, vacuum drying and forced air drying. The granulation process may be carried out using granulation equipment commonly used in the art.
The present invention is further illustrated by the following specific embodiments, which are not intended to limit the scope of the invention.
Example 1:
the preparation method of the fresh rehmannia granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal juice and the second concentrated medicinal juice, mixing, lyophilizing, and granulating to obtain granule of fresh rehmanniae radix.
Example 2
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at the temperature of 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at the temperature of 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Example 3:
the preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and placing the clean platform under the ultraviolet condition for direct irradiation sterilization for 2 hours;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount 5 times of the feed amount, homogenizing at the low temperature of 4 ℃ for 60min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount 10 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1.5h, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Example 4:
the preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and placing the clean platform under the ultraviolet condition for direct irradiation sterilization for 2 hours;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 2 times of the feed amount, homogenizing at the low temperature of 20 ℃ for 20min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice in an ultrahigh-temperature instant sterilizer at 100-200 ℃ for 10 seconds to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water 13 times the amount of fresh rehmannia root dregs into the fresh rehmannia root dregs, heating and decocting the mixture for 2 hours, collecting an extracting solution, filtering the extracting solution to obtain a second medicinal juice, and concentrating the second medicinal juice at the temperature of 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. and mixing the first concentrated medicinal juice and the second concentrated medicinal juice, uniformly mixing, drying in vacuum, and granulating to obtain the fresh rehmannia granules.
Example 5
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 0.5h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 1 time of the feed amount, homogenizing at the low temperature of 30 ℃ for 10min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 60 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. taking fresh rehmannia root dregs, adding water with the amount 15 times of the feeding amount, heating and decocting for 0.5h, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, drying, and granulating to obtain granule.
Example 6
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing for 30min at the temperature of 40 ℃, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Example 7
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 5min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. and mixing the first concentrated medicinal juice and the second concentrated medicinal juice, uniformly mixing, spray-drying, and granulating to obtain the fresh rehmannia granules.
Example 8
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 120 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Example 9
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount 20 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 3 hours, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Comparative example 1: dried rehmannia root formula particle
The preparation method of the dried rehamnnia root formula particle comprises the following steps:
a. taking radix rehmanniae decoction pieces, and sterilizing under ultraviolet irradiation for 1 h;
b. crushing sterilized radix rehmanniae into blocks by adopting a coarse crusher, adding water with the amount 15 times of the material amount, heating and decocting for 1h, collecting an extracting solution, filtering, and concentrating the filtrate under reduced pressure at 40-85 ℃ until the relative density is 1.08 to obtain radix rehmanniae extract;
c. taking the dried rehmannia root clear paste, freeze-drying and granulating to obtain the dried rehmannia root formula granules.
Comparative example 2: fresh rehmannia root (juice) prescription granule
The preparation method of the fresh rehmannia (juice) formula particle comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding 15 times of water by the feeding amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer, and then concentrating the juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain fresh juice concentrated juice;
d. taking the fresh juice concentrated juice, freeze-drying and granulating to obtain the fresh rehmannia (juice) formula granules.
Comparative example 3: fresh rehmannia root (decoction) prescription granule
The preparation method of the fresh rehmannia (decocted) formula granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing sterilized fresh rehmannia root into blocks by using a coarse crusher, adding water with the amount 15 times that of the fed material, heating and decocting for 1 hour, collecting an extracting solution, filtering, and concentrating the filtrate under reduced pressure at 40-85 ℃ until the relative density is 1.08 to obtain a fresh rehmannia root extract;
c. taking the clear paste of the fresh rehmannia root, freezing, drying and granulating to obtain the (decocted) prescription granule of the fresh rehmannia root.
Comparative example 4
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; spreading the drained fresh rehmannia root on a clean platform, and sterilizing for 1h under ultraviolet irradiation;
b. crushing the sterilized fresh rehmannia root into blocks by adopting a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, and concentrating under reduced pressure at 40-65 ℃ until the relative density is 1.02 to obtain a first concentrated medicine juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Comparative example 5
The preparation method of the fresh rehmannia root granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water;
b. crushing the dried fresh rehmannia root into blocks by using a coarse crusher, putting the blocks into a refiner, adding water with the amount of 3 times of the feed amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal liquid and the second concentrated medicinal liquid, mixing, spray drying, and granulating to obtain fresh rehmanniae radix granule.
