CN114965808A - A control extract of Morinda citrifolia granule and its preparation method - Google Patents
A control extract of Morinda citrifolia granule and its preparation method Download PDFInfo
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- CN114965808A CN114965808A CN202210490266.3A CN202210490266A CN114965808A CN 114965808 A CN114965808 A CN 114965808A CN 202210490266 A CN202210490266 A CN 202210490266A CN 114965808 A CN114965808 A CN 114965808A
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- morinda
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- morinda citrifolia
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- 239000000284 extract Substances 0.000 title claims abstract description 128
- 235000017524 noni Nutrition 0.000 title claims abstract description 96
- 244000131360 Morinda citrifolia Species 0.000 title claims abstract description 93
- 235000008898 Morinda citrifolia Nutrition 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000008187 granular material Substances 0.000 title claims description 34
- 241000096284 Gynochthodes officinalis Species 0.000 claims abstract description 204
- 239000002245 particle Substances 0.000 claims abstract description 46
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 34
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 105
- 238000000034 method Methods 0.000 claims description 54
- 238000001514 detection method Methods 0.000 claims description 37
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000009472 formulation Methods 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 27
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 25
- 239000011780 sodium chloride Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- 229940006364 morinda citrifolia extract Drugs 0.000 claims description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- 235000015145 nougat Nutrition 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001228 spectrum Methods 0.000 claims description 8
- 238000007689 inspection Methods 0.000 claims description 7
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- HPWWQPXTUDMRBI-COZRGLNQSA-N Monotropein Natural products O=C(O)C=1[C@H]2[C@H]([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)[C@](O)(CO)C=C2 HPWWQPXTUDMRBI-COZRGLNQSA-N 0.000 claims description 5
- HPWWQPXTUDMRBI-NJPMDSMTSA-N monotropein Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@@H]2[C@@](O)(CO)C=C[C@@H]2C(C(O)=O)=CO1 HPWWQPXTUDMRBI-NJPMDSMTSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000004587 chromatography analysis 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
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 239000011148 porous material 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
- 238000003892 spreading Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 8
- 239000003814 drug Substances 0.000 description 20
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- 239000013558 reference substance Substances 0.000 description 11
- 238000003908 quality control method Methods 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 241000157491 Morinda Species 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000012846 chemical reference substance Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 241000233855 Orchidaceae Species 0.000 description 2
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- 229930182470 glycoside Natural products 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- 229940054967 vanquish Drugs 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 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
- 241000196324 Embryophyta Species 0.000 description 1
- 239000009429 Ginkgo biloba extract Substances 0.000 description 1
- 241001107098 Rubiaceae Species 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UDHCJQLFFYNMNT-UHFFFAOYSA-N chembl1255666 Chemical compound C1=CC=C2OC(=O)C(C=3C(=O)C=4C(O)=CC(C)=C(C=4C(=O)C=3C=3C(OC4=CC=CC(C)=C4C=3O)=O)C3=C(C(C4=CC=CC(O)=C4C3=O)=O)C)=C(O)C2=C1C UDHCJQLFFYNMNT-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000010812 external standard method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229940068052 ginkgo biloba extract Drugs 0.000 description 1
- 235000020686 ginkgo biloba extract Nutrition 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000006049 herbal material Substances 0.000 description 1
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- 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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- 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
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- G01N30/02—Column chromatography
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Abstract
The invention provides a preparation method of a salted morinda officinalis formula particle contrast extract, which comprises the steps of respectively carrying out extraction, concentration and low-temperature drying on a plurality of batches of salted morinda officinalis powder for a plurality of times to obtain different batches of salted morinda officinalis extracts, and then blending the different batches of salted morinda officinalis extracts to obtain the salted morinda officinalis formula particle contrast extract. The preparation method of the morinda citrifolia 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 morinda citrifolia formula particle contrast extract ensures the consistency of the morinda citrifolia formula particle contrast extracts of different batches, and the morinda citrifolia formula particle contrast 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 morinda officinalis formula particle contrast extract are consistent with the corresponding ones.
