CN105859804A - Eucommia ulmoides extract as well as preparation method and application thereof - Google Patents

Eucommia ulmoides extract as well as preparation method and application thereof Download PDF

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Publication number
CN105859804A
CN105859804A CN201610267548.1A CN201610267548A CN105859804A CN 105859804 A CN105859804 A CN 105859804A CN 201610267548 A CN201610267548 A CN 201610267548A CN 105859804 A CN105859804 A CN 105859804A
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cortex eucommiae
ethanol
column volume
preparation
extracts
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CN201610267548.1A
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Inventor
康兴东
肖军平
吴永忠
张荷英
刘恩位
毛金娣
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JIANGXI POZIN PHARMACEUTICAL Co Ltd
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JIANGXI POZIN PHARMACEUTICAL Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/18Acyclic radicals, substituted by carbocyclic rings
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/26Acyclic or carbocyclic radicals, substituted by hetero rings

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a eucommia ulmoides extract as well as a preparation method and application thereof, belonging to the technical field of traditional Chinese medicine. The eucommia ulmoides extract contains the following components in percentage by mass: 3.10-3.70% of cycloolivil-9-glucoside, 1.40-1.70% of cycloolivil-4'-glucoside and 9.50-10.50% of arctiin. The eucommia ulmoides extract is prepared by the steps of eucommia ulmoides grinding, extraction, concentration, centrifugation, standing and separation using macroporous adsorption resin. The eucommia ulmoides extract has a remarkable anti-inflammatory effect.