Comparative example 6
The preparation method of the fresh rehmannia granules comprises the following steps:
a. removing fresh rhizoma Phragmitis, fibrous root and silt from fresh rehmanniae radix, cleaning, and draining off surface water; after the surface moisture is drained, crushing the fresh rehmannia root into blocks by adopting a coarse crusher, and then placing the blocks under the ultraviolet condition for direct irradiation sterilization for 1 hour;
b. putting the sterilized fresh rehmannia root fragments into a homogenizer, adding water with the amount of 3 times of the material amount, homogenizing at the low temperature of 5 ℃ for 30min, and filtering to obtain fresh rehmannia root homogenate juice and dregs;
c. taking the fresh rehmannia root homogenate juice, sterilizing the fresh rehmannia root homogenate juice for 30 seconds at 100-200 ℃ in an ultrahigh-temperature instant sterilizer to obtain first medicinal juice, and then concentrating the first medicinal juice at 40-65 ℃ under reduced pressure until the relative density is 1.02 to obtain first concentrated medicinal juice;
d. adding water with the amount being 12 times of the feed amount into fresh rehmannia root dregs, heating and decocting for 1 hour, collecting an extracting solution, filtering to obtain a second medicinal juice, and concentrating the second medicinal juice at 40-85 ℃ under reduced pressure until the relative density is 1.08 to obtain a second concentrated medicinal juice;
e. mixing the first concentrated medicinal juice and the second concentrated medicinal juice, mixing, lyophilizing, and granulating to obtain granule of fresh rehmanniae radix.
Effect testing experiment
The fresh rehmannia glutinosa particles of examples 1 to 9 and comparative examples 1 to 6 were measured for cream yield, index ingredient content, and microorganism status, and the results of examples 1 to 9 are shown in Table 1, and the results of comparative examples 1 to 6 are shown in Table 2.
The method for measuring the cream yield comprises the following steps: the measurement is carried out by referring to the method under the item of the water-soluble extract measurement method (the general rule 2201 of the national pharmacopoeia 2015). The specific method comprises precisely measuring 25mL of filtrate, placing in an evaporating dish M1 dried to constant weight, drying in water bath, drying at 105 deg.C for 3 hr, cooling in a desiccator for 30min, and rapidly and precisely weighing M2. The feeding amount of the decoction pieces is M, the volume of the extracting solution is V, and the paste yield calculation formula is as follows:
the measuring method of the content of the index components comprises the following steps:
catalpol: the determination is carried out by referring to high performance liquid chromatography (China pharmacopoeia 2015 edition general rules 0512).
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile-0.1% phosphoric acid solution (1:99) is used as a mobile phase; the detection wavelength is 210 mn; the number of theoretical plates is not less than 5000 calculated according to catalpol peak.
Verbascoside: the determination is carried out by referring to high performance liquid chromatography (China pharmacopoeia 2015 edition general rules 0512).
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile 0.1% acetic acid solution (16:84) is used as a mobile phase; the detection wavelength is 334 nm; the theoretical plate number is not less than 5000 calculated according to the verbascoside peak.
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
TABLE 2
From examples 1-9, it can be seen that the active components (catalpol and verbascoside) of the fresh rehmannia granules prepared by the above method have high content, and the microbial detection is qualified.
In addition, example 1 is different from examples 6 to 9 in the parameters such as homogenization temperature, time, the amount of water added, and the time for decoction. As can be seen from table 1, the above parameters have certain influence on the content of the active component, and in particular, example 8 is substantially the same as example 1, except that the ultrahigh-temperature instant sterilization time is 120s in example 8 and 30s in example 1, while the catalpol content in example 8 is significantly lower than that in example 1, which may be due to partial decomposition of the active component during the ultrahigh-temperature instant sterilization process, and it is again demonstrated that by using the ultraviolet sterilization and ultrahigh-temperature instant sterilization combination of the present invention, the content of the active component can be maintained on the basis of ensuring the sterilization effect, and further, the medical value of the product can be improved.
The comparative example 1 is that the radix rehmanniae decoction pieces are directly adopted for preparation, and the comparative example 1 show that the content of catalpol and verbascoside in the fresh radix rehmanniae granules in the example 1 is greatly different from that of the radix rehmanniae formula granules, the catalpol content is about 2 times different, and the verbascoside content is about 4-5 times different, which indicates that the fresh radix rehmanniae granules prepared by the method are different from the radix rehmanniae formula granules in the current market.
In addition, comparative example 2 is a step of lacking decoction of the dregs (only homogenization) compared to example 1, and comparative example 3 is a step of lacking homogenization (only decoction) compared to example 1. As can be seen from tables 1 and 2, the fresh rehmannia granules prepared by the combination of fresh rehmannia juice extraction and decoction extraction of herb residue in example 1 have higher contents of catalpol and verbascoside than the granules prepared by only juice extraction and decoction extraction, and thus the active ingredients of the fresh rehmannia can be retained to the maximum extent, and the clinical efficacy of the fresh rehmannia can be ensured.