Description
Technical Field
The invention relates to the technical field of quality control of traditional Chinese medicines, in particular to a saline morinda officinalis formula particle contrast extract as well as 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 adds 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 has four basic requirements (ASCS) for the traditional Chinese medicine control extract by Mr. schehren, which also is a control extract with the following basic conditions: 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, 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 morinda citrifolia granule control extract and a method for making the same. The invention provides a preparation method of a contrast extract of saline morinda officinalis formula particles, which is simple and convenient to operate, low in cost, good in repeatability and high in extraction rate; the invention also provides a saline morinda root formula particle contrast extract prepared by the preparation method of the saline morinda root formula particle contrast extract, and the prepared saline morinda root 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 saline morinda officinalis formula particle contrast extract on one hand, and the preparation method comprises the following steps:
step one, water extraction, wherein the water extraction comprises the following steps:
a) mixing salted morinda officinalis 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 morinda officinalis;
step two, preparing a morinda citrifolia extract: dissolving the morinda citrifolia dry paste obtained in the step two in water to obtain a morinda citrifolia dry paste water solution, adding auxiliary materials, drying at low temperature and sieving to obtain a morinda citrifolia extract;
step three, blending: blending different batches of the morinda citrifolia extract to obtain a morinda citrifolia formula particle control extract.
The temperature adopted for low-temperature drying in the preparation process is 20-60 ℃.
Different batches of the salted morinda officinalis extract are blended, and it can be understood that at least fifteen batches of the salted morinda officinalis extract 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 1.
Preferably, in the first step, the weight-to-volume ratio of the salted morinda officinalis powder to the water is 1: 5-1: 50, and the unit of the weight-to-volume ratio is g/mL.
More preferably, the weight volume ratio of the morinda officinalis 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 decocting time in the above step one is 60 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 filtration with a filter bag.
Preferably, the aperture of the filter bag in the first step 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 dried morinda officinalis extract to 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 dried morinda officinalis extract to water in the second step is 1: 5.
Preferably, the weight of the auxiliary materials is 20% -60% of the weight of the dry extract of morinda officinalis.
More preferably, the weight of the auxiliary materials is 45% of the dry extract of morinda citrifolia.
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 the morinda citrifolia 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 of the present invention, there is provided a salted morinda citrifolia granule control extract, said salted morinda citrifolia granule control extract being obtained by the above-described preparation method.
Preferably, the above-mentioned morinda citrifolia granule control extract has a profile consistent with that obtained by thin layer chromatography and/or high performance liquid chromatography.
Preferably, the above-mentioned morinda citrifolia formulation granule control extract has a spectrum obtained by thin layer chromatography and/or high performance liquid chromatography that is consistent with the spectrum of the morinda citrifolia granules at the site of the nougat or monothiopogon.
Preferably, the morinda citrifolia granule control extract as described above contains a major amount of a composition comprising nougat and monotropein.
In a third aspect of the present invention, there is provided the use of a control extract of the above morinda citrifolia formulation granulate for identification.
Preferably, the quality control method comprises: detecting the above mentioned control extract of Morinda citrifolia formulation 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 main components of the morinda citrifolia formula granules, wherein the main components comprise the nougat or the monotropein.
Preferably, when the above-mentioned morinda citrifolia formula particle control extract is detected by thin layer chromatography, the morinda citrifolia formula particle control extract is required to be prepared into a solution for detection, wherein the preparation method of the morinda citrifolia formula particle control extract solution comprises: weighing 1g to 5g of the saline morinda officinalis formula particle contrast extract as claimed in claim 6, adding 10mL to 40mL of water for dissolving, carrying out ultrasonic treatment for 10 min to 60min, adding ethyl acetate for shaking extraction for 1mL to 3 times, 10mL to 50mL each time, combining ethyl acetate solutions, evaporating to dryness, adding 0.5mL to 2mL of methanol for dissolving residues, and filtering through a 0.12 μm to 0.32 μm filter membrane to obtain a saline morinda officinalis formula particle contrast extract solution;
preferably, 3g of the morinda officinalis formula particle control extract is weighed, 25ml of water is added for dissolving, ultrasonic treatment is carried out for 30min, ethyl acetate is used for shaking and extracting for 2 times, 20ml of each time, ethyl acetate liquid is combined and volatilized to dryness, 1ml of methanol is added for dissolving residues, and the residues are filtered through a 0.22 mu m filter membrane to obtain the morinda officinalis formula particle control extract solution;
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 g-5 g, adding 10 mL-40 mL of water to dissolve, carrying out ultrasonic treatment for 10-60 min, adding ethyl acetate, shaking and extracting for 1-3 times, 10 mL-50 mL each time, combining ethyl acetate solutions, evaporating to dryness, adding 0.5 mL-2 mL of methanol 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;
preferentially weighing 3g of product to be detected, adding 25ml of water to dissolve, carrying out ultrasonic treatment for 30min, extracting for 2 times by shaking ethyl acetate, 20ml each time, combining ethyl acetate solutions, volatilizing, adding 1ml of methanol to dissolve residues, and filtering through a 0.22-micron filter membrane to obtain a solution of the 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: 10 mu l of the mixture; carrying out strip-shaped spotting;
developing agent: toluene-Ethyl acetate-Carboxylic acid (8:2:0.1)
And (6) inspection:
inspecting under an ultraviolet lamp (354 nm).
