CN115327001A - Ficus simplicissima lour formula particle contrast extract and preparation method thereof - Google Patents
Ficus simplicissima lour formula particle contrast extract and preparation method thereof Download PDFInfo
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- CN115327001A CN115327001A CN202210490231.XA CN202210490231A CN115327001A CN 115327001 A CN115327001 A CN 115327001A CN 202210490231 A CN202210490231 A CN 202210490231A CN 115327001 A CN115327001 A CN 115327001A
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- 239000000284 extract Substances 0.000 title claims abstract description 130
- 239000002245 particle Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000000605 extraction Methods 0.000 title claims abstract description 9
- 241001578027 Ficus simplicissima Species 0.000 title 1
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 34
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 239000008187 granular material Substances 0.000 claims description 29
- 238000001514 detection method Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 21
- 239000000706 filtrate Substances 0.000 claims description 14
- ZCCUUQDIBDJBTK-UHFFFAOYSA-N psoralen Chemical group C1=C2OC(=O)C=CC2=CC2=C1OC=C2 ZCCUUQDIBDJBTK-UHFFFAOYSA-N 0.000 claims description 14
- 238000001228 spectrum Methods 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- VXGRJERITKFWPL-UHFFFAOYSA-N 4',5'-Dihydropsoralen Natural products C1=C2OC(=O)C=CC2=CC2=C1OCC2 VXGRJERITKFWPL-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000007689 inspection Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000003809 water extraction Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- AUALQMFGWLZREY-UHFFFAOYSA-N acetonitrile;methanol Chemical compound OC.CC#N AUALQMFGWLZREY-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 35
- 244000173782 Ficus hirta Species 0.000 description 26
- 239000003814 drug Substances 0.000 description 20
- 239000002994 raw material Substances 0.000 description 11
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- 241001631271 Prunus fasciculata Species 0.000 description 4
- 239000013558 reference substance Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
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- 239000012925 reference material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000009429 Ginkgo biloba extract Substances 0.000 description 1
- 241000218231 Moraceae Species 0.000 description 1
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- 238000010812 external standard method Methods 0.000 description 1
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- 235000020686 ginkgo biloba extract Nutrition 0.000 description 1
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- 239000002075 main ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- -1 n-hexane-trichloromethane-ethyl acetate-formic acid Chemical compound 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention provides a preparation method of a hispid fig formula particle control extract, which comprises the steps of respectively carrying out extraction, concentration and low-temperature drying on multiple batches of hispid fig powder for multiple times to obtain different batches of hispid fig extracts, and then blending the different batches of hispid fig extracts to obtain the hispid fig formula particle control extract. The preparation method of the hispid fig formula particle contrast extract is simple and convenient to operate, low in cost, good in repeatability and high in extraction rate; the preparation method is used for preparing the hispid fig formula particle control extract, so that the consistency of different batches of hispid fig formula particle control extracts is ensured, and the hispid fig formula particle control extract has stable and uniform properties and is convenient to use; the thin-layer chromatography fingerprint and the HPLC fingerprint of the contrast extract finally obtained by adopting the preparation method of the hispid fig formula particle contrast extract are consistent with each other.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine quality control, in particular to a control extract of hispid fig formula granules, a preparation method and application thereof.
Background
The quality control mode of the traditional Chinese medicine is basically along the development of natural medicinal chemistry, an analysis method for taking one or more active ingredients of the traditional Chinese medicine as targets and the concept of qualitative and quantifiable quality standard, the quality control method of foreign plant medicines is referred, the mode of chemical medicine quality control is referred, corresponding simple physicochemical identification is established by means of literature reports, and the quality standard of identification and content determination mainly based on spectrum and chromatogram is developed.
Each Chinese medicinal material is a multi-component complex, which determines the unique integrity and fuzziness of the Chinese medicinal material, and also shows that the evaluation method of taking one, two or even a plurality of components in the Chinese medicinal material as the quality of the Chinese medicinal material has great limitation. The 1990 edition of Chinese pharmacopoeia increases the thin-layer chromatography identification of reference medicinal materials, so that the identification of traditional Chinese medicines and Chinese patent medicines has great progress. At present, chinese medicine and foreign herbal medicine pay more and more attention to the detection of multiple components or multiple components, such as the quality control of German ginkgo biloba extract. The analysis method of the fingerprint spectrum can carry out quality control on the medicinal materials on the whole, and still has great research value at present.
