CN110946761A - Preparation method and qualitative detection method of grifola soup reference substance - Google Patents
Preparation method and qualitative detection method of grifola soup reference substance Download PDFInfo
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Abstract
The embodiment of the invention discloses a preparation method and a qualitative detection method of a grifola decoction reference substance, wherein the preparation method comprises the following steps: processing Polyporus, Poria, Alismatis rhizoma, pulvis Talci and colla Corii Asini to obtain medicinal liquid; and freeze-drying the liquid medicine to prepare the grifola decoction reference substance. The qualitative detection method comprises the following steps: preparing a control solution; preparing a test solution; performing chromatographic contrast detection by adopting a thin-layer chromatography; and respectively obtaining the chromatographic control results of the two groups of silica gel G thin-layer plates for analysis. The invention furthest retains the medicinal properties of the traditional Chinese medicinal materials in the polyporus umbellatus soup by adopting a freeze-drying operation mode after decoction, and effectively ensures the medicinal effects and medicinal properties of the reference substances of the polyporus umbellatus soup produced in a large scale by further qualitatively analyzing the medicinal materials and components in the medicinal materials.
Description
Technical Field
The embodiment of the invention relates to the field of large-scale production and quality control of traditional Chinese medicine formulas, in particular to a preparation method and a qualitative detection method of a grifola decoction reference substance.
Background
The classical famous prescription is a prescription which is derived from ancient books of traditional Chinese medicine, is still widely applied at present, has definite curative effect and obvious characteristics and advantages. The national traditional Chinese medicine administration of 4 months in 2018 publishes the catalogue of ancient classic famous prescriptions, and the polyporus umbellatus soup is included as a classic famous prescription in the catalogue of ancient classic famous prescriptions.
However, in practical applications, the polyporus umbellatus soup is often obtained by traditional Chinese medicine decoction when needed, that is, the polyporus umbellatus soup is suitable for decoction in small batches, and is not prepared by modern mass production.
Meanwhile, if a modern large-scale production mode is adopted for production, due to the problems of the property and the components of the traditional Chinese medicinal materials in the polyporus umbellatus soup, the quality of the traditional Chinese medicinal materials subjected to batch production in a general mode can not be guaranteed to reach the quality of the traditional Chinese medicinal materials subjected to decoction, and the conventional large-scale production mode can easily cause the reduction of the cream yield and the reduction of effective components.
Disclosure of Invention
Therefore, the preparation method and the qualitative detection method of the grifola decoction reference substance provided by the embodiment of the invention can be used for maximally keeping the medicinal properties of the grifola decoction traditional Chinese medicinal materials by adopting a freeze-drying operation mode after decoction, and effectively ensuring the medicinal effects and medicinal properties of the large-scale produced grifola decoction reference substance by further qualitatively analyzing the medicinal materials and components in the medicinal materials.
In order to achieve the above object, an embodiment of the present invention provides the following:
in one aspect of the embodiment of the present invention, there is provided a method for preparing a grifola soup reference substance, comprising:
s10, processing Polyporus, Poria, rhizoma Alismatis, pulvis Talci, and colla Corii Asini to obtain medicinal liquid;
s20, lyophilizing the medicinal liquid to obtain the basic substance of Polyporus umbellatus decoction.
As a preferable embodiment of the present invention, step S20 specifically includes:
s21, concentrating the liquid medicine to a relative density of 1.01-1.04 under the conditions that the vacuum degree is-0.090-0.099 MPa and the temperature is 40-60 ℃ to obtain concentrated paste;
s22, sequentially pre-freezing and stage-wise freeze-drying the concentrated paste to obtain the grifola soup reference substance; wherein the content of the first and second substances,
the maximum temperature of the temperature during the prefreezing process is not higher than the minimum temperature during the staged lyophilization operation.
As a preferable embodiment of the present invention, step S21 specifically includes:
s211, placing the liquid medicine in a concentration tank, vacuumizing and simultaneously heating until the vacuum degree in the concentration tank is-0.090-0.099 MPa and the temperature is 40-60 ℃;
s212, evaporating and concentrating to obtain concentrated paste with the relative density of 1.01-1.04 under the ultrasonic oscillation condition.
As a preferred aspect of the present invention, the concentration tank includes a tank body and a fin assembly disposed in the tank body; and the number of the first and second electrodes,
the end surface part of the tank body is inwards sunken to form an upright post;
the fin component is arranged on the side face of the upright column in the tank body and at least comprises a plurality of groups of first fin groups and second fin groups which are arranged at intervals in the axial direction of the upright column, each group of the first fin groups comprises a plurality of first fins which are arranged at equal intervals in the circumferential direction, each group of the first fin groups comprises a plurality of second fins which are arranged at equal intervals in the circumferential direction, and the first fins and the second fins are different in shape.