The second detection condition is as follows:
thin-layer plate: TLC G60 precast slab;
sample application: 2 mul strip sample application;
developing agent: ethyl acetate-methanol-glacial acetic acid-water (8:3:3: 1.8);
and (6) inspection: viewing under visible light.
Optionally, when the above-mentioned morinda citrifolia formula particle control extract is detected by high performance liquid chromatography, the morinda citrifolia formula particle control extract is required to be prepared into a solution for detection, wherein the preparation method of the morinda citrifolia formula particle control extract solution is method one or method two, and the method one is as follows: adding 10% -50% methanol to the saline morinda citrifolia formulation granule control extract of claim 6 to form a methanol solution of the saline morinda citrifolia formulation granule control extract with a concentration of 2mg/mL to 15mg/mL, and filtering through a 0.12-0.32 μm filter membrane to obtain a saline morinda citrifolia formulation granule control extract solution; the second method comprises the following steps: adding 1% -10% methanol to the control extract of Morinda citrifolia formulation of claim 6 to obtain a methanol solution of 2mg/mL-15mg/mL, and filtering through a 0.12-0.32 μm membrane to obtain a control extract solution of Morinda citrifolia formulation;
preferably, in the first method, the concentration of the methanol is 10%, and the concentration of the solution is 10 mg/mL; the filter membrane is 0.22 mu m;
preferably, the concentration of methanol is 3% in the second method, and the concentration of the solution is 10 mg/mL; the filter membrane is 0.22 mu m;
further, in the detection by high performance liquid chromatography, the preparation method of the solution to be detected is method one or method two, and the method one is as follows: grinding a product to be detected, weighing 0.1-0.5 g, adding 10-50 mL of 10% -50% methanol, 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 a subsequent filtrate to obtain a solution of the product to be detected. The second method comprises the following steps: grinding a product to be detected, weighing 0.1-0.5 g, adding 10-50 mL of 1% -10% methanol, 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 a subsequent filtrate to obtain a solution of the product to be detected.
Preferably, in the first method, 0.5g of the product to be detected is weighed, 50mL of 10% methanol is added, ultrasonic treatment is carried out for 30min at the power of 500W, shaking is carried out evenly, and the product solution to be detected is obtained after the product solution passes through a 0.22 mu m filter membrane.
Preferably, in the second method, 0.5g of the product to be detected is weighed, 50mL of 3% methanol is added, ultrasonic treatment is carried out for 30min with the power of 500W, shaking is carried out evenly, and the product solution to be detected is obtained after the product solution passes through a 0.22 mu m filter membrane.
Preferably, the detection conditions of the high performance liquid chromatography are detection condition one or detection condition two:
the first detection condition is as follows:
chromatography apparatus: thermo Scientific Vanqish ultra high performance liquid chromatograph;
a detector: DAD detector
A chromatographic column: YMC Triart C18, 2.1mm × 100mm, 1.9 μm;
mobile phase: (A) methanol; (B) 0.1% phosphoric acid solution
Gradient of mobile phase:
detection wavelength: 235 nm; the flow rate is 0.4 ml/min; the sample volume is 2 mul; the column temperature is 35 ℃; operating time: and (4) 14 min.
The second detection condition is as follows:
chromatography apparatus: thermo Scientific Vanqish ultra-high performance liquid chromatograph;
a detector: CAD detector
And (3) chromatographic column: waters ACQUITY
BEH Amide，2.1mm×100mm，1.7μm；
Mobile phase: (A) acetonitrile; (B) water (W)
Gradient of mobile phase:
the flow rate is 0.4 ml/min; the sample amount is 1 mul; the column temperature is 35 ℃; operating time: and (3) 30 min.
The invention has the following beneficial effects:
the preparation method of the morinda citrifolia formula particle contrast extract adopts the steps of extracting, preparing the morinda citrifolia extract and blending, and has the advantages of simple and convenient operation, low cost, good repeatability and high extraction rate. The contrast extract of the saline morinda officinalis 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 contrast medicinal materials is overcome, and the consistency of the contrast extract of the saline morinda officinalis 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 morinda officinalis formula particle contrast extract are consistent with the corresponding ones.