At present, chinese pharmacopoeia has two kinds of reference substances, namely a chemical reference substance and a traditional Chinese medicine reference medicinal material, in the aspect of controlling the quality of medicinal materials. The chemical reference substance can be used for qualitative identification and quantitative analysis of medicinal materials, and the traditional Chinese medicine reference medicinal material can be used for microscopic identification and thin-layer identification. However, both chemical reference substances and traditional Chinese medicine reference medicinal materials have limitations in traditional Chinese medicine quality control. The limitation is shown in that chemical components in the traditional Chinese medicine are diversified, single or a plurality of compounds cannot reflect the whole appearance of the medicinal materials, and the existing standard has a plurality of holes which are sometimes generated due to the phenomenon of sub-optimal effect; 2. the traditional Chinese medicine reference medicinal materials are influenced by the producing area and the growth environment, the quality consistency of each batch is difficult to ensure, and the traditional Chinese medicine reference medicinal materials can only be used for qualitative identification and cannot reflect the content of the medicinal material components.
The traditional Chinese medicine control extract is an extract which is prepared from traditional Chinese medicinal materials, has stable properties and components and can be used for qualitative or quantitative analysis, wherein Mr. Xie Peishan provides four basic requirements (ASCS) for the traditional Chinese medicine control extract, and the control extract also has the basic conditions: the herbal material source is reliable and representative; specificity, specificity of the detection method used; con-static, the control extracts should remain consistent from batch to batch; stability, stable and uniform properties and convenient use. The method can be used for qualitative identification of medicinal materials by using high performance thin layer chromatography fingerprint, high performance liquid chromatography fingerprint and other methods, and the control extract marked by an external standard method can be further used for semi-quantitative and quantitative analysis and detection. The traditional Chinese medicine control extract has important significance for controlling the quality of the traditional Chinese medicine.
Disclosure of Invention
In view of the above, there is a need for a control extract of hispid fig granule, and a preparation method and application thereof. The invention provides a preparation method of a hispid fig formula particle contrast extract, which has the advantages of simple and convenient operation, low cost, good repeatability and high extraction rate; the invention also provides a hispid fig formula particle contrast extract prepared by the preparation method of the hispid fig formula particle contrast extract, and the prepared hispid fig formula particle contrast extract has good consistency, stable and uniform properties, is convenient to use and can reflect the overall appearance.
The invention provides a preparation method of a hispid fig formula particle contrast extract, which comprises the following steps:
step one, water extraction, wherein the water extraction comprises the following steps:
a) Mixing hispid fig powder with water, decocting, and filtering to obtain filtrate 1 and residue 1;
b) Repeating the step a) on the filter residue 1 to obtain a filtrate 2 and a filter residue 2, repeating the step a) on the obtained filter residue 2, repeating the step a) by the analogy of the step b) for N times to obtain a filtrate N +1 and a filter residue N +1;
c) Mixing the filtrate 1 to (N + 1) to obtain an extracting solution 1, and concentrating the extracting solution 1 at low temperature to obtain the dry extract of the hispid fig;
step two, preparing the hispid fig extract: dissolving the hispid fig dry paste obtained in the step two in water to obtain a hispid fig dry paste water solution, adding auxiliary materials, drying at low temperature and sieving to obtain a hispid fig extract;
step three, blending: and blending the hispid fig extracts of different batches to obtain the reference hispid fig granule extract.
The temperature adopted for low-temperature drying in the preparation process is 20-60 ℃.
The hispid fig extracts of different batches are blended, and it can be understood that there are at least fifteen batches of hispid fig extracts.
Preferably, in the first step, N is more than or equal to 8 and more than or equal to 0, and N is an integer.
Preferably, N in the above step one is 1.
Preferably, the weight-to-volume ratio of the hispid fig powder to the water in the first step is 1:5-1, and the unit of the weight-to-volume ratio is g/mL.
More preferably, the weight volume ratio of the hispid fig powder to the water in the step one is 1:10.
preferably, the decocting time in the step one is 1-300 min.