In a preferred embodiment of the present invention, the first fin is formed in a rectangular parallelepiped structure extending from a side surface of the pillar in an extending direction of a radius of the pillar, and a height of the rectangular parallelepiped structure is 1/20 to 1/10 of a length of the rectangular parallelepiped structure in the extending direction;
the second fin is formed into a fan-shaped ring structure extending from the side surface of the upright column along the extending direction of the radius of the upright column, and the height of the fan-shaped ring structure is 1/20-1/10 of the length of the fan-shaped ring structure along the extending direction.
As a preferred embodiment of the present invention, the dosage ratio of the polyporus umbellatus, the poria cocos, the alisma orientale, the talc and the donkey-hide gelatin is 1: 0.8-1.2: 0.8-1.2: 0.8-1.2: 0.8 to 1.2; further, step S10 specifically includes:
s11, boiling Polyporus, Poria, Alismatis rhizoma and pulvis Talci in water, decocting for 30-60min, and filtering to obtain filtrate;
s12, adding the donkey-hide gelatin into the filtrate, and melting until the donkey-hide gelatin is dissolved in the filtrate to obtain a liquid medicine.
As a preferred scheme of the invention, the pre-freezing temperature in the pre-freezing process is-50 to-60 ℃, and the pre-freezing time is 30 to 120 min;
the staged freeze-drying operation comprises a first freeze-drying section, a second freeze-drying section, a third freeze-drying section, a fourth freeze-drying section and a fourth freeze-drying section which are arranged in sequenceA five freeze-drying section and a temperature return section; the temperature of the first freeze-drying section is-50 to-40 ℃, the time is 2 to 3 hours, and the pressure is 20 to 25 Pa; the temperature of the second freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is 10 to 15 Pa; the temperature of the third freeze-drying section is-55 to-40 ℃, the time is 3 to 6 hours, and the pressure is 15 to 20 Pa; the temperature of the fourth freeze-drying section is-55 to-40 ℃, the time is 4 to 6 hours, and the pressure is 5 to 10 Pa; the temperature of the fifth freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is 20 to 25 Pa; the temperature return section is heated at a heating rate of 0.2-0.5 ℃/min and simultaneously CO is introduced into the temperature return section2And continuously standing for 1-2 hours until the ambient temperature is 20-30 ℃ and the pressure is 0.9-1.1 atm.
In another aspect of the embodiment of the present invention, there is provided a qualitative detection method for herbal ingredients in the above-mentioned grifola decoction reference substance, comprising:
s100, preparing a polyporus umbellatus medicinal material, a poria cocos medicinal material, an rhizoma alismatis medicinal material and 23-acetyl alisol B into control solutions for later use, wherein the control solutions are respectively marked as a polyporus umbellatus control medicinal material solution, a poria cocos control medicinal material solution, an rhizoma alismatis control medicinal material solution and a 23-acetyl alisol B control solution;
s200, preparing two different test solution for later use by taking the grifola decoction reference substance, and respectively recording the two test solution as a test solution A and a test solution B;
s300, taking the polyporus umbellatus reference medicinal material solution, the poria cocos reference medicinal material solution and a sample solution A as a group, taking the rhizoma alismatis reference medicinal material solution, the 23-acetyl alisol B reference solution and the sample solution B as a group, and respectively pointing the groups on the same silica gel G thin-layer plate for chromatographic contrast detection;
s400, obtaining the chromatographic control results of the two groups of silica gel G thin-layer plates respectively for analysis.
