CN114965806A - Pummelo peel formula particle contrast extract and preparation method thereof - Google Patents
Pummelo peel formula particle contrast extract and preparation method thereof Download PDFInfo
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- CN114965806A CN114965806A CN202210490237.7A CN202210490237A CN114965806A CN 114965806 A CN114965806 A CN 114965806A CN 202210490237 A CN202210490237 A CN 202210490237A CN 114965806 A CN114965806 A CN 114965806A
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- 239000012528 membrane Substances 0.000 claims description 14
- 239000001606 7-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2S,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxyoxan-2-yl]oxy-5-hydroxy-2-(4-hydroxyphenyl)chroman-4-one Substances 0.000 claims description 12
- DFPMSGMNTNDNHN-ZPHOTFPESA-N naringin Chemical group O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C3O[C@@H](CC(=O)C3=C(O)C=2)C=2C=CC(O)=CC=2)O[C@H](CO)[C@@H](O)[C@@H]1O DFPMSGMNTNDNHN-ZPHOTFPESA-N 0.000 claims description 12
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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
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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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention provides a preparation method of a pummelo peel formula particle comparison extract, which comprises the steps of respectively carrying out multiple extraction, concentration and low-temperature drying on multiple batches of pummelo peel powder to obtain different batches of pummelo peel extracts, and then blending the different batches of pummelo peel extracts to obtain the pummelo peel formula particle comparison extract. The preparation method of the pummelo peel formula particle contrast extract is simple and convenient to operate, low in cost, good in repeatability and high in extraction rate; the preparation method for preparing the control extract of the pummelo peel formula particles ensures the consistency of the control extracts of different batches of pummelo peel formula particles, and the pummelo peel formula particles have stable and uniform properties and are convenient to use; the thin-layer chromatography fingerprint and the UPLC fingerprint of the contrast extract finally obtained by the preparation method of the pummelo peel formula particle contrast extract are consistent with the corresponding fingerprints.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine quality control, in particular to a pummelo peel formula particle contrast extract and 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 ambiguity 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 materials as the quality of the Chinese medicinal materials 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; secondly, the traditional Chinese medicine reference medicinal materials are influenced by the producing area and the growth environment, so that 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 components of the medicinal materials.
The traditional Chinese medicine control extract is an extract which is prepared from traditional Chinese medicinal materials, has stable properties and components, can be used for qualitative or quantitative analysis, and provides four basic requirements (ASCS) for the traditional Chinese medicine control extract by Mr. Shipeheng, and also provides basic conditions for the control extract: the herbal material source is reliable and representative; specificity, Specificity of the detection method used; con-sistence, 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 and high performance liquid chromatography fingerprint, and the control extract standardized by 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 pummelo peel (pomelo) formula granules, and a preparation method and application thereof. The invention provides a preparation method of a pummelo peel (pomelo) 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 pummelo peel (pomelo) formula particle contrast extract prepared by the preparation method of the pummelo peel (pomelo) formula particle contrast extract, and the prepared pummelo peel (pomelo) 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 pummelo peel (pomelo) formula particle contrast extract, which comprises the following steps:
step one, water extraction, wherein the water extraction comprises the following steps:
a) mixing exocarpium Citri Grandis 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 filtrates 1 to (N +1) to obtain an extracting solution 1, and concentrating the extracting solution 1 at low temperature to obtain pummelo peel (pomelo) dry paste;
step two, preparing pummelo peel (pomelo) extract: dissolving the pummelo peel (pomelo) dry paste obtained in the step two in water to obtain a pummelo peel (pomelo) dry paste water solution, adding auxiliary materials, drying at low temperature and sieving to obtain a pummelo peel (pomelo) extract;
step three, blending: blending different batches of pummelo peel (pomelo) extracts to obtain the pummelo peel (pomelo) formula particle control extract.
The temperature adopted for low-temperature drying in the preparation process is 20-60 ℃.
Different batches of pummelo peel (pomelo) extracts are blended, and at least fifteen batches of pummelo peel (pomelo) extracts are blended or blended.
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 2.