More preferably, the decocting time in the above step one is 30min.
Preferably, the filtration in the first step is performed by using medium-speed filter paper or a filter bag.
More preferably, the filtration in the first step is filtration with a filter bag.
Preferably, the aperture of the filter bag in the step one is 10-200 μm.
More preferably, the aperture of the filter bag in the first step is 10 μm.
Preferably, the weight-volume ratio of the dry extract of hispid fig to water in the second step is 1:5-1. The unit of the weight-volume ratio is g/mL.
More preferably, the weight-to-volume ratio of the dry extract of hispid fig to water in the second step is 1:5.
Preferably, the weight of the auxiliary materials is 20 to 60 percent of the weight of the dry extract of the radix fici simplicissimae.
More preferably, the weight of the auxiliary materials is 30% of the weight of the dry extract of the radix fici simplicissimae.
Preferably, the auxiliary material is aerosil.
Preferably, the second step is carried out at low temperature and then filtered by a sieve of 90-200 meshes.
More preferably, the low-temperature drying in the second step is performed by passing through a 110-mesh screen.
Preferably, a preparation pretreatment step of detecting different batches of the hispid fig extract by thin layer chromatography and/or high performance liquid chromatography is further included between the second step and the fourth step.
In a second aspect, the invention provides a hispid fig formula particle control extract, which is obtained by the preparation method.
Preferably, the above Ficus Simplicissima lour formula granule control extract has a consistent spectrum obtained by thin layer chromatography and/or high performance liquid chromatography.
Preferably, the spectrum of the above Ficus Simplicissima formula granule control extract obtained by thin layer chromatography and/or high performance liquid chromatography is consistent with the spectrum of Ficus Simplicissima granules at the position of psoralen.
Preferably, the above-mentioned Ficus Simplicissima formula granule control extract contains psoralen as the main ingredient.
In a third aspect, the invention provides the application of the above-mentioned radix fici simplicissimae formula particle control extract in identification.
Preferably, the quality control method comprises: detecting the above-mentioned radix fici Simplicissimae formula granule control extract by thin layer chromatography and/or high performance liquid chromatography, and comparing and judging.
Preferably, the thin layer chromatography and/or high performance liquid chromatography is used for detecting the main components of the control extract and the main components of the formula granules of the hispid fig, wherein the main components comprise psoralen.
Preferably, when the above-mentioned five-finger wild peach formula particle control extract is detected by thin-layer chromatography, the five-finger wild peach formula particle control extract needs to be prepared into a solution for detection, wherein the preparation method of the five-finger wild peach formula particle control extract solution comprises: weighing 0.1-0.5 g of the hispid fig formula particle control extract of claim 6, adding 10-40 mL of water to dissolve, adding ether to shake and extract for 1-3 times, 10-30 mL each time, combining ether solutions, volatilizing, adding 0.5-2 mL of ethanol to dissolve residues, and filtering through a 0.12-0.32 μm filter membrane to obtain a hispid fig formula particle control extract solution;
preferably, 0.25g of the control extract of the hispid fig formula particles is weighed, 30ml of water is added for dissolving, the mixture is shaken and extracted for 2 times by using ether, 30ml of each time, the ether solution is combined and volatilized to be dry, 0.5ml of ethanol is added for dissolving the residue, and the solution is filtered by a 0.22 mu m filter membrane to obtain the control extract solution of the hispid fig formula particles;
further, the preparation method of the solution to be detected in the thin layer chromatography comprises the following steps: grinding a product to be detected, weighing 1-3 g, adding 10-40 mL of water to dissolve, shaking and extracting for 1-3 times by using ether, 10-30 mL of ether liquid each time, combining the ether liquid, volatilizing, adding 0.5mL of ethanol to dissolve residues, and filtering through a 0.12-0.32 mu m filter membrane to obtain a solution of the product to be detected;
preferably weighing 2g of product to be detected, adding 30ml of water to dissolve, extracting with diethyl ether for 2 times (30 ml each time), mixing diethyl ether solution, volatilizing, dissolving the residue with 0.5ml of ethanol, and filtering with 0.22 μm filter membrane to obtain the solution of product to be detected.