As a preferable aspect of the present invention, the step S100 or S200 includes:
s101, mixing a grifola medicinal material, a poria cocos medicinal material and a grifola soup reference substance with one part of diethyl ether respectively, taking residues obtained after filtrate is evaporated to dryness, adding methanol into the residues and mixing to obtain a grifola reference medicinal material solution, a poria cocos reference medicinal material solution and a sample solution A respectively;
s102, mixing the rhizoma alismatis medicinal material and the grifola decoction reference substance with one part of methanol respectively, taking the residue obtained after filtrate is evaporated to dryness, adding the methanol into the residue and mixing to obtain rhizoma alismatis reference medicinal material solution and sample solution B respectively; adding the 23-acetyl alisol B into methanol for mixing to obtain a 23-acetyl alisol B control solution;
step S300 includes:
s301, taking 2-5 mu L of each of the polyporus umbellatus reference medicinal material solution and the poria cocos reference medicinal material solution, taking 20-50 mu L of the sample solution A, dropping the sample solution A on the same silica gel G thin layer plate, taking cyclohexane-ethyl acetate-formic acid with the volume ratio of 8:1:0.1 as a developing agent, developing, airing, and directly placing under 365nm for fluorescence color development or spraying 10% sulfuric acid ethanol, airing, and placing under 365nm for inspection;
s302, taking 2-5 mu L of each of the alisma control medicinal material solution, the 23-acetyl alisol B control solution and the sample solution B, placing the solution on the same silica gel G thin-layer plate, developing by taking cyclohexane-ethyl acetate as a developing agent in a volume ratio of 1:1, airing, spraying a 2% vanillin-sulfuric acid solution, heating at 105 ℃ until spots are clear, and inspecting.
As a preferred scheme of the invention, the method also comprises the step of carrying out high performance liquid chromatography identification on the grifola decoction reference substance, the alisol A, the alisol B and the 23-acetyl alisol B.
The embodiment of the invention has the following advantages:
1. the processing mode of decocting and freeze-drying the polyporus umbellatus soup medicinal material is adopted, so that the effective components in the medicinal material are relatively completely extracted, and the mode can be used for mass production and storage, and the field of mass production of the polyporus umbellatus soup is developed;
2. the obtained grifola decoction reference substance is identified by thin-layer chromatography, so that the quality control effect in the whole large-scale production is improved;
3. the preparation method of the test solution and the reference medicinal material solution is relatively simple, the pretreatment steps are few, and partial medicinal materials are tested in multiple ways in one plate, so that the evaluation cost is effectively reduced, and the identification efficiency is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a flow chart of a method for preparing a grifola decoction reference substance according to an embodiment of the present invention;
FIG. 2 is a flow chart of a qualitative detection method according to an embodiment of the present invention;
FIG. 3 is a TLC chart of 365nm of the test solution A, the control solution of Polyporus umbellatus and the control solution of Poria cocos in the present invention;
FIG. 4 is a TLC chart of 365nm after spraying 10% ethanol sulfate solution on the test solution A, the polyporus umbellatus control solution and the poria cocos control solution in the example of the present invention;
FIG. 5 is a TLC chart of the sample solution B, the Alisma orientale control solution and 23-acetyl alisol B in the example of the present invention;
FIG. 6 is an HPLC characteristic spectrum of a Grifola decoction reference substance provided by the embodiment of the present invention;
fig. 7 is a schematic view of the internal structure of a concentration tank according to an embodiment of the present invention;
fig. 8 is a side view of a thickening tank provided by an embodiment of the present invention.
In the figure:
1-tank body; 2-a fin assembly;
11-upright post;
21-a first fin group; 22-a second fin set;
211-a first fin; 221-second fin.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, a method for preparing a grifola decoction reference substance comprises:
s10, processing Polyporus, Poria, rhizoma Alismatis, pulvis Talci, and colla Corii Asini to obtain medicinal liquid;
s20, lyophilizing the medicinal liquid to obtain the basic substance of Polyporus umbellatus decoction.
In a preferred embodiment of the present invention, in order to further improve the lyophilization effect and increase the content of each component in the grifola soup reference substance obtained after lyophilization, step S20 specifically includes:
s21, concentrating the liquid medicine to a relative density of 1.01-1.04 under the conditions that the vacuum degree is-0.090-0.099 MPa and the temperature is 40-60 ℃ to obtain concentrated paste;
s22, sequentially pre-freezing and stage-wise freeze-drying the concentrated paste to obtain the grifola soup reference substance; wherein the content of the first and second substances,
the maximum temperature of the temperature during the prefreezing process is not higher than the minimum temperature during the staged lyophilization operation.
The relative density here is 1.01 to 1.04 of the density of the obtained concentrated paste before concentration of the drug solution.
In a more preferred embodiment, the concentration process may be further limited to better avoid the damage to the active ingredients in the herbs during the concentration process, for example, step S21 specifically includes:
s211, placing the liquid medicine in a concentration tank, vacuumizing and simultaneously heating until the vacuum degree in the concentration tank is-0.090-0.099 MPa and the temperature is 40-60 ℃;
s212, evaporating and concentrating to obtain concentrated paste with the relative density of 1.01-1.04 under the ultrasonic oscillation condition.