Preferably, the weight-volume ratio of the pummelo peel (pomelo) powder to the water in the first step is 1: 5-1: 50, and the unit of the weight-volume ratio is g/mL.
More preferably, the weight volume ratio of the pummelo peel powder to the water in the first step is 1: 10.
preferably, the decocting time in the first step is 1-300 min.
More preferably, the decoction time in the first step is 30 min.
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 a medium speed filter paper.
Preferably, the weight-volume ratio of the pummelo peel (pomelo) dry paste to the water in the second step is 1: 5-1: 50. The unit of the weight-volume ratio is g/mL.
More preferably, the weight-volume ratio of the pummelo peel (pomelo) dry paste to the water in the second step is 1: 5.
Preferably, the weight of the auxiliary materials is 20 to 60 percent of the dry paste weight of pummelo peel (pomelo).
More preferably, the weight of the auxiliary materials is 40% of the dry extract weight of pummelo peel (pomelo).
Preferably, the auxiliary material is aerosil.
Preferably, the second step is carried out at low temperature and then filtered by a screen 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 pre-blending treatment step of detecting different batches of pummelo peel (pomelo) extracts 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 present invention provides a control extract of pummelo peel (pomelo) formula particles, which is obtained by the above-mentioned preparation method.
Preferably, the above-mentioned control extract of pummelo peel (pomelo) formula granules has a spectrum obtained by thin layer chromatography and/or high performance liquid chromatography, and is identical to the spectrum obtained by thin layer chromatography and/or high performance liquid chromatography.
Preferably, the spectrum of the control extract of the pummelo peel formula granules obtained by adopting the thin layer chromatography and/or the high performance liquid chromatography is consistent with the spectrum of the pummelo peel formula granules at the position of naringin.
Preferably, the above-mentioned control extract of pummelo peel (pomelo) formula granules contains naringin as the main ingredient.
In a third aspect, the present invention provides the use of the above control extract of pummelo peel granules for identification.
Preferably, the quality control method comprises: detecting the above control extract of exocarpium Citri Grandis granule by thin layer chromatography and/or high performance liquid chromatography, and comparing.
Preferably, the thin layer chromatography and/or high performance liquid chromatography is used for detecting the main components of the control extract and the control extract of the pummelo peel (pomelo) formula particles, and the main components comprise naringin.
Preferably, when the control extract of the pummelo peel formula particle is detected by thin layer chromatography, the control extract of the pummelo peel formula particle is prepared into a solution for detection, wherein the preparation method of the control extract solution of the pummelo peel formula particle is as follows: adding methanol into the pummelo peel formula particle control extract of claim 6 to prepare a methanol solution of the pummelo peel formula particle control extract, and filtering the methanol solution through a filter membrane of 0.12-0.32 μm to obtain the pummelo peel formula particle control extract solution;
optionally, the pummelo peel formula granule control extract methanol solution concentration is 70 mg/mL; the filter membrane is 0.22 mu m;
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 0.35-2 g, adding 5-30 mL of methanol, carrying out ultrasonic treatment for 15-60 minutes, and filtering through a 0.12-0.32 mu m filter membrane to obtain a solution of the product to be detected;
preferably weighing 0.7g of the product to be detected, adding 10mL of methanol, carrying out ultrasonic treatment for 30 minutes, and filtering through a 0.22 mu m filter membrane to obtain the solution of the product to be detected.
Preferably, the detection condition of the thin layer chromatography is a first detection condition or a second detection condition, and the first detection condition is:
thin-layer plate: TLC G60 precast slab;
sample application: orange (pomelo) formula granule control extract solution and solution each 2 μ l, strip-like spotting;
developing agent: ethyl acetate-acetone-glacial acetic acid-water (8: 4: 0.3: 1)
And (6) inspection: spraying 5% ethanol solution of aluminum trichloride, heating at 105 deg.C for 1 min, and inspecting under ultraviolet lamp (365 nm).
The second detection condition is as follows:
thin layer plate: TLC G60 precast slab;
sample application: orange (pomelo) formula granule control extract solution and solution each 2 μ l, strip-like spotting;
developing agent: toluene-Ethyl acetate-formic acid (5: 4: 0.1);
and (6) inspection: inspecting under an ultraviolet lamp (365 nm).