Preferably, the detection condition of the thin layer chromatography is one or two, and the one is:
thin-layer plate: TLC G60 precast slab;
sample application: control extract solution of radix fici simplicissimae formula granules: 10. Mu.l, solution: 1.5 mul of strip-like sample application;
developing agent:
n-hexane-trichloromethane-ethyl acetate-glacial acetic acid (20: 4: 7: 1)
And (3) inspecting:
the sample was examined under an ultraviolet lamp (365 nm).
The second detection condition is as follows:
thin-layer plate: TLC G60 precast slab;
sample application: control extract solution of radix fici simplicissimae formula granules: 10. Mu.l, solution: 1.5 mul of strip-like sample application;
developing agent: toluene-ethyl acetate-formic acid-water (20: 1) at 10 deg.C;
and (3) inspecting: and (5) placing under an ultraviolet lamp (365 nm) for inspection.
Optionally, when the above-mentioned hispid fig formula granule control extract is detected by high performance liquid chromatography, the hispid fig formula granule control extract needs to be prepared into a solution for detection, wherein the preparation method of the hispid fig formula granule control extract solution is as follows: adding methanol into the hispid fig formula particle control extract of claim 6 to prepare a hispid fig formula particle control extract methanol solution with the concentration of 2mg/mL-15mg/mL, and filtering with a 0.12-0.32 μm filter membrane to obtain the hispid fig formula particle control extract solution.
Preferably, the concentration of the methanol solution of the control extract of the hispid fig formula particles is 10mg/mL; the filter was 0.22 μm.
Further, in the detection by the high performance liquid chromatography, the preparation method of the solution to be detected comprises the following steps: grinding a product to be detected, weighing 0.1-2 g, adding 5-50 mL of methanol, carrying out ultrasonic treatment for 30-60 min with the power of 100W-3 kW, shaking up, filtering with a 0.12-0.32 mu m filter membrane, and taking the subsequent filtrate to obtain a solution of the product to be detected.
Preferably weighing 0.2g of the product to be detected, adding 20mL of methanol, carrying out ultrasonic treatment for 30min at the power of 500W, shaking up, and filtering through a 0.22 mu m filter membrane to obtain the solution of the product to be detected.
Preferably, the detection conditions of the high performance liquid chromatography described above are:
a chromatographic instrument: thermo Fisher U3000 high performance liquid chromatograph;
a detector: a Thermo Fisher DAD detector;
and (3) chromatographic column: waters Symmetry C18.6 mm x 250,5 μm
Mobile phase: (a) acetonitrile-methanol (3:1); (B) 0.1% phosphoric acid solution
Gradient of mobile phase:
detection wavelength: 254nm; the flow rate is 1ml/min; the sample amount is 10 mul; the column temperature is 35 ℃; operating time: 40min;
the invention has the following beneficial effects:
the preparation method of the hispid fig formula particle control extract adopts the steps of extracting, preparing the hispid fig extract and blending, and has the advantages of simple and convenient operation, low cost, good repeatability and high extraction rate. The reference extract of the hispid fig formula particles prepared by the preparation method is prepared from different batches of extracts, so that the defect that the quality of each batch is difficult to ensure to be consistent due to the influence of production areas and growth environments on traditional Chinese medicine reference medicinal materials is overcome, and the consistency of the reference extracts of the hispid fig formula particles of different batches is ensured; the character is stable and uniform and is convenient to use; the thin-layer chromatography fingerprint and the HPLC fingerprint of the contrast extract finally obtained by adopting the preparation method of the hispid fig formula particle contrast extract are consistent with each other.
The invention also provides an identification method or a quality control method of the hispid fig, which can carry out qualitative identification.