Of course, in order to ensure better concentration effect and effectively improve the heat conduction performance in the concentration process, as shown in fig. 7 and 8, the concentration tank comprises a tank body 1 and a fin assembly 2 arranged in the tank body 1; and the number of the first and second electrodes,
the end surface part of the tank body 1 is inwards sunken to form an upright post 11;
the fin assembly 2 is arranged on the side face of the upright post 11 inside the tank body 1, the fin assembly 2 at least comprises a plurality of groups of first fin groups 21 and second fin groups 22 which are arranged at intervals along the axial direction of the upright post 11, each group of the first fin groups 21 comprises a plurality of first fins 211 which are arranged at equal intervals along the circumferential direction, each group of the second fin groups 22 comprises a plurality of second fins 221 which are arranged at equal intervals along the circumferential direction, and the first fins 211 and the second fins 221 are different in shape.
In a further preferred embodiment, in order to enable the first fins 211 and the second fins 221 to ensure effective heat conduction and reduce damage of drug properties caused by unbalanced heat on the premise of improving a concentration effect, the first fins 211 are formed into a rectangular parallelepiped structure extending from the side surfaces of the upright post 11 along the extending direction of the radius of the upright post 11, and the height of the rectangular parallelepiped structure is 1/20-1/10 of the length of the rectangular parallelepiped structure along the extending direction;
the second fins 221 are formed in a fan-shaped ring structure extending from the side surface of the upright post 11 in the extending direction of the radius of the upright post 11, and the height of the fan-shaped ring structure is 1/20-1/10 of the length of the fan-shaped ring structure in the extending direction.
In a more preferred embodiment, the ratio of the grifola, the poria cocos, the rhizoma alismatis, the talc and the donkey-hide gelatin is 1: 0.8-1.2: 0.8-1.2: 0.8-1.2: 0.8 to 1.2; further, step S10 specifically includes:
s11, boiling Polyporus, Poria, Alismatis rhizoma and pulvis Talci in water, decocting for 30-60min, and filtering to obtain filtrate;
s12, adding the donkey-hide gelatin into the filtrate, and melting until the donkey-hide gelatin is dissolved in the filtrate to obtain a liquid medicine.
For example, in a specific embodiment, 13.8-15.6 g of polyporus, poria cocos, rhizoma alismatis and talc are weighed respectively, 800mL of water is added, the mixture is boiled and then decocted for 45 minutes by slow fire, the hot mixture is filtered, 13.8-15.6 g of donkey-hide gelatin is added into the filtrate, and the mixture is melted by heat to obtain a liquid medicine for later use.
In a preferred embodiment of the invention, in order to better retain the effective components of the traditional Chinese medicinal materials in the liquid medicine to the maximum extent through the freeze-drying process, the pre-freezing temperature in the pre-freezing process is-50 to-60 ℃, and the pre-freezing time is 30 to 120 min;
the staged freeze-drying operation comprises a first freeze-drying section, a second freeze-drying section, a third freeze-drying section, a fourth freeze-drying section, a fifth freeze-drying section and a temperature return section which are sequentially arranged; the temperature of the first freeze-drying section is-50 to-40 ℃, the time is 2 to 3 hours, and the pressure is 20 to 25 Pa; the temperature of the second freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is 10 to 15 Pa; the temperature of the third freeze-drying section is-55 to-40 ℃, the time is 3 to 6 hours, and the pressure is 15 to 20 Pa; the temperature of the fourth freeze-drying section is-55 to-40 ℃, the time is 4 to 6 hours, and the pressure is 5 to 10 Pa; the temperature of the fifth freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is 20 to 25 Pa; the temperature return section is heated at a heating rate of 0.2-0.5 ℃/min and simultaneously CO is introduced into the temperature return section2And continuously standing for 1-2 hours until the ambient temperature is 20-30 ℃ and the pressure is 0.9-1.1 atm.
Of course, although there is an overlap in temperature between the first, second, third, fourth and fifth lyophilization sections given, the lyophilization temperature of the first, second, third, fourth and fifth lyophilization sections gradually increases during the same lyophilization operation. By way of example, a similar set up of-50 ℃ in the first lyophilization stage, then-48 ℃ in the second lyophilization stage, -46 ℃ in the third lyophilization stage, -45 ℃ in the fourth lyophilization stage, and-42 ℃ in the fifth lyophilization stage may be used herein.