Description

A kind of Cortex Eucommiae extract and its preparation method and application
Technical field
The invention belongs to technical field of Chinese medicines, particularly belong to a kind of Cortex Eucommiae extract and its preparation method and application.
Background technology
The Cortex Eucommiae (Eucommia ulmoides Oliv.) is the dry bark of the Eucommiaceae plant Cortex Eucommiae, is China's tradition name Your tonic Chinese medicine, for invigorating the liver and kidney, bone and muscle strengthening.Modern pharmacology research finds, the Cortex Eucommiae has several functions activity, such as: fall blood Pressure effect, defying age, anticancer, antibacterial, analgesia, antiinflammatory, diuresis, calmness, to calm the nerves, antivirus action, enhancing body is non-specific to be exempted from Epidemic disease power, and cellular immunization can be carried out the effects such as dual modulation, additionally nerve centre is also had certain effect etc..
The Cortex Eucommiae being shown in, the chemical composition that document is reported includes lignanoids, iridoids, Phenylpropanoid Glycosides class, flavonoid etc. About 200 chemical compositions altogether.Lignanoids compounds is most study in chemical component of eucommia bark used, composition is the clearest and the most definite, structure is the most clear A clear compounds, separated obtain is double tetrahydrofuran compounds mostly.Up to now, separate from the Cortex Eucommiae Lignanoids compounds have 44, mostly be glycosides compound, its glycosyl is β-D-Glucose.Structure type mostly is bis-epoxy Lignanoid (bisepoxylignans, i.e. double tetrahydrofuran class), such as pinoresinol diglucoside, Flos Caryophylli fat diglucoside Deng, the most a small amount of monocycle oxygen lignanoid (monoepoxylignans), neolignan (neolignans), sesquilignan And ring lignanoid (cyclolignans) etc. (sesqiulignans).Have no Cortex Eucommiae report in terms of inflammatory applications.
Summary of the invention
It is an object of the invention to for defect described above, it is provided that a kind of Cortex Eucommiae extract with notable anti-inflammatory activity.
It is a further object of the present invention to provide the preparation method and application of a kind of Cortex Eucommiae extract.
It is an object of the invention to be accomplished by.
A kind of Cortex Eucommiae extract, extracts with the Cortex Eucommiae for raw material and obtains, described Cortex Eucommiae extract Fructus Canarii albi resin on ring Element 9-glucosides, ring olivil 4'-glucosides and arctiin, its mass percent should be 3.10~3.70%, 1.40 mutually ~1.70%, 9.50~10.50%.
The preparation method of a kind of Cortex Eucommiae extract, comprises the steps:
Take the Cortex Eucommiae to pulverize, successively with the 80-95% alcohol reflux 2 times of its 8-12 times of volume, each 2h, filtration;Medicinal residues add The 60-80% alcohol reflux of 6-10 times of volume 1 time, extracts 2h, filters;Merge 3 eucommoil extracts, reclaim ethanol also It is concentrated into containing 0.4-0.6g crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 0.8- 1.2mlmin-1Speed by HPD 100 macroporous resin;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively with 4-6 times Column volume purified water, 6-10 times of column volume 10-30% ethanol elution, discard, then wash with 6-10 times of column volume 80-95% ethanol De-, collect 80-95% ethanol elution part, eluent decompression and solvent recovery, 60 DEG C are dried.Pulverize, to obtain final product.
Preferably include following steps:
Take the Cortex Eucommiae to pulverize, successively with 90% alcohol reflux 2 times of its 10 times of volumes, each 2h, filtration;Medicinal residues add 8 times of bodies 70% alcohol reflux of accumulated amount 1 time, extracts 2h, filters;Merge 3 eucommoil extracts, reclaim ethanol and be concentrated into containing 0.5g Crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 1.0mlmin-1Speed by HPD 100 Macroporous resin;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively by 5 times of column volume purified water, 8 times of column volume 20% ethanol Eluting, discards, and then with 8 times of column volume 90% ethanol elutions, collects 90% ethanol elution part, eluent decompression and solvent recovery, 60 DEG C are dried.Pulverize, to obtain final product.
Above-mentioned Cortex Eucommiae extract can be applied in anti-inflammatory drug.
Compared with prior art the invention has the beneficial effects as follows: present invention firstly provides with ring olivil 9-sugar Glycosides, ring olivil 4'-glucosides and arctiin are the Cortex Eucommiae extract of main active.The test of pesticide effectiveness shows, the Cortex Eucommiae Extract has obvious anti-inflammatory activity.
Detailed description of the invention
The present invention will be further described by the following examples, but not thereby limiting the invention.
The preparation one of embodiment 1 Cortex Eucommiae extract.
Eucommia ulmoides 20kg pulverizes, the 95% ethanol 220L being separately added into, heating and refluxing extraction 2 times, each 2 hours, filter Cross;Medicinal residues add 80% ethanol 200L reflux, extract, 1 time, extract 2h, filter;Merge 3 eucommoil extracts, reclaim ethanol and concentrate To containing 0.6g crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 1.2mlmin-1Speed pass through HPD 100 macroporous resin;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively by 6 times of column volume purified water, 10 times of column volumes 20% ethanol elution, discards, and then with 10 times of column volume 90% ethanol elutions, collects 90% ethanol elution part, and eluent reduces pressure back Receiving solvent, 60 DEG C are dried.Pulverize, obtain Cortex Eucommiae extract 0.32kg.
Through HPLC method assay, Cortex Eucommiae extract medium ring olivil 9-glucosides, ring olivil 4'-glucosides and The content of arctiin is respectively 3.24%, and 1.52%, 9.77%.
The preparation two of embodiment 2 Cortex Eucommiae extract.
Eucommia ulmoides 100kg, the 90% ethanol 1000L being separately added into, heating and refluxing extraction 2 times, each 2 hours, filter; Medicinal residues add 70% ethanol 800L reflux, extract, 1 time, extract 2h, filter;Merge 3 eucommoil extracts, reclaim ethanol being concentrated into and contain 0.5g crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 1.0mlmin-1Speed pass through HPD 100 macroporous resins;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively by 5 times of column volume purified water, 8 times of column volume 20% second Alcohol eluting, discards, and then with 8 times of column volume 90% ethanol elutions, collects 90% ethanol elution part, and eluent recovered under reduced pressure is molten Agent, 60 DEG C are dried.Pulverize, obtain Cortex Eucommiae extract 1.44kg.
Through HPLC method assay, Cortex Eucommiae extract medium ring olivil 9-glucosides, ring olivil 4'-glucosides and The content of arctiin is respectively 3.53%, and 1.68%, 10.36%.
The application in terms of antiinflammatory of embodiment 3 Cortex Eucommiae extract.
Take male mice in kunming 60, male and female half and half, be randomly divided into negative control group (the CMC-Na solution of 0.6%), Positive controls (aspirin 100mgkg-1, celecoxib 5mgkg-1), Cortex Eucommiae extract high, medium and low dosage group (400mgkg-1、200mgkg-1、100mgkg-1) often organize 10.Gastric infusion every day 1 time respectively of each treated animal, successive administration 3d, last is administered Uniformly being applied to two sides before and after left ear with dimethylbenzene 0.1ml after 30min, auris dextra compares.After causing inflammation, 20min is by sacrifice, edge Two ears cut by auricle line, lay auricle with the rustless steel card punch of diameter 8mm respectively at same position, weigh, with left and right auricle The difference of quality be swelling.
Auricle edema suppression ratio (%)=(blank group auricle swelling degree average administration group auricle swelling degree average)/blank group Auricle swelling degree average × 100%
Mice auricle swelling degree experimental result t inspection statistics through between group is analyzed, and shows Cortex Eucommiae extract each dosage group and model group Relatively having pole significant difference (P < 0.01), display Cortex Eucommiae extract each dosage group all has good antiinflammatory action.Mouse ear Wide swelling test the results are shown in Table 1.
Table 1 mouse auricle swelling test result
Note: compare with negative control group, * P < 0.01.