Drawings
FIG. 1 is a thin-layer chromatogram obtained by performing thin-layer chromatography on Ficus Simplicissima lour raw material with Ficus Simplicissima lour reference medicinal material as reference substance. 1 is a radix fici simplicissimae reference medicinal material, 2-16 correspond to radix fici simplicissimae sequentially: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
FIG. 2 is a thin-layer chromatogram obtained by performing thin-layer chromatography on Ficus Simplicissima lour raw material with Ficus Simplicissima lour reference medicinal material as reference substance. 1 is a radix fici simplicissimae reference medicinal material, 2-16 correspond to radix fici simplicissimae sequentially: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
FIG. 3 is a HPLC fingerprint chromatogram overlay obtained by high performance liquid chromatography of Ficus Simplicissima lour raw material, wherein R corresponds to Ficus Simplicissima lour common mode (common mode), and 1-15 correspond to Ficus Simplicissima lour in sequence: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
Fig. 4 is a flow chart of the preparation of the hispid fig formulation granule control extract of the present invention.
FIG. 5 shows the fingerprint spectrum measured by HPLC and the common mode spectrum of 15 batches of Ficus simplicissima lour extract, ERS corresponding to the control extract of Ficus simplicissima lour formula granule, and R is the common mode of 15 batches of Ficus simplicissima lour extract.
Detailed Description
The following describes in detail embodiments of the present invention. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The following examples use the following sources of instruments and materials:
the medicinal material to be used for preparing the control extract is hispid fig.
Thermo Fisher U3000 HPLC, thermo Fisher DAD detector.
Acetonitrile chromatographically pure (Merck).
The purity of the methanol not marked by the invention is more than or equal to 99.5 percent.
The proportion of the developing solvent and the mobile phase is volume ratio.
Toluene, ethyl acetate, methanol, ethanol, diethyl ether, formic acid, n-hexane, and chloroform were all analytically pure (Guangzhou chemical reagent plant).
Psoralen reference substance (China institute for testing and drug administration, batch No. 110739-201918, marked content is more than or equal to 99.6%);
wuzhimaotao reference medicine (China institute for testing and drug products; batch No. 121486-201202)
Testing raw materials (decoction pieces) of radix fici simplicissimae:
15 batches of radix fici simplicissimae are purchased in various large medicinal material markets in China: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
Example 1: screening of Ficus Simplicissima lour raw material
This example provides a method for screening the raw materials of a control extract of hispid fig granule of the present invention.
Analyzing and screening Ficus Simplicissima lour by thin layer chromatography and high performance liquid chromatography with Ficus Simplicissima lour reference material as reference material.
Ficus hirta Vahl is purchased from various major medicinal material markets in China, and is identified as dry root of Moraceae plant Ficus hirta Vahl by the plant research institute of Chinese medical academy. The identified 15 batches of medicinal materials can be used for standby after meeting the standard.
1 thin layer chromatography
1.1 sample preparation
Raw material solution: weighing Ficus simplicissima lour (1-15) powder, weighing each powder precisely 10g, adding diethyl ether 40mL, sealing, performing ultrasonic treatment for 30min at power of 500w, filtering with medium speed filter paper 30-50 μm, volatilizing diethyl ether from filtrate, and dissolving residue with ethanol 0.5 mL.
Control solution: weighing herba fici Simplicissimae reference medicinal material powder 10g each, adding diethyl ether 40mL, sealing, and performing ultrasonic treatment for 30min at power of 500w, filtering with medium speed filter paper 30-50 μm, volatilizing diethyl ether from filtrate, and dissolving residue with ethanol 0.5 mL.
The detection conditions were as follows:
the method comprises the following steps:
thin-layer plate: TLC G60 precast slab;
sample application: 7.5 mul, strip-shaped spotting;
developing agent: n-hexane-trichloromethane-ethyl acetate-formic acid (20: 4: 5: 0.7)
And (6) inspection: the sample was examined under an ultraviolet lamp (365 nm).
The second method comprises the following steps:
thin-layer plate: TLC G60 precast slab;
sample application: 7.5 mul, spot in a strip shape;
developing agent: toluene-Ethyl acetate-formic acid-Water (20: 1) supernatant solution which was separated at 10 deg.C
And (6) inspection: the sample was examined under an ultraviolet lamp (365 nm).