The invention also provides a qualitative detection method for Chinese herbal medicine components in the grifola decoction reference substance prepared by the preparation method, as shown in figure 2, the method comprises the following steps:
s100, preparing a polyporus umbellatus medicinal material, a poria cocos medicinal material, an rhizoma alismatis medicinal material and 23-acetyl alisol B into control solutions for later use, wherein the control solutions are respectively marked as a polyporus umbellatus control medicinal material solution, a poria cocos control medicinal material solution, an rhizoma alismatis control medicinal material solution and a 23-acetyl alisol B control solution;
s200, preparing two different test solution for later use by taking the grifola decoction reference substance, and respectively recording the two test solution as a test solution A and a test solution B;
s300, taking the polyporus umbellatus reference medicinal material solution, the poria cocos reference medicinal material solution and a sample solution A as a group, taking the rhizoma alismatis reference medicinal material solution, the 23-acetyl alisol B reference solution and the sample solution B as a group, and respectively pointing the groups on the same silica gel G thin-layer plate for chromatographic contrast detection;
s400, obtaining the chromatographic control results of the two groups of silica gel G thin-layer plates respectively for analysis.
Of course, the dosage ratio of each substance can be selected correspondingly according to actual conditions.
In a further preferred embodiment, step S100 or S200 comprises:
s101, mixing a grifola medicinal material, a poria cocos medicinal material and a grifola soup reference substance with one part of diethyl ether respectively, taking residues obtained after filtrate is evaporated to dryness, adding methanol into the residues and mixing to obtain a grifola reference medicinal material solution, a poria cocos reference medicinal material solution and a sample solution A respectively;
s102, mixing the rhizoma alismatis medicinal material and the grifola decoction reference substance with one part of methanol respectively, taking the residue obtained after filtrate is evaporated to dryness, adding the methanol into the residue and mixing to obtain rhizoma alismatis reference medicinal material solution and sample solution B respectively; adding the 23-acetyl alisol B into methanol for mixing to obtain a 23-acetyl alisol B control solution;
step S300 includes:
s301, taking 2-5 mu L of each of the polyporus umbellatus reference medicinal material solution and the poria cocos reference medicinal material solution, taking 20-50 mu L of the sample solution A, dropping the sample solution A on the same silica gel G thin layer plate, taking cyclohexane-ethyl acetate-formic acid with the volume ratio of 8:1:0.1 as a developing agent, developing, airing, and directly placing under 365nm for fluorescence color development or spraying 10% sulfuric acid ethanol, airing, and placing under 365nm for inspection;
s302, taking 2-5 mu L of each of the alisma control medicinal material solution, the 23-acetyl alisol B control solution and the sample solution B, placing the solution on the same silica gel G thin-layer plate, developing by taking cyclohexane-ethyl acetate as a developing agent in a volume ratio of 1:1, airing, spraying a 2% vanillin-sulfuric acid solution, heating at 105 ℃ until spots are clear, and inspecting.
In a preferred group of embodiments of the present invention, the method further comprises performing high performance liquid chromatography identification on the grifola decoction reference substance and alisol A, alisol B and 23-acetyl alisol B.
It is further described that the following specific methods can be further used for the identification by high performance liquid chromatography: taking 1.0g of the grifola decoction reference substance, precisely weighing, placing in a conical flask with a stopper, adding 50mL of acetone or acetonitrile, sealing the stopper, ultrasonically treating for 30 minutes, cooling, filtering, evaporating the filtrate to dryness, dissolving the residue in 80% acetonitrile, diluting to a constant volume of 5mL, and filtering to obtain a solution to be identified; taking a proper amount of alisol A, alisol B and 23-acetyl alisol B, precisely weighing, adding acetonitrile for dissolving, and preparing a mixed solution containing 40 mu g of alisol A, 25 mu g of alisol B and 23 mu g of 23-acetyl alisol B per 1mL as a reference solution; precisely absorbing 20 μ L of each of the reference solution and the solution to be identified, injecting into a college liquid chromatograph, and measuring according to the following chromatographic conditions:
octadecylsilane chemically bonded silica was used as a filler (column length 250mm, inner diameter 4.6mm, particle diameter 5 μm), acetonitrile was used as a mobile phase A, and 0.2% phosphoric acid solution was used as a mobile phase B, and gradient elution was carried out.
Flow rate: 1.0 mL/min; detection wavelength: 208 nm; column temperature: at 30 ℃. The theoretical plate number is not less than 4000 based on alisol B. Of course, the specific values of the content and the time are not limited to the above, and those skilled in the art can adjust them within a suitable range.