Optionally, when the control extract of the pummelo peel (pomelo) formula particles is detected by high performance liquid chromatography, the control extract of the pummelo peel (pomelo) formula particles needs to be prepared into a solution for detection, wherein the preparation method of the solution of the control extract of the pummelo peel (pomelo) formula particles comprises the following steps: adding 75% ethanol to the pummelo peel (pomelo) formula granule control extract of claim 6 to prepare a pummelo peel (pomelo) formula granule control extract solution with a concentration of 0.5mg/mL to 10mg/mL, and filtering with a 0.12 μm to 0.32 μm filter membrane to obtain the pummelo peel (pomelo) formula granule control extract solution.
Preferably, the concentration of the control extract solution of the pummelo peel formula particles is 1 mg/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 0.1-1 g, adding 100-1000 mL of 75% ethanol, carrying out ultrasonic treatment for 30-60 min at a 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 0.1g of the product to be detected, adding 100mL of 75% ethanol, carrying out ultrasonic treatment for 45min at the power of 500W, shaking up, and filtering with 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:
chromatography apparatus: a Thermo Vanqish ultra performance liquid chromatograph;
a detector: a Thermo DAD detector;
a chromatographic column: waters HSS T3 C182.1mm × 100, 1.8 μm;
mobile phase: (A) methanol; (B) 0.1% acetic acid solution
Gradient of mobile phase:
detection wavelength: 315 nm; the flow rate is 0.3 ml/min; the sample size is 1 mul; the column temperature is 40 ℃; operating time: and (5) for 27 min.
The invention has the following beneficial effects:
the preparation method of the pummelo peel formula particle contrast extract adopts the steps of extraction, preparation of the pummelo peel extract and blending, and has the advantages of simple and convenient operation, low cost, good repeatability and high extraction rate. The pummelo peel (pomelo) formula particle contrast extract prepared by the preparation method is prepared by mixing different batches of extracts, so that the defect that the quality consistency of each batch is difficult to ensure due to the influence of production areas and growth environments on traditional Chinese medicine contrast medicinal materials is overcome, and the consistency of the pummelo peel (pomelo) formula particle contrast extracts of different batches is ensured; the character is stable and uniform and is convenient to use; the thin-layer chromatography fingerprint and HPLC fingerprint of the contrast extract finally obtained by the preparation method of the pummelo peel (pomelo) formula particle contrast extract are consistent with the corresponding ones.
The invention also provides an identification method or a quality control method of pummelo peel (pomelo), which can carry out qualitative identification.
Drawings
FIG. 1 is a thin layer chromatogram obtained by performing thin layer chromatography on exocarpium Citri Grandis (fructus Citri Grandis) with naringin as reference substance. Reference naringin 1, pummelo peel (fructus Citri Grandis) 2-17: pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
FIG. 2 is a thin-layer chromatogram obtained by performing thin-layer chromatography on exocarpium Citri Grandis (fructus Citri Grandis) with control drug as reference substance. 1 is pummelo peel (pomelo) reference medicinal material, and 2-17 are sequentially corresponding to pummelo peel (pomelo): pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
FIG. 3 is an overlay of HPLC fingerprints obtained by HPLC of exocarpium Citri Grandis raw material, wherein R corresponds to exocarpium Citri Grandis common mode (common mode), and 1-16 correspond to exocarpium Citri Grandis (fructus Citri Grandis) in sequence: pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
FIG. 4 is a flow chart of the preparation of a control extract of pummelo peel formula of the present invention.
FIG. 5 shows the common pattern of the fingerprint of the control extract of pummelo peel (pomelo) formula granules measured by HPLC with 16 batches of pummelo peel (pomelo) extracts, ERS corresponds to the control extract of pummelo peel (pomelo) formula granules, and R is the common pattern of 16 batches of pummelo peel (pomelo) extracts.