The detection results are shown in fig. 1-2, in which fig. 1 shows the thin-layer chromatogram observed under an ultraviolet lamp (365 nm) after the first method is developed, and fig. 2 shows the thin-layer chromatogram observed under ultraviolet light (365 nm) after the second method is developed. Fig. 1 and 2:1 is a radix fici simplicissimae reference medicinal material, 2-16 are corresponding to the radix fici simplicissimae in sequence: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
2 high performance liquid chromatography
2.1 sample preparation
Raw material solution: precisely weighing 2g of hispid fig (1-15) powder, placing into a conical flask with a plug, adding 25mL of 70% methanol, performing ultrasonic treatment for 30min at a power of 500W, cooling, and filtering with 0.22 μm filter membrane to obtain a raw material solution.
2.2 high Performance liquid chromatography detection
The detection conditions of the high performance liquid chromatography are as follows:
chromatography apparatus: thermo Fisher U3000 high performance liquid chromatograph;
a detector: a Thermo Fisher DAD detector;
a chromatographic column: agilent Eclipse XDB-C18.6 mm × 250,5 μm
Mobile phase: (a) acetonitrile-methanol (3:1); (B) 0.1% phosphoric acid solution;
gradient of mobile phase:
detection wavelength: 254nm; the flow rate is 1ml/min; the sample amount is 10 mul; the column temperature is 35 ℃; operating time: 40min;
the detection method of the high performance liquid chromatography comprises the following steps: the raw material solutions were injected into a liquid chromatograph in an amount of 10. Mu.l each.
And (3) detecting results by high performance liquid chromatography:
measuring, and recording chromatogram to obtain HPLC fingerprint chromatogram overlay shown in figure 3, wherein R corresponds to Ficus Simplicissima lour common mode (common mode), and S1-S15 correspond to Ficus Simplicissima lour in sequence: 1 part of hispid fig, 2 parts of hispid fig, 3 parts of hispid fig, 4 parts of hispid fig, 5 parts of hispid fig, 6 parts of hispid fig, 7 parts of hispid fig, 8 parts of hispid fig, 9 parts of hispid fig, 10 parts of hispid fig, 11 parts of hispid fig, 12 parts of hispid fig, 13 parts of hispid fig, 14 parts of hispid fig and 15 parts of hispid fig.
As can be seen from fig. 3, the fingerprint spectrums of Ficus Simplicissima 1-15 have high consistency, so that a common fingerprint spectrum mode of Ficus Simplicissima medicinal materials is established, and similarity analysis is performed on all samples. And (3) according to the common mode map, performing similarity evaluation on 15 batches of hispid fig raw medicinal materials by adopting an included angle cosine algorithm according to each sample component and the peak area thereof, wherein the result is shown in table 1.
TABLE 1
According to the similarity analysis results, the similarity of 15 batches of hispid fig is very high, and the hispid fig can be selected as the raw material of the hispid fig formula particle control extract.
Example 2: preparation of control extract of radix fici Simplicissimae formula granule
This example provides a method for preparing a control extract of hispid fig granule of the present invention, the flow chart of which is shown in fig. 4.
Firstly, the method comprises the following steps: extraction of
Selecting multiple batches of hispid fig to prepare powder, then respectively adding water with the volume being 10 times of the mass of the hispid fig (namely the solid-to-liquid ratio is 1 (w/V, g/ml)), decocting for 30min, filtering by using a 10-micron filter bag, collecting filter residue 1 and filtrate 1, extracting the filter residue 1 once again by using the same method, combining the filtrate collected by re-extraction with the filtrate 1 to obtain an extracting solution, and concentrating a solvent of the extracting solution to obtain the hispid fig dry paste.
II, secondly, the method comprises the following steps: preparation of Ficus Simplicissima extract
Dissolving the dry extract of the hispid fig with water of which the mass is 5 times volume (w/V, g/ml) of the dry extract of the hispid fig to obtain an aqueous solution of the dry extract of the hispid fig, adding superfine silica gel powder (202106013210, tianjin Longhua honest powder technology Limited) of which the weight is 30 percent of the weight of the dry extract of the hispid fig, uniformly mixing, concentrating by using a rotary evaporator at low temperature (less than 45 ℃) to be dry, crushing and sieving by using a 110-mesh sieve to obtain the hispid fig extract.
And preparing different batches of hispid fig extract from the multi-batch hispid fig powder according to the operation methods from the first step to the second step.