The following is a further description by way of specific examples.
Examples
Preparing a grifola soup reference substance:
putting 13.8g of polyporus, poria cocos, rhizoma alismatis and talc into a 2L decoction kettle respectively, adding 800mL of water, boiling, decocting for 45 minutes with slow fire, filtering while hot, adding 13.8g of donkey-hide gelatin into the filtrate, and melting to obtain a liquid medicine; concentrating the obtained medicinal liquid in 1000mL eggplant-shaped bottle (vacuum degree-0.090-0.099 MPa), and concentrating at 60 deg.C to obtain concentrated solution of 1.01-1.04g/mL (density value at 20 deg.C); placing the concentrated solution in a 1000ml eggplant-shaped bottle, pre-freezing for 30 minutes, placing the bottle on a freeze dryer, and drying for 24 hours at the temperature of between 45 ℃ below zero and 50 ℃ below zero and under the pressure of no more than 25Pa to obtain five batches of agaric soup reference substances A1, A2, A3, A4 and A5. Wherein A4 is the standard substance of Polyporus umbellatus decoction obtained by directly lyophilizing at-50 deg.C for 24 hr without staged lyophilization.
Detection example 1
Detection of the grifola and the poria cocos:
weighing 2.0g of the Grifola decoction reference substance prepared in the example, adding diethyl ether 50mL, performing ultrasonic treatment for 10 min, filtering, evaporating the filtrate to dryness, and adding methanol 1mL into the residue to dissolve to obtain a sample solution A;
taking poria cocos reference medicinal material and grifola umbellata medicinal material 1.0g respectively, and preparing poria cocos reference medicinal material solution and grifola umbellata reference medicinal material solution according to the method of the test solution A;
respectively sucking Poria contrast medicinal material solution and Polyporus contrast medicinal material solution 2-5 μ L, respectively, and sample solution A20-50 μ L, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate-formic acid (8:1:0.1) as developing agent, air drying, and directly placing at 365nm for fluorescence development, or spraying with 10% sulphuric acid ethanol, air drying, and placing at 365nm for fluorescence development. (wherein, the TLC chart of fluorescence coloration directly under 365nm is shown in figure 3, the TLC chart of coloration after spraying with ethanol sulfate is shown in figure 4, wherein, the first strip from left to right in figures 3 and 4 is the solution of Grifola contrast medicinal material, the second strip is the solution of Poria contrast medicinal material, the third to fifth strips correspond to the standard substances A1, A2 and A3 of Grifola soup in sequence, the sixth strip is the freeze-dried powder without Grifola, the seventh strip is the freeze-dried powder without Poria, and the eighth strip is the freeze-dried powder without Grifola and Poria)
Detection example 2
And (3) detection of rhizoma alismatis:
weighing 2.0g of the standard substance of Polyporus decoction prepared in example, adding 50mL of methanol, ultrasonic dissolving, filtering, evaporating filtrate, adding 1mL of methanol into residue, dissolving to obtain sample solution B;
taking another 1g of rhizoma alismatis medicinal material, and preparing rhizoma alismatis reference medicinal material solution according to the method of the test solution B; adding methanol into 23-acetyl alisol B to obtain 23-acetyl alisol B control solution;
respectively sucking 2 μ L of medicinal material sample solution and 5 μ L of sample solution, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate (1:1) as developing agent, air drying, spraying 2% vanillin sulfuric acid solution, and heating at 105 deg.C until spots are clear. (the TLC chart obtained is shown in FIG. 5, wherein the first band from left to right is 23-acetyl alisol B control solution, the second band is alisma rhizome control solution, the third to fifth bands correspond to grifola decoction reference substances A1, A2 and A3 in sequence, and the sixth and seventh bands are freeze-dried powder without alisma rhizome)
Detection example 3
Establishing an HPLC characteristic spectrum:
taking 1.0g of the grifola decoction reference substance prepared in the embodiment, precisely weighing, placing in a conical flask with a stopper, adding 50mL of acetone, sealing the stopper, carrying out ultrasonic treatment for 30 minutes, cooling, filtering, evaporating the filtrate to dryness, dissolving the residue in 80% acetonitrile, fixing the volume to 5mL, filtering, and taking the filtrate as a liquid to be identified;
taking a proper amount of alisol A, alisol B and 23-acetyl alisol B, precisely weighing, adding acetonitrile for dissolving, and preparing a mixed solution containing 40 mu g of alisol A, 25 mu g of alisol B and 23 mu g of 23-acetyl alisol B per 1mL as a reference solution;
20 μ L of each of the reference solution and the sample solution was precisely aspirated and injected into a liquid chromatograph of university, and the obtained HPLC characteristic spectrum is shown in FIG. 6. As shown in fig. 6, the characteristic spectrum of the solution to be identified shows 8 characteristic peaks, wherein 3 peaks have the same retention time as the corresponding reference peak.