Compared with the example 2, the comparative example 4 lacks the step of ultra-high temperature instantaneous sterilization, and the comparative example 5 lacks the step of ultraviolet sterilization, and as can be seen from tables 1 and 2, the rehmannia glutinosa particles prepared by the dual control technology of ultraviolet sterilization and ultra-high temperature instantaneous sterilization in the example 2 can meet the requirement of each microorganism index, while the total number of aerobic colonies and the microorganism indexes of mold and yeast bacteria in the comparative examples 4 and 5 which only adopt one sterilization technology of ultraviolet sterilization or ultra-high temperature instantaneous sterilization are seriously beyond the specified limits. The invention shows that the fresh rehmannia granules prepared by adopting ultraviolet sterilization on source control and adopting a double-control technology of ultrahigh-temperature instantaneous sterilization on process control can strictly control the microorganisms of the product, solve the problem that the microorganisms of the fresh medicine preparation are easily unqualified, and ensure the safety of the fresh medicine clinical medication.
Compared with the example 1, the comparative example 6 is that fresh rehmannia is firstly crushed and then subjected to ultraviolet sterilization, and as can be seen from tables 1 and 2, the microorganism content of the comparative example 6 is far greater than that of the example 1, so that the method of the example 1 that plants are firstly subjected to ultraviolet sterilization to comprehensively sterilize the plant walls and then subjected to subsequent extraction steps has obvious advantages.
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. A method for extracting fresh rehmannia is characterized by comprising the following steps:
taking a fresh rehmannia root plant for ultraviolet sterilization;
crushing and homogenizing ultraviolet sterilized fresh rehmannia root to obtain juice and dregs;
carrying out ultrahigh-temperature instantaneous sterilization on the juice to obtain first medicinal juice;
decocting the dregs to obtain a second medicinal juice;
and combining the first medicinal juice and the second medicinal juice to obtain the fresh rehmannia root extracting solution.
2. The method for extracting fresh rehmannia glutinosa as claimed in claim 1, wherein the step of subjecting the fresh rehmannia glutinosa plant to ultraviolet sterilization comprises ultraviolet irradiation at 253.7nm and at an intensity of more than 90 μ W/cm2The sterilization time is 0.5h-2 h.
3. The fresh rehmannia glutinosa libosch extraction method as claimed in claim 1, wherein the step of crushing and homogenizing the uv-sterilized fresh rehmannia glutinosa libosch comprises the steps of:
crushing the ultraviolet sterilized fresh rehmannia to obtain crushed fresh rehmannia;
mixing the crushed fresh rehmannia root and water, and homogenizing at 0-30 ℃ for 10-60min, wherein the feeding amount of the water is 1-5 times of the weight of the crushed fresh rehmannia root.
4. The fresh rehmannia glutinosa libosch extraction method according to claim 1, wherein the step of subjecting the juice to ultra high temperature flash sterilization is performed at a temperature of 100-200 ℃ for 5-60 s.
5. The fresh rehmannia root extraction method according to claim 1, wherein the decoction of the decoction dregs comprises the following steps:
mixing the medicine residues with water, decocting for 0.5-2h, and filtering to obtain a second decoction, wherein the dosage of water is 5-20 times of the weight of the medicine residues.
6. The fresh rehmannia glutinosa libosch extraction method according to any one of claims 1-5, further comprising a step of concentrating the first juice and/or the second juice, wherein the relative density of the concentrated juice obtained after concentration is 1.01-1.20.
7. The fresh rehmannia glutinosa libosch extraction method according to claim 6, wherein the step of concentrating the first juice and/or the second juice comprises the steps of:
and (2) concentrating the first medicinal juice and/or the second medicinal juice under reduced pressure at 40-85 ℃ until the relative density is 1.01-1.2.
8. An extract of fresh rehmannia glutinosa prepared by the method of any one of claims 1 to 7.
9. A fresh rehmannia glutinosa granule prepared from the fresh rehmannia glutinosa extract of claim 8.
10. A Chinese medicinal composition comprising the fresh rehmannia root extract according to claim 8 and/or the fresh rehmannia root granules according to claim 9.
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| CN108619305A (en) * | 2018-07-06 | 2018-10-09 | 芜湖天成普阳中药科技有限公司 | Glutinous rehmannia is fresh to carry freeze-drying granule pieces |
| CN110115731A (en) * | 2019-03-30 | 2019-08-13 | 北京葆年堂(菏泽)药业有限公司 | A kind of preparation method and fresh rehmannia powder medicine materical crude slice of fresh rehmannia powder |
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| CN108619304A (en) * | 2018-07-06 | 2018-10-09 | 徐自升 | Glutinous rehmannia is fresh to carry spray-dried granules medicine materical crude slice |
| CN108619305A (en) * | 2018-07-06 | 2018-10-09 | 芜湖天成普阳中药科技有限公司 | Glutinous rehmannia is fresh to carry freeze-drying granule pieces |
| CN110115731A (en) * | 2019-03-30 | 2019-08-13 | 北京葆年堂(菏泽)药业有限公司 | A kind of preparation method and fresh rehmannia powder medicine materical crude slice of fresh rehmannia powder |
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