The invention also provides an identification method or a quality control method of the salted morinda officinalis, which can carry out qualitative identification.
Drawings
FIG. 1 is a thin layer chromatogram obtained by thin layer chromatography method I of Morinda citrifolia with Morinda citrifolia control as reference. 1 is a medicinal material of Morinda officinalis, 2-16 are corresponding to salt Morinda officinalis 1, salt Morinda officinalis 2, salt Morinda officinalis 3, salt Morinda officinalis 4, salt Morinda officinalis 5, salt Morinda officinalis 6, salt Morinda officinalis 7, salt Morinda officinalis 8, salt Morinda officinalis 9, salt Morinda officinalis 10, salt Morinda officinalis 11, salt Morinda officinalis 12, salt Morinda officinalis 13, salt Morinda officinalis 14, and salt Morinda officinalis 15.
FIG. 2 is a thin layer chromatogram obtained by performing thin layer chromatography method II on Morinda citrifolia decoction pieces with nougat as reference substance. 1 is noutose, 2-16 correspond to saline morinda officinalis in sequence: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
Fig. 3 is a superimposed graph of HPLC fingerprints obtained by performing high performance liquid chromatography method one on the morinda officinalis decoction pieces, which sequentially corresponds from bottom to top: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
Fig. 4 is a superimposed graph of HPLC fingerprints obtained by performing high performance liquid chromatography method two on morinda officinalis decoction pieces, which sequentially corresponds from bottom to top: : salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
FIG. 5 is a flow chart of the preparation of a control extract of Morinda citrifolia formulation particles of the present invention.
FIG. 6 shows the first HPLC method to determine the fingerprint of the control extract of Morinda citrifolia formulation and the first mode of the 15 batches of Morinda citrifolia extract, where ERS corresponds to the control extract of Morinda citrifolia formulation and R is the common mode of the 15 batches of Morinda citrifolia extract.
FIG. 7 shows the fingerprint of the control extract of Morinda citrifolia formulation measured by HPLC method II and the common mode of the extracts of Morinda citrifolia in 15 batches, where ERS corresponds to the control extract of Morinda citrifolia formulation, and R is the common mode of the extracts of Morinda citrifolia in 15 batches.
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:
the decoction pieces to be used for preparing the control extract are morinda officinalis.
Thermo Scientific Vanqish ultra performance liquid chromatograph, Thermo DAD, CAD detector.
Methanol, acetonitrile chromatically pure (Merck); phosphoric acid (Fisher).
The purity of the methanol not marked by the invention is more than or equal to 99.5 percent.
The proportions of the developing solvent are volume ratios.
Toluene, ethyl acetate, methanol, glacial acetic acid, formic acid were all analytically pure (Guangzhou chemical Co., Ltd.).
A glucose-resistant reference substance (China institute for food and drug testing; batch No. 111891-201704, mark content is more than or equal to 92.2%);
a crystal orchid glycoside reference substance, (China food and drug testing research institute; batch No. 111870-;
test salted morinda officinalis (decoction pieces):
the salted morinda officinalis is purchased from 15 batches of all the national large medicinal material markets: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
Example 1: screening of salted morinda officinalis
This example provides a method for screening the raw materials of a morinda citrifolia formulation granule control extract of the present invention.
Analyzing and screening Morinda citrifolia salt by thin layer chromatography and high performance liquid chromatography with Morinda citrifolia reference drug, and diospyrone and monothioglucoside as reference substances.
Morinda citrifolia is purchased from the national markets of various herbs and identified as the dry root of Morinda citrifolia (Morinda officinalis How) belonging to the family Rubiaceae. The identified 15 batches of medicinal materials can be used for standby after meeting the standard.
1 thin layer chromatography
1.1 methods 1
Sample preparation:
raw material medicinal material solution: collecting powder of Morinda citrifolia (1-15), weighing 2.5g each precisely, adding 25ml ethanol, heating and refluxing for 1 hr, cooling, filtering with medium speed filter paper (30-502 μm), and concentrating the filtrate to 1 ml.
Control solution: collecting Morinda citrifolia control 1.6g, adding ethanol 25ml, heating and refluxing at 100 deg.C for 1 hr, cooling, filtering with medium speed filter paper (30-502 μm), and concentrating the filtrate to 1 ml.