Detection example 4
Detecting water content, sample yield, thin layer identification, characteristic map and content measurement in the prepared standard substances A1, A2, A3, A4 and A5 of the grifola soup material. Detecting water content by conventional method, and calculating sample yield according to the ratio of the obtained standard substance of Polyporus decoction to the total weight of medicinal materials. The amino acid content is detected according to a donkey-hide gelatin item determination method (part of the 'Chinese pharmacopoeia' 2015 edition). The results of the tests are shown in Table 1.
TABLE 1
As can be seen from the above table, the preparation method and the detection method of the invention can well control the quality of the prepared grifola soup reference substance, and the yield and the amino acid content are effectively maintained. In addition, the yield and the amino acid content of A4 without the step-wise freeze-drying operation are relatively low compared with other grifola soup reference substances.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a grifola decoction reference substance is characterized by comprising the following steps:
s10, processing Polyporus, Poria, rhizoma Alismatis, pulvis Talci, and colla Corii Asini to obtain medicinal liquid;
s20, lyophilizing the medicinal liquid to obtain the basic substance of Polyporus umbellatus decoction.
2. The method for preparing the grifola decoction reference substance according to claim 1, wherein the step S20 specifically comprises:
s21, concentrating the liquid medicine to a relative density of 1.01-1.04 under the conditions that the vacuum degree is-0.090-0.099 MPa and the temperature is 40-60 ℃ to obtain concentrated paste;
s22, sequentially pre-freezing and stage-wise freeze-drying the concentrated paste to obtain the grifola soup reference substance; wherein the content of the first and second substances,
the maximum temperature of the temperature during the prefreezing process is not higher than the minimum temperature during the staged lyophilization operation.
3. The method for preparing the grifola decoction reference substance according to claim 2, wherein the step S21 specifically comprises:
s211, placing the liquid medicine in a concentration tank, vacuumizing and simultaneously heating until the vacuum degree in the concentration tank is-0.090-0.099 MPa and the temperature is 40-60 ℃;
s212, evaporating and concentrating to obtain concentrated paste with the relative density of 1.01-1.04 under the ultrasonic oscillation condition.
4. The method for preparing a grifola soup reference substance according to claim 3, wherein the concentration tank comprises a tank body (1) and a fin assembly (2) disposed in the tank body (1); and the number of the first and second electrodes,
the end surface part of the tank body (1) is inwards sunken to form an upright post (11);
the fin component (2) is arranged on the side face of a vertical column (11) inside the tank body (1), the fin component (2) at least comprises a plurality of groups of first fin groups (21) and second fin groups (22) which are arranged at intervals along the axial direction of the vertical column (11), each group of the first fin groups (21) comprises a plurality of first fins (211) which are arranged at equal intervals along the circumferential direction, each group of the second fin groups (22) comprises a plurality of second fins (221) which are arranged at equal intervals along the circumferential direction, and the first fins (211) and the second fins (221) are different in shape.
5. The method for preparing the grifola soup reference substance as claimed in claim 4, wherein the first fin (211) is formed as a rectangular parallelepiped structure extending from a side surface of the pillar (11) in an extending direction of a radius of the pillar (11), and a height of the rectangular parallelepiped structure is 1/20-1/10 of a length of the rectangular parallelepiped structure in the extending direction;
the second fin (221) is formed into a fan-shaped ring structure extending from the side surface of the upright post (11) along the extending direction of the radius of the upright post (11), and the height of the fan-shaped ring structure is 1/20-1/10 of the length of the fan-shaped ring structure along the extending direction.
6. The method for preparing the grifola decoction reference substance according to any one of claims 1 to 4, wherein the ratio of the dosages of the grifola, the poria cocos, the alisma orientale, the talc and the donkey-hide gelatin is 1: 0.8-1.2: 0.8-1.2: 0.8-1.2: 0.8 to 1.2; further, step S10 specifically includes:
s11, boiling Polyporus, Poria, Alismatis rhizoma and pulvis Talci in water, decocting for 30-60min, and filtering to obtain filtrate;
s12, adding the donkey-hide gelatin into the filtrate, and melting until the donkey-hide gelatin is dissolved in the filtrate to obtain a liquid medicine.