Detailed Description
The following describes embodiments of the present invention in detail. 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:
pummelo peel (grapefruit) is a raw material to be used for preparing a control extract. Further, the present pummelo peel refers to pummelo peel (grapefruit).
Thermo Vanqish ultra performance liquid chromatograph, Thermo DAD detector.
Methanol (Merck) and acetic acid (Fisher Chemical).
The purity of the methanol not marked by the invention is more than or equal to 99.5 percent.
The 5% aluminum trichloride ethanol mixed solution related by the invention is an ethanol solution containing 5% aluminum trichloride by volume percentage.
The proportions of the developing solvent are volume ratios.
Toluene, ethyl acetate, acetone, methanol, ethanol, glacial acetic acid, formic acid, and aluminum trichloride were all analytically pure (Guangzhou chemical laboratories).
Naringin reference substance (China institute for testing and testing food and drug; lot No. 110722 and 202116, mark content is not less than 93.5%);
pummelo peel (pomelo) reference medicine (China institute for testing food and drug; batch number: 121165-once 201804)
Test raw material pummelo peel (pomelo) (decoction pieces):
16 batches of pummelo peel (pomelo) are purchased in the markets of various national medicinal materials: pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14 and pummelo peel (pomelo) 15.
Example 1: screening of pummelo peel formula granule reference extract raw material
This example provides a method for screening the raw material of a control extract of pummelo peel formula granules of the present invention.
Analyzing and screening exocarpium Citri Grandis (fructus Citri Grandis) with naringin and exocarpium Citri Grandis (fructus Citri Grandis) control materials as reference materials by thin layer chromatography and high performance liquid chromatography.
Pummelo peel (pomelo) is purchased from various major medicinal material markets throughout the country and is identified as immature or near mature dry outer pericarp of Citrus grandis (L.) Osbeck, a rutaceae plant. 16 batches of pummelo peel (pomelo) are qualified and can be used for standby.
1 thin layer chromatography
1.1 sample preparation
Raw material solution: weighing exocarpium Citri Grandis (1-16) powder, precisely weighing 0.5g each, adding 5mL methanol, performing ultrasonic treatment for 15 min at power of 500w, centrifuging for 10min at rotation speed of 4000 rpm, and filtering the supernatant with 0.22 μm filter membrane to obtain raw material solution.
Control solution: taking pummelo peel (pomelo) reference medicinal material powder, sieving with a No. four sieve, precisely weighing 0.5g, adding 5mL of methanol, performing ultrasonic treatment for 15 min at a power of 500w, centrifuging for 10min at a rotation speed of 4000 rpm, and taking supernatant to obtain the final product.
Preparation of a reference solution: weighing appropriate amount of naringin reference substance, preparing into 1mg/mL solution with methanol, and filtering with 0.22 μm filter membrane.
The detection conditions were as follows:
the method comprises the following steps:
thin-layer plate: TLC G60 precast slab;
sample application: 2 μ l, strip spotting;
developing agent: ethyl acetate-acetone-glacial acetic acid-water (8: 4: 0.3: 1)
And (3) inspecting: spraying 5% ethanol solution of aluminum trichloride, heating at 105 deg.C for 1 min, and inspecting under ultraviolet lamp (365 nm).
The second method comprises the following steps:
thin-layer plate: TLC G60 precast slab;
sample application: 5 μ l, strip spotting;
developing agent: toluene-ethyl acetate-formic acid (5: 4: 0.1);
and (6) inspection: the sample was inspected under an ultraviolet lamp (365 nm).
The results are shown in FIG. 1-FIG. 2, in which FIG. 1 shows the thin-layer chromatogram observed under an ultraviolet lamp (365nm) after the first method, and FIG. 2 shows the thin-layer chromatogram observed under an ultraviolet lamp (365nm) after the second method.
FIG. 1: reference naringin 1, pummelo peel (fructus Citri Grandis) 2-17: pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
FIG. 2: 1 is pummelo peel (pomelo) reference medicinal material, and 2-17 are sequentially corresponding to pummelo peel (pomelo): pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
As can be seen from fig. 1-2, each batch of pummelo peel (grapefruit) material showed the same spot at the same location, and was initially screened as a pummelo peel material for the control extract.