The detection conditions were as follows:
thin layer plate: TLC GF 254 Prefabricating a slab;
sample application: control solution: 16 μ l, crude drug solution: 5 mul, carrying out strip-shaped spotting;
developing agent: toluene-Ethyl acetate-Carboxylic acid (8:2:0.1)
And (6) inspection: inspecting under ultraviolet lamp (254 nm).
The detection result is shown in fig. 1, wherein 1 is a saline morinda officinalis control medicinal material, and 2-16 correspond to saline morinda officinalis in sequence: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
1.2 method two:
sample preparation:
control solution: dissolving appropriate amount of the glucose-resistant control with 50% methanol, and making into solution containing 0.5mg per 1 ml.
Raw material medicinal material solution: weighing 2g of salted morinda officinalis (1-15) powder accurately, adding water 80ml into a round bottom flask, heating and refluxing in 100 ℃ water bath for 1 hour, filtering with medium-speed filter paper (30-502 mu m), washing filter residue with 15ml of water, combining filtrate and washing liquid, transferring to a 100ml volumetric flask, adding water to scale, shaking up, and filtering with 0.22 mu m microporous membrane to obtain the final product.
Thin-layer plate: TLC G60 precast slab;
sample application: 2 mul, carrying out strip-shaped spotting;
developing agent: spreading ethyl acetate-methanol-glacial acetic acid-water (8:3:3:1.8) twice
And (6) inspection: and (5) placing under visible light for inspection.
The detection result is shown in fig. 2, wherein 1 is the nougat, and 2-16 correspond to the saline morinda officinalis in sequence: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
2 high performance liquid chromatography
2.1 methods 1
Sample preparation
Raw material medicinal material solution: taking 0.5g of salted morinda officinalis (1-15) powder, putting the powder into a 50ml measuring flask, adding 10% methanol, carrying out ultrasonic treatment (power is 250W, frequency is 40kHz) for 30 minutes, cooling, diluting with 10% methanol to scale, shaking up, filtering with medium-speed filter paper (30-502 mu m), and taking the subsequent filtrate to obtain the morinda officinalis salt preparation.
Control solution: taking a proper amount of the crystal orchid glycoside reference substance, accurately weighing, adding 10% methanol to prepare a solution containing 100 mug per 1ml as the reference substance solution of the reference substance.
High performance liquid chromatography detection
The detection conditions of the high performance liquid chromatography are as follows:
a chromatographic instrument: thermo Scientific Vanquish (ultra high performance liquid phase);
a detector: a DAD detector;
a chromatographic column: YMC-Triart C18(100 mm. times.2.1 mm,1.9 μm)
Mobile phase: (A) methanol; (B) 0.1% phosphoric acid solution;
gradient of mobile phase:
detection wavelength: 235 nm; the flow rate is 0.4 ml/min; the sample volume is 2 mul; the column temperature is 35 ℃; operating time: 14 min;
measuring, and recording the chromatogram map to obtain an HPLC fingerprint map overlay map shown in figure 3, which sequentially corresponds to each other from bottom to top: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
2.2 method two
Sample preparation
Raw material medicinal material solution: taking 0.5g of salted morinda officinalis (1-15) powder, putting the powder into a 50ml measuring flask, adding 3% methanol, carrying out ultrasonic treatment (power is 250W, frequency is 40kHz) for 30 minutes, cooling, diluting with 3% methanol to scale, shaking up, filtering with medium-speed filter paper (30-502 mu m), and taking the subsequent filtrate to obtain the morinda officinalis salt preparation.
Control solution: a proper amount of the reference substance of the nougat is precisely weighed, and 3% methanol is added to prepare a solution containing 0.35mg per 1ml as a reference substance solution of the reference substance.
High performance liquid chromatography detection
The detection conditions of the high performance liquid chromatography are as follows:
chromatography apparatus: thermo Scientific Vanquish (ultra high performance liquid phase);
a detector: a CAD detector;
a chromatographic column: waters ACQUITY
BEH Amide(2.1mm×100mm,1.7μm)
Mobile phase: (A) acetonitrile; (B) water;
gradient of mobile phase:
the flow rate is 0.4 ml/min; the sample amount is 1 mul; the column temperature is 35 ℃; operating time: 30 min;
measuring, and recording the chromatogram map to obtain an HPLC fingerprint map overlay map shown in figure 4, which sequentially corresponds to each other from bottom to top: salted morinda officinalis 1, salted morinda officinalis 2, salted morinda officinalis 3, salted morinda officinalis 4, salted morinda officinalis 5, salted morinda officinalis 6, salted morinda officinalis 7, salted morinda officinalis 8, salted morinda officinalis 9, salted morinda officinalis 10, salted morinda officinalis 11, salted morinda officinalis 12, salted morinda officinalis 13, salted morinda officinalis 14 and salted morinda officinalis 15.