7. The method for preparing the grifola decoction reference substance according to claim 2, wherein the pre-freezing temperature in the pre-freezing process is-50 to-60 ℃, and the pre-freezing time is 30 to 120 min;
the staged freeze-drying operation comprises a first freeze-drying section, a second freeze-drying section, a third freeze-drying section, a fourth freeze-drying section, a fifth freeze-drying section and a temperature return section which are sequentially arranged; the temperature of the first freeze-drying section is-50 to-40 ℃, the time is 2 to 3 hours, and the pressure is 20 to 25 Pa; the temperature of the second freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is10-15 Pa; the temperature of the third freeze-drying section is-55 to-40 ℃, the time is 3 to 6 hours, and the pressure is 15 to 20 Pa; the temperature of the fourth freeze-drying section is-55 to-40 ℃, the time is 4 to 6 hours, and the pressure is 5 to 10 Pa; the temperature of the fifth freeze-drying section is-55 to-40 ℃, the time is 6 to 8 hours, and the pressure is 20 to 25 Pa; the temperature return section is heated at a heating rate of 0.2-0.5 ℃/min and simultaneously CO is introduced into the temperature return section2And continuously standing for 1-2 hours until the ambient temperature is 20-30 ℃ and the pressure is 0.9-1.1 atm.
8. A qualitative detection method for herbal ingredients in the standard substance of Grifola decoction prepared by the method according to any one of claims 1 to 7, comprising:
s100, preparing a polyporus umbellatus medicinal material, a poria cocos medicinal material, an rhizoma alismatis medicinal material and 23-acetyl alisol B into control solutions for later use, wherein the control solutions are respectively marked as a polyporus umbellatus control medicinal material solution, a poria cocos control medicinal material solution, an rhizoma alismatis control medicinal material solution and a 23-acetyl alisol B control solution;
s200, preparing two different test solution for later use by taking the grifola decoction reference substance, and respectively recording the two test solution as a test solution A and a test solution B;
s300, taking the polyporus umbellatus reference medicinal material solution, the poria cocos reference medicinal material solution and a sample solution A as a group, taking the rhizoma alismatis reference medicinal material solution, the 23-acetyl alisol B reference solution and the sample solution B as a group, and respectively pointing the groups on the same silica gel G thin-layer plate for chromatographic contrast detection;
s400, obtaining the chromatographic control results of the two groups of silica gel G thin-layer plates respectively for analysis.
9. The method for qualitatively detecting herbal components in the grifola decoction reference substance as set forth in claim 8, wherein step S100 or S200 includes:
s101, mixing a grifola medicinal material, a poria cocos medicinal material and a grifola soup reference substance with one part of diethyl ether respectively, taking residues obtained after filtrate is evaporated to dryness, adding methanol into the residues and mixing to obtain a grifola reference medicinal material solution, a poria cocos reference medicinal material solution and a sample solution A respectively;
s102, mixing the rhizoma alismatis medicinal material and the grifola decoction reference substance with one part of methanol respectively, taking the residue obtained after filtrate is evaporated to dryness, adding the methanol into the residue and mixing to obtain rhizoma alismatis reference medicinal material solution and sample solution B respectively; adding the 23-acetyl alisol B into methanol for mixing to obtain a 23-acetyl alisol B control solution;
step S300 includes:
s301, taking 2-5 mu L of each of the polyporus umbellatus reference medicinal material solution and the poria cocos reference medicinal material solution, taking 20-50 mu L of the sample solution A, dropping the sample solution A on the same silica gel G thin layer plate, taking cyclohexane-ethyl acetate-formic acid with the volume ratio of 8:1:0.1 as a developing agent, developing, airing, and directly placing under 365nm for fluorescence color development or spraying 10% sulfuric acid ethanol, airing, and placing under 365nm for inspection;
s302, taking 2-5 mu L of each of the alisma control medicinal material solution, the 23-acetyl alisol B control solution and the sample solution B, placing the solution on the same silica gel G thin-layer plate, developing by taking cyclohexane-ethyl acetate as a developing agent in a volume ratio of 1:1, airing, spraying a 2% vanillin-sulfuric acid solution, heating at 105 ℃ until spots are clear, and inspecting.
10. The method of claim 8 or 9, further comprising performing high performance liquid chromatography identification on the grifola decoction reference substance and alisol A, alisol B and 23-acetyl alisol B.
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