2 high performance liquid chromatography
2.1 sample preparation
Raw material medicinal material solution: accurately weighing 0.1g of pummelo peel (pomelo) (1-16) powder, placing in a conical flask with a plug, adding 20mL of water, heating and refluxing for 30 minutes, filtering with medium-speed filter paper at 30-50 μm, evaporating filtrate to dryness, adding 100mL of 75% ethanol into residue, performing ultrasonic treatment for 45 minutes at the power of 500w, cooling, shaking up, and filtering with a 0.22 μm filter membrane to obtain the pummelo peel and pummelo peel powder.
2.2 high Performance liquid chromatography detection
The detection conditions of the high performance liquid chromatography are as follows:
chromatography apparatus: a Thermo Vanqish ultra performance liquid chromatograph;
a detector: a Thermo DAD detector;
a chromatographic column: waters HSS T3 C182.1mm × 100, 1.8 μm;
mobile phase: (A) methanol; (B) 0.1% acetic acid solution
Gradient of mobile phase:
detection wavelength: 315 nm; the flow rate is 0.3 ml/min; the sample amount is 1 mul; the column temperature is 40 ℃; operating time: and (5) 27 min.
The detection method of the high performance liquid chromatography comprises the following steps: the raw material solutions are injected into a liquid chromatograph with 1 mul each.
And (3) detecting results by high performance liquid chromatography:
measuring, and recording chromatogram to obtain HPLC fingerprint overlay shown in figure 3, wherein R corresponds to exocarpium Citri Grandis common mode (common mode), and S1-S16 sequentially corresponds to exocarpium Citri Grandis raw materials: pummelo peel (pomelo) 1, pummelo peel (pomelo) 2, pummelo peel (pomelo) 3, pummelo peel (pomelo) 4, pummelo peel (pomelo) 5, pummelo peel (pomelo) 6, pummelo peel (pomelo) 7, pummelo peel (pomelo) 8, pummelo peel (pomelo) 9, pummelo peel (pomelo) 10, pummelo peel (pomelo) 11, pummelo peel (pomelo) 12, pummelo peel (pomelo) 13, pummelo peel (pomelo) 14, pummelo peel (pomelo) 15 and pummelo peel (pomelo) 16.
As can be seen from fig. 3, the fingerprints of pummelo peel (pomelo) 1-pummelo peel (pomelo) 16 have high consistency, thereby establishing a common fingerprint pattern of pummelo peel (pomelo), and performing similarity analysis on all samples. According to the common mode map, similarity evaluation is carried out on 16 batches of pummelo peel (pomelo) according to each sample component and the peak area thereof by adopting an included angle cosine algorithm, and the result is shown in table 1.
TABLE 1
According to the similarity analysis results, the similarity of 16 batches of pummelo peel (pomelo) is very high, and the pummelo peel (pomelo) formula particle control extract can be selected as a raw material.
Example 2: preparation of control extract of pummelo peel (pomelo) formula granule
This example provides a method for preparing a control extract of pummelo peel formula of the present invention, the flow chart of which is shown in fig. 4.
Firstly, the method comprises the following steps: extraction of
Selecting 16 batches of pummelo peel (pomelo) raw materials, respectively preparing into powder, then respectively adding water with the volume 20 times of the mass of the pummelo peel (namely the solid-liquid ratio is 1: 20(w/V, g/ml)), decocting for 30min, filtering with medium-speed filter paper (general electric and biological technology (Hangzhou) limited company, model: 99-103-.
II, secondly: preparation of exocarpium Citri Grandis extract
Dissolving dried pummelo peel (pomelo) extract paste with water with volume (w/V, g/ml) 5 times of dried pummelo peel (pomelo) paste mass to obtain water solution of dried pummelo peel (pomelo) paste, adding silica gel micropowder (Tianjin Longhua Chengxin powder technology Limited, lot number 202106013210) 40% of dried pummelo peel (pomelo) paste weight, mixing, concentrating at low temperature (less than 45 deg.C) with rotary evaporator to dry, pulverizing, and sieving with 110 mesh sieve to obtain pummelo peel (pomelo) extract.