As can be seen from fig. 3-4, the fingerprints of morinda citrifolia 1-morinda citrifolia 15 are highly consistent, thereby establishing a common fingerprint pattern for morinda citrifolia and performing similarity analysis on all samples. According to the common mode map, an included angle cosine algorithm is adopted to evaluate the similarity of 15 batches of the raw materials of the salted morinda officinalis according to the components of each sample and the peak area of the component, and the result is shown in table 1.
TABLE 1
According to the above similarity analysis results, the similarity of the original medicinal materials of 15 batches of salted morinda officinalis is very high, and the raw materials can be selected as the raw materials of the contrast extract of the salted morinda officinalis formula particles.
Example 2: preparation of Morinda citrifolia granule control extract
This example provides a method for preparing a morinda citrifolia formulation granule control extract of the present invention, the flow chart of which is shown in fig. 5.
Firstly, the following steps: extraction of
Selecting morinda officinalis, making into powder, adding water with a volume 10 times of the mass of morinda officinalis (namely a solid-to-liquid ratio of 1: 10(w/V, g/ml)), decocting for 30min, filtering with a filter bag with a pore diameter of 10 mu m, collecting filter residue 1 and filtrate 1, extracting filter residue 1 again by the same method, combining the filtrate collected by re-extraction with filtrate 1 to obtain an extract, and concentrating the extract into a solvent to obtain the morinda officinalis dry paste.
II, secondly: preparing Morinda citrifolia extract
Dissolving the dried extract of Morinda citrifolia with water 5 times the weight (w/V, g/ml) of Morinda citrifolia dry extract to obtain water solution, adding silica gel micropowder (Tianjin Longhua Chengxin powder technology Co., Ltd., batch No. 202106013210) 45% of the dried extract, mixing, concentrating at low temperature (less than 45 deg.C) with rotary evaporator to dry, pulverizing, and sieving with 110 mesh sieve to obtain Morinda citrifolia extract.
The multi-batch morinda citrifolia powder is prepared into different batches of the morinda citrifolia extract 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 salted morinda officinalis extract obtained in the step (II) according to the weight ratio of 1:1:1:1: the morinda citrifolia control extract is obtained by mixing and blending in a ratio of 1:1:1:1:1:1:1, and the extraction method has stronger pertinence and is a method adopted by the formula particle control extract, so the obtained morinda citrifolia control extract is also called the morinda citrifolia formula particle control extract.
The blending standard is as follows: the spectrum of the finally obtained control extract is consistent with the spectrum of the morinda citrifolia, and the content range of each component in the blending standard is also the best data obtained by comprehensively maintaining stability and consistency through repeated experiments and the subsequent application.
Fourthly, the method comprises the following steps: detection of
Measuring the reference extract of the formula granules of the salted morinda officinalis 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 reference fingerprint of the salted morinda officinalis) of 15 batches of the salted morinda officinalis extracts, wherein as shown in figures 6-7, ERS corresponds to the reference extract of the formula granules of the salted morinda officinalis, R is the reference fingerprint of the salted morinda officinalis, the similarity obtained in the first method is 1.000, the similarity obtained in the second method is 0.999, and the similarity between the reference extract of the formula granules of the salted morinda officinalis and the reference fingerprint of the salted morinda officinalis is high.
Example 3: character analysis of morinda citrifolia formula granule control extract
1. Apparent state: the control extract of the salted morinda citrifolia formulation of example 2 was a light tan powder.
2. The water content is determined according to the second method of 0832 (determination. detection result is that the water content of the control extract of the morinda officinalis formula particles is 5.7 percent).
3. And (3) testing consistency: control extracts of 15 batches of morinda citrifolia formulation granules were prepared as in example 2 and the differences in TLC profile from batch to batch were determined to be small. Therefore, the consistency of the saline morinda officinalis formula particle control extract prepared by the preparation method of the saline morinda officinalis formula particle control extract is very good.
Claims (9)
1. A method for preparing a morinda citrifolia 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 salted morinda officinalis 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 a dried morinda officinalis extract;
step two, preparing a morinda citrifolia extract: dissolving the morinda citrifolia dry paste obtained in the step two in water to obtain a morinda citrifolia dry paste water solution, adding auxiliary materials, drying and sieving to obtain a morinda citrifolia extract;
step three, blending: blending different batches of the morinda citrifolia extract to obtain a morinda citrifolia formula particle 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 ═ 1.