Thirdly, the method comprises the following steps: blending
And (3) mixing the 15 batches of the hispid fig extract obtained in the second step according to the following ratio of 1:1: 16 (g/g).
The blending standard is as follows: the spectrum obtained by the finally obtained control extract and 15 batches of hispid fig extracts share a mode (hispid fig control fingerprint spectrum), and the content range of each component in the blending standard is also the best data obtained by comprehensively maintaining stability and consistency and later application and the like through repeated experiments.
Fourthly, the method comprises the following steps: detection of
Determining the fingerprint of the hispid fig formula particle control extract prepared in the third step by using a high performance liquid chromatography, and detecting the similarity with a common mode (hispid fig control fingerprint) of 15 batches of hispid fig extracts, wherein as shown in figure 5, ERS corresponds to the hispid fig formula particle control extract, R is the hispid fig control fingerprint, the obtained similarity is 0.999, and the similarity between the hispid fig formula particle control extract and the hispid fig control fingerprint is high.
Example 3: character analysis of five-finger wild peach formula particle control extract
1. Apparent state: the control extract of the hispid fig granule obtained in example 2 was a yellow powder.
2. The moisture content was measured according to the first method (1, volumetric titration method P104) in the section of the 2015 th chinese pharmacopoeia qua 0832 moisture content measurement method. The detection result shows that the water content of the control extract of the hispid fig formula granules is 9.0%.
3. And (3) testing consistency: 15 batches of the control extract of hispid fig granule were prepared according to the method of example 2, and the differences in the thin layer chromatography detection profiles of the respective batches were determined to be small. Therefore, the consistency of the reference extract of the hispid fig formula particle prepared by the preparation method of the reference extract of the hispid fig formula particle is very good.
Claims (9)
1. A preparation method of a hispid fig formula particle control extract is characterized by comprising the following steps:
step one, water extraction, wherein the water extraction comprises the following steps:
a) Mixing hispid fig powder with water, decocting, and filtering to obtain filtrate 1 and residue 1;
b) Repeating the operation of the step a) on the filter residue 1 to obtain a filtrate 2 and a filter residue 2, repeating the operation of the step a) on the obtained filter residue 2, and repeating the operation of the step a) for N times by analogy with the operation of the step b) to obtain a filtrate N +1 and a filter residue N +1;
c) Mixing the filtrate 1-N +1 to obtain an extracting solution 1, and concentrating the extracting solution 1 to obtain the dry extract of the hispid fig;
step two, preparing a hispid fig extract: dissolving the hispid fig dry paste obtained in the step two in water to obtain a hispid fig dry paste water solution, adding auxiliary materials, drying and sieving to obtain a hispid fig extract;
step three, blending: and blending the hispid fig extracts of different batches to obtain the reference hispid fig granule extract.
2. The method according to claim 1, wherein in the first step, N is not less than 8 and not less than 0, and N is an integer;
optionally, the N =1.
3. The preparation method according to claim 1, wherein the weight-to-volume ratio of the hispid fig powder to water in the first step is 1:5-1, and the unit of the weight-to-volume ratio is g/mL;
optionally, the weight volume ratio of the hispid fig to the water in the step one is 1:10;
optionally, the decocting time in the step one is 1-300 min;
optionally, the decocting time in the first step is 30min;
optionally, the filtration in the first step is medium-speed filter paper or a filter bag;
optionally, the filtration in the first step is filtration with a filter bag.
Optionally, the aperture of the filter bag in the step one is 10-200 μm
Optionally, the aperture of the filter bag in the first step is 10 μm.
4. The preparation method according to claim 1, wherein the weight-to-volume ratio of the dry extract of hispid fig to water in the second step is 1:5-1, and the unit of the weight-to-volume ratio is g/mL;
optionally, the weight-volume ratio of the dry extract of the hispid fig to the water in the second step is 1:5;
optionally, the weight of the auxiliary material is 10-50% of the weight of the dry extract of the fici simplicissima lour;
optionally, the weight of the auxiliary materials is 30% of the weight of the dry paste of the fici simplicissima lour;
optionally, the auxiliary material is micropowder silica gel;
optionally, filtering the dried product in the third step by a sieve with 90 to 200 meshes;
optionally, the drying in step three is followed by 110 mesh sieving.