Claims (4)

1. the preparation method of a Cortex Eucommiae extract, it is characterised in that: described Cortex Eucommiae extract containing ring olivil 9-glucosides, Ring olivil 4'-glucosides and arctiin, mass percent should be mutually 3.10~3.70%, 1.40~1.70%, 9.50~10.50%.
2. the preparation method of a kind of Cortex Eucommiae extract described in claim 1, it is characterised in that: comprise the steps: to take the Cortex Eucommiae Pulverize, successively with the 80-95% alcohol reflux 2 times of its 8-12 times of volume, each 2h, filtration;Medicinal residues add 6-10 times of volume The 60-80% alcohol reflux of amount 1 time, extracts 2h, filters;Merge 3 eucommoil extracts, reclaim ethanol being concentrated into and contain 0.4-0.6g crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 0.8-1.2ml min-1Speed Degree is by HPD 100 macroporous resin;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively with 4-6 times of column volume purified water, 6- 10 times of column volume 10-30% ethanol elutions, discard, and then with 6-10 times of column volume 80-95% ethanol elution, collect 80-95% ethanol Elution fraction, eluent decompression and solvent recovery, 60 DEG C dry, pulverize, to obtain final product.
The preparation method of a kind of Cortex Eucommiae extract the most according to claim 2, it is characterised in that: comprise the steps: to take The Cortex Eucommiae is pulverized, successively with 90% alcohol reflux 2 times of its 10 times of volumes, and each 2h, filtration;Medicinal residues add 8 times of volumes 70% alcohol reflux 1 time, extracts 2h, filters;Merge 3 eucommoil extracts, reclaim ethanol and be concentrated into containing 0.5g crude drug ml-1Runny plaste;Runny plaste stands 12h, centrifugal, takes supernatant;Supernatant is with 1.0ml min-1Speed by HPD 100 macropore Resin;Applied sample amount is less than 2.0g crude drug ml-1Resin, successively by 5 times of column volume purified water, 8 times of column volume 20% ethanol elutions, Discard, then with 8 times of column volume 90% ethanol elutions, collect 90% ethanol elution part, eluent decompression and solvent recovery, do for 60 DEG C Dry, pulverize, to obtain final product.
4. a kind of Cortex Eucommiae extract described in claim 1, it is characterised in that: it is applied to prepare in anti-inflammatory drug.
CN201610267548.1A 2016-04-27 2016-04-27 Eucommia ulmoides extract as well as preparation method and application thereof Pending CN105859804A (en)

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CN110679688A (en) * 2019-10-31 2020-01-14 青川县川申农特产开发有限公司 Honey oolong tea beverage
CN113559142A (en) * 2021-08-20 2021-10-29 江西普正制药股份有限公司 Extraction method and application of eucommia lignans
CN113797215A (en) * 2021-08-31 2021-12-17 江西普正制药股份有限公司 Composition containing pinoresinol and cycloolivil 9-glucoside and preparation method and application thereof
CN113797214A (en) * 2021-08-31 2021-12-17 江西普正制药股份有限公司 Composition containing cycloolivil 4' -glucoside and preparation method and application thereof
CN115837026A (en) * 2022-11-08 2023-03-24 暨南大学附属第一医院(广州华侨医院) Composition and application thereof in preparing medicine with anti-hepatitis effect

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110679688A (en) * 2019-10-31 2020-01-14 青川县川申农特产开发有限公司 Honey oolong tea beverage
CN113559142A (en) * 2021-08-20 2021-10-29 江西普正制药股份有限公司 Extraction method and application of eucommia lignans
CN113797215A (en) * 2021-08-31 2021-12-17 江西普正制药股份有限公司 Composition containing pinoresinol and cycloolivil 9-glucoside and preparation method and application thereof
CN113797214A (en) * 2021-08-31 2021-12-17 江西普正制药股份有限公司 Composition containing cycloolivil 4' -glucoside and preparation method and application thereof
CN113797215B (en) * 2021-08-31 2023-11-24 江西普正制药股份有限公司 Composition containing pinoresinol and cycloolivil 9-glycoside and preparation method and application thereof
CN113797214B (en) * 2021-08-31 2023-11-24 江西普正制药股份有限公司 Composition containing cyclo-olivil 4' -glycoside and preparation method and application thereof
CN115837026A (en) * 2022-11-08 2023-03-24 暨南大学附属第一医院(广州华侨医院) Composition and application thereof in preparing medicine with anti-hepatitis effect
CN115837026B (en) * 2022-11-08 2024-01-26 暨南大学附属第一医院(广州华侨医院) Composition and application thereof in preparation of medicines with anti-hepatitis effect

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