3. The preparation method of claim 1, wherein the weight-to-volume ratio of the salted morinda citrifolia 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 morinda officinalis how to the water in the first step is 1: 5;
optionally, the decocting time in the first step is 1-300 min;
optionally, the decocting time in the first step is 60 min;
optionally, the filtration in the first step is medium-speed filter paper or a filter bag;
optionally, the filtration in step one is filtration with a filter bag;
optionally, the aperture of the filter bag in the first step is 10-200 μm;
optionally, the filter bag in the first step has a pore size of 10 μm.
4. The preparation method of claim 1, wherein the weight-to-volume ratio of the dry extract of morinda officinalis how to the 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 morinda officinalis dry paste to water in the second step is 1: 5;
optionally, the weight of the auxiliary materials is 10-50% of the weight of the dry extract of morinda officinalis;
optionally, the weight of the auxiliary materials is 45% of the dry extract of morinda citrifolia;
optionally, the auxiliary material is micropowder silica gel;
optionally, filtering the dried product in the third step by a screen of 90-200 meshes;
optionally, the step three is dried and then screened by a 110-mesh screen.
5. The method as claimed in claim 1, further comprising a pre-blending step of detecting different batches of the Morinda citrifolia extract by thin layer chromatography and/or high performance liquid chromatography between the second and third steps.
6. A control extract of salted morinda citrifolia granules, wherein the control extract of salted morinda citrifolia granules is obtained by the preparation method of any one of claims 1 to 5;
optionally, the reference extract of the salted morinda citrifolia formula particles is obtained by adopting thin layer chromatography and/or high performance liquid chromatography, and the obtained map is consistent with the map;
optionally, the spectrum of the control extract of the morinda citrifolia formulation particles obtained by thin layer chromatography and/or high performance liquid chromatography is consistent with the spectrum of the morinda citrifolia at the position of the nougat and/or the monotropein;
optionally, the salted morinda citrifolia granule control extract contains a major amount of a composition comprising nougat and monotropein.
7. The use of the salted Morinda citrifolia formulation control extract of claim 6 for identification.
8. The use of claim 7, wherein said identification method is: detecting the control extract of Morinda citrifolia formulation particles of claim 6 by thin layer chromatography and/or high performance liquid chromatography, and comparing;
optionally, the thin layer chromatography and/or high performance liquid chromatography is used for detecting the main components in the control extract and the medium of the morinda citrifolia formula granules, wherein the main components comprise the nougat and/or the monotropein;
optionally, when the salted morinda citrifolia formulation granule control extract of claim 6 is tested by thin layer chromatography, the salted morinda citrifolia formulation granule control extract is tested after being formulated into a solution, wherein the formulation method of the salted morinda citrifolia formulation granule control extract solution is method one or method two, and the method one is as follows: weighing 1g to 5g of the saline morinda officinalis formula particle control extract as claimed in claim 6, adding 10mL to 40mL of water to dissolve the saline morinda officinalis formula particle control extract, carrying out ultrasonic treatment for 10 min to 60min, adding 10mL to 50mL of water to extract for 1 to 3 times by shaking with ethyl acetate, merging ethyl acetate solutions, evaporating to dryness, adding 0.5mL to 2mL of methanol to dissolve residues, and filtering with 0.12 μm to 0.32 μm of filter membrane to obtain a saline morinda officinalis formula particle control extract solution; the second method comprises the following steps: weighing a proper amount of the morinda citrifolia formula particle control extract as claimed in claim 7, adding water, performing ultrasonic dissolution to prepare a solution containing 10-30 mg of the morinda citrifolia formula particle control extract per 1ml, and filtering through a 0.12-0.32 μm filter membrane to obtain a morinda citrifolia formula particle control extract solution;
optionally, the sample size of the morinda citrifolia granule control extract obtained in the first mentioned method is 3 g; the water adding amount is 25 ml; the number of times of shaking and extracting the ethyl acetate is 2, and each time is 20 ml; the amount of the methanol is 1ml, and the filter membrane is 0.22 mu m;
optionally, the second method prepares 1ml solution containing 15m, 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 GF 254 Prefabricating a slab;
sample application: 10 mul, spot in a strip shape;
developing agent:
toluene-ethyl acetate-formic acid in a volume ratio of 8:2: 0.1;
and (6) inspection:
inspecting under 254nm 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: spreading ethyl acetate-methanol-glacial acetic acid-water in a volume ratio of 8:3:3:1.8 twice;
and (6) inspection: viewing under visible light.