5. The method of claim 1, wherein a pre-blending treatment step of detecting different batches of hispid Fig extract by thin layer chromatography and/or high performance liquid chromatography is further included between the second step and the third step.
6. A hispid fig formula particle control extract is characterized in that the hispid fig formula particle control extract is obtained by the preparation method of any one of claims 1 to 5;
optionally, the spectrum of the control extract of the hispid fig granule obtained by adopting thin layer chromatography and/or high performance liquid chromatography is consistent with that of the control extract of the hispid fig granule;
optionally, the spectrum of the radix fici simplicissimae formula particle reference extract obtained by adopting thin-layer chromatography and/or high performance liquid chromatography is consistent with the spectrum of the radix fici simplicissimae at the position of psoralen;
optionally, the hispid fig formula granule control extract contains a main substance containing psoralen.
7. Use of the hispid Fig formulation control extract of claim 6 for the identification thereof.
8. The use of claim 7, wherein said identification method is: detecting the control extract of the hispid fig formula particle of claim 6 by thin layer chromatography and/or high performance liquid chromatography, and comparing and judging;
optionally, the thin layer chromatography and/or high performance liquid chromatography is used for detecting the main components in the control extract and the middle of the formula particles of the hispid fig, wherein the main components comprise psoralen;
optionally, when the hispid fig formula particle control extract of claim 6 is subjected to detection by thin layer chromatography, the hispid fig formula particle control extract is prepared into a solution for detection, wherein the preparation method of the hispid fig formula particle control extract solution comprises the following steps: weighing 0.1-0.5 g of the hispid fig formula particle control extract of claim 7, adding 10-40 mL of water to dissolve, adding ether to shake and extract for 1-3 times, 10-30 mL each time, combining ether solutions, volatilizing, adding 0.5-2 mL of ethanol to dissolve residues, and filtering through a 0.12-0.32 μm filter membrane to obtain a hispid fig formula particle control extract solution;
optionally, the sample volume of the control extract of the hispid fig formula particle is 0.25g; the water adding amount is 30ml; the number of times of shaking extraction of the ether is 2, and each time is 30ml; the ethanol amount is 0.5ml, and the filter membrane is 0.22 μm;
optionally, the detection condition of the thin layer chromatography is detection condition one or detection condition two, and the detection condition one is:
thin-layer plate: TLC G60 precast slab;
sample application: 10 mul, spot in a strip shape;
developing agent:
n-hexane-trichloromethane-ethyl acetate-glacial acetic acid with the volume ratio of 20: 4: 7: 1;
and (6) inspection:
inspecting under 365nm ultraviolet lamp.
The second detection condition is as follows:
thin-layer plate: TLC G60 precast slab;
sample application: 10 mul, spot in a strip shape;
developing agent: toluene-ethyl acetate-formic acid-water, the volume ratio is 20: 1, the upper layer solution which is layered under 10 ℃;
and (6) inspection: inspecting under 365nm ultraviolet lamp.
9. The use of claim 8, wherein the hispid fig granule control extract of claim 6 is prepared into a solution for testing, wherein the hispid fig granule control extract is prepared by the following steps: adding methanol into the hispid fig formula particle control extract of claim 6 to obtain a hispid fig formula particle control extract methanol solution with a concentration of 2mg/mL-15mg/mL, and filtering with a 0.12-0.32 μm filter membrane to obtain a hispid fig formula particle control extract solution;
optionally, the concentration of the hispid fig formulation granule in the methanol solution of the control extract is 10mg/mL; the filter membrane is 0.22 μm;
optionally, the detection conditions of the high performance liquid chromatography are as follows:
chromatography apparatus: thermo Fisher U3000 high performance liquid chromatograph;
a detector: a Thermo Fisher DAD detector;
a chromatographic column: waters Symmetry C18.6 mm × 250,5 μm;
mobile phase: (A) acetonitrile-methanol, volume ratio 3:1; (B) 0.1% phosphoric acid solution
Gradient of mobile phase:
detection wavelength: 254nm; the flow rate is 1ml/min; the sample amount is 10 mul; the column temperature is 35 ℃; operating time: and (4) 40min.
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