And (4) preparing different batches of pummelo peel (pomelo) extracts from the multiple batches of pummelo peel (pomelo) 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 16 batches of pummelo peel (pomelo) extracts in the second step according to the ratio of 1:1:1:1:1:1:1: and (3) mixing and blending at a ratio of 1:1:1:1:1:1:1:1 to obtain a pummelo peel (pomelo) control extract, wherein the extraction method has stronger pertinence and is a method adopted by the formula particle control extract, so that the pummelo peel (pomelo) control extract is also called the pummelo peel (pomelo) formula particle control extract, and the ratio of a final product to the pummelo peel (pomelo) (decoction pieces) is about 1: 1.4 (g/g).
The blending standard is as follows: the spectrum of the finally obtained control extract is consistent with the common mode of 16 batches of pummelo peel (pomelo) extract (control fingerprint spectrum of pummelo peel (pomelo) formula granule control extract), and the content range of each component in the blending standard is the best data obtained by comprehensively maintaining stability, consistency and later application through repeated experiments.
Fourthly, the method comprises the following steps: detection of
And (3) determining the comparison extract of the pummelo peel (pomelo) formula particles prepared in the third step by using a high performance liquid chromatography to obtain a fingerprint, and detecting the similarity with a common mode (the comparison extract of the pummelo peel (pomelo) formula particles is compared with the fingerprint) of 16 batches of pummelo peel (pomelo) extracts, wherein as shown in fig. 5, ERS corresponds to the comparison extract of the pummelo peel (pomelo) formula particles, R is the comparison extract of the pummelo peel (pomelo) formula particles and the fingerprint, the similarity is 1, and the similarity between the comparison extract of the pummelo peel (pomelo) formula particles and the comparison fingerprint of the pummelo peel (pomelo) is high.
Example 3: property analysis of control extract of pummelo peel (pomelo) formula granule
1. Apparent state: the control extract of the pummelo peel formula granules obtained in example 2 were all pale yellow powders.
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 pummelo peel formula particle is 9.0%.
3. And (3) testing consistency: control extracts of 16 batches of pummelo peel (grapefruit) formula were prepared as in example 2, and were determined to have very little difference in the thin layer chromatography profiles of the individual batches. Therefore, the prepared pummelo peel (pomelo) formula particle control extract has very good consistency by using the preparation method of the pummelo peel (pomelo) formula particle control extract.
Claims (9)
1. A preparation method of a pummelo peel formula particle contrast extract is characterized by comprising the following steps:
step one, water extraction, wherein the water extraction comprises the following steps:
a) mixing pummelo peel 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 pummelo peel dry paste;
step two, preparing a pummelo peel extract: dissolving the dried pummelo peel paste obtained in the step two in water to obtain a water solution of the dried pummelo peel paste, adding auxiliary materials, drying and sieving to obtain a pummelo peel extract;
step three, blending: blending different batches of pummelo peel extract to obtain pummelo peel formula granule control extract.
2. The method according to claim 1, wherein in the first step, N is 8. gtoreq.N.gtoreq.0, and N is an integer;
optionally, the N ═ 2.
3. The preparation method according to claim 1, wherein the weight-to-volume ratio of the neutralized grapefruit powder to water in the first step is 1:5 to 1:50, and the unit of the weight-to-volume ratio is g/mL;
optionally, the weight volume ratio of the pummelo peel and water in the first step is 1: 20;
optionally, the decocting time in the first step is 1-300 min;
optionally, the decocting time in the first step is 30 min;
optionally, the filtration in the first step is medium-speed filter paper or a filter bag;
optionally, the filtering in the first step is filtering with medium-speed filter paper.
4. The preparation method according to claim 1, wherein the weight-to-volume ratio of the pummelo peel dry paste to water in the second step is 1: 5-1: 50, and the unit of the weight-to-volume ratio is g/mL;
optionally, the weight-volume ratio of the pummelo peel dry paste to water in the second step is 1: 5;
optionally, the weight of the auxiliary materials is 20-60% of the dry extract weight of pummelo peel;
optionally, the weight of the auxiliary materials is 40% of the dry extract weight of pummelo peel;
optionally, the auxiliary material is micropowder silica gel;
optionally, filtering the mixture through a 90-200-mesh screen after drying in the third step;
optionally, the drying in step three is followed by 110 mesh sieving.