9. The use of claim 8, wherein said comparison extract of Morinda citrifolia formulation of claim 6 and said detection by HPLC requires the detection of said comparison extract of Morinda citrifolia formulation in solution, wherein said comparison extract of Morinda citrifolia formulation is prepared by one or two methods, said one method comprising: adding 10% -50% methanol to the saline morinda citrifolia formulation granule control extract of claim 6 to form a methanol solution of the saline morinda citrifolia formulation granule control extract with a concentration of 2mg/mL to 15mg/mL, and filtering through a 0.12-0.32 μm filter membrane to obtain a saline morinda citrifolia formulation granule control extract solution; the second method comprises the following steps: adding 1% -10% methanol to the control extract of Morinda citrifolia formulation of claim 6 to obtain a methanol solution of 2mg/mL-15mg/mL, and filtering through a 0.12-0.32 μm membrane to obtain a control extract solution of Morinda citrifolia formulation;
optionally, in the first method, the concentration of the methanol is 10%, and the concentration of the solution is 10 mg/mL; the filter membrane is 0.22 mu m;
optionally, in the first method, the concentration of the methanol is 3%, and the concentration of the solution is 10 mg/mL; the filter membrane is 0.22 mu m;
optionally, the detection conditions of the high performance liquid chromatography are detection condition one or detection condition two:
the first detection condition is as follows:
a chromatographic instrument: thermo Scientific Vanqish ultra high performance liquid chromatograph;
a detector: DAD detector
And (3) chromatographic column: YMC Triart C18, 2.1mm × 100mm, 1.9 μm;
mobile phase: (A) methanol; (B) 0.1% phosphoric acid solution
Gradient of mobile phase:
detection wavelength: 235 nm; the flow rate is 0.4 ml/min; the sample volume is 2 mul; the column temperature is 35 ℃; operating time: and (4) 14 min.
The second detection condition is as follows:
chromatography apparatus: thermo Scientific Vanqish ultra high performance liquid chromatograph;
a detector: CAD detector
A chromatographic column: waters ACQUITY
BEH Amide，2.1mm×100mm，1.7μm；
Mobile phase: (A) acetonitrile; (B) water (W)
Gradient of mobile phase:
the flow rate is 0.4 ml/min; the sample amount is 1 mul; the column temperature is 35 ℃; operating time: and (3) 30 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030675A (en) * | 2018-07-05 | 2018-12-18 | 广州卡马生物科技有限公司 | A kind of Morinda officinalis reference extract and its preparation method and application |
| CN109464518A (en) * | 2018-09-30 | 2019-03-15 | 康美药业股份有限公司 | A kind of preparation method of stir-baking RADIX MORINDAE after sprinking salt solution day granule |
| CN110824095A (en) * | 2019-11-29 | 2020-02-21 | 北京康仁堂药业有限公司 | Method for identifying morinda officinalis formula particles and prepared morinda officinalis formula particles |
-
2022
- 2022-05-07 CN CN202210490266.3A patent/CN114965808A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030675A (en) * | 2018-07-05 | 2018-12-18 | 广州卡马生物科技有限公司 | A kind of Morinda officinalis reference extract and its preparation method and application |
| CN109464518A (en) * | 2018-09-30 | 2019-03-15 | 康美药业股份有限公司 | A kind of preparation method of stir-baking RADIX MORINDAE after sprinking salt solution day granule |
| CN110824095A (en) * | 2019-11-29 | 2020-02-21 | 北京康仁堂药业有限公司 | Method for identifying morinda officinalis formula particles and prepared morinda officinalis formula particles |
Non-Patent Citations (3)
| Title |
|---|
| 国家药典委员会: "中华人民共和国药典 2005版 第一部", 31 December 2005, 化学工业出版社, pages: 55 * |
| 廖慧君 等: "巴戟天寡糖的高效薄层色谱指纹图谱研究", 中国药学杂志, vol. 46, no. 18, 30 September 2011 (2011-09-30), pages 1385 - 1388 * |
| 梁丽金 等: "蒸制时间对盐巴戟天含量及特征图谱的影响研究", 现代中药研究与实践, vol. 34, no. 3, 31 December 2020 (2020-12-31), pages 42 - 47 * |
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