5. The preparation method according to claim 1, further comprising a pre-blending treatment step of detecting different batches of pummelo peel extract by thin layer chromatography and/or high performance liquid chromatography between the second step and the third step.
6. A pummelo peel formula particle control extract, which is obtained by the preparation method of any one of claims 1 to 5;
optionally, the spectrum of the control extract of the pummelo peel formula particles obtained by adopting thin layer chromatography and/or high performance liquid chromatography is consistent with that obtained by adopting the thin layer chromatography and/or the high performance liquid chromatography;
optionally, the spectrum of the control extract of the pummelo peel formula particle obtained by adopting thin layer chromatography and/or high performance liquid chromatography is consistent with the spectrum of the pummelo peel at the position of naringin;
optionally, the control extract of the citrus grandis formula granule contains a major component comprising naringin.
7. Use of a control extract of a pummelo peel formula of claim 6 for identification.
8. The use of claim 7, wherein said identification method is: detecting and comparing the control extract of the pummelo peel formula particle of claim 6 with thin layer chromatography and/or high performance liquid chromatography;
optionally, the thin layer chromatography and/or high performance liquid chromatography is used for detecting the main component in the control extract and the middle of the pummelo peel formula particles, wherein the main component comprises naringin;
optionally, the citrus grandis formula granule control extract of claim 6 is formulated into a solution for testing by thin layer chromatography, wherein the citrus grandis formula granule control extract solution is formulated by: adding methanol into the pummelo peel formula particle comparison extract of claim 6 to prepare a methanol solution of the pummelo peel formula particle comparison extract of 30mg/mL-80mg/mL, and filtering the methanol solution with a 0.12-0.32 μm filter membrane to obtain a pummelo peel formula particle comparison extract solution;
optionally, the concentration of the control extract methanol solution of the pummelo peel formula particles is 70 mg/mL; the filter membrane is 0.22 mu m;
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: 2 μ l, strip spotting;
developing agent: ethyl acetate-acetone-glacial acetic acid-water in a volume ratio of 8: 4: 0.3: 1;
and (3) inspecting: spraying 5% aluminum trichloride ethanol solution, heating at 105 deg.C for 1 min, and inspecting under 365nm ultraviolet lamp;
the second detection condition is as follows:
thin-layer plate: TLC G60 precast slab;
sample application: 2 μ l, strip spotting;
developing agent: toluene-ethyl acetate-formic acid with the volume ratio of 5: 4: 0.1;
and (3) inspecting: inspecting under 365nm ultraviolet lamp.
9. The use of claim 8, wherein the testing of a control extract of a citrus grandis formula of claim 6 by hplc requires testing the control extract of a citrus grandis formula in a solution, wherein the control extract of a citrus grandis formula is prepared by: adding 75% ethanol to the citrus grandis formula granule control extract of claim 6 to obtain a citrus grandis formula granule control extract solution with a concentration of 0.5mg/mL to 10mg/mL, and filtering with a 0.12 μm to 0.32 μm filter membrane to obtain a citrus grandis formula granule control extract solution;
optionally, the concentration of the control extract solution of the pummelo peel formula particles is 1 mg/mL; the filter membrane is 0.22 μm;
optionally, the detection conditions of the high performance liquid chromatography are as follows:
chromatography apparatus: thermo Vanqish ultra performance liquid chromatograph;
a detector: a Thermo DAD detector;
a chromatographic column: waters HSS T3 C182.1mm × 100, 1.8 μm;
mobile phase: (A) methanol; (B) 0.1% acetic acid solution;
gradient of mobile phase:
detection wavelength: 315 nm; the flow rate is 0.3 ml/min; the sample amount is 1 mul; the column temperature is 40 ℃; operating time: and (5) for 27 min.
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