CN107325071A - A kind of preparation method and purposes of the Hickory Leaves pinostrobin with hypoglycemic effect - Google Patents
A kind of preparation method and purposes of the Hickory Leaves pinostrobin with hypoglycemic effect Download PDFInfo
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- CN107325071A CN107325071A CN201710415347.6A CN201710415347A CN107325071A CN 107325071 A CN107325071 A CN 107325071A CN 201710415347 A CN201710415347 A CN 201710415347A CN 107325071 A CN107325071 A CN 107325071A
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- pinostrobin
- hickory leaves
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- hickory
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- 241000723418 Carya Species 0.000 title claims abstract description 71
- ORJDDOBAOGKRJV-CQSZACIVSA-N (2S)-Pinocembrin Natural products C1([C@H]2CC(=O)C3=C(O)C=C(C=C3O2)OC)=CC=CC=C1 ORJDDOBAOGKRJV-CQSZACIVSA-N 0.000 title claims abstract description 43
- ORJDDOBAOGKRJV-UHFFFAOYSA-N Dihydrotectochrysin Natural products O1C2=CC(OC)=CC(O)=C2C(=O)CC1C1=CC=CC=C1 ORJDDOBAOGKRJV-UHFFFAOYSA-N 0.000 title claims abstract description 43
- ORJDDOBAOGKRJV-AWEZNQCLSA-N pinostrobin Chemical compound C1([C@@H]2CC(=O)C3=C(O)C=C(C=C3O2)OC)=CC=CC=C1 ORJDDOBAOGKRJV-AWEZNQCLSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000002218 hypoglycaemic effect Effects 0.000 title claims abstract description 16
- 239000003814 drug Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 57
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000287 crude extract Substances 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000004952 Polyamide Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 229920002647 polyamide Polymers 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
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- 239000003480 eluent Substances 0.000 claims description 3
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- 239000000203 mixture Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
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- 238000012644 addition polymerization Methods 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000002775 capsule Substances 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- 239000003405 delayed action preparation Substances 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000006187 pill Substances 0.000 claims description 2
- 239000007901 soft capsule Substances 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 239000003826 tablet Substances 0.000 claims 1
- 206010012601 diabetes mellitus Diseases 0.000 abstract description 13
- 239000008280 blood Substances 0.000 abstract description 9
- 210000004369 blood Anatomy 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 241000699670 Mus sp. Species 0.000 abstract description 3
- 206010018473 Glycosuria Diseases 0.000 abstract description 2
- 241000699666 Mus <mouse, genus> Species 0.000 description 15
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 8
- 229940079593 drug Drugs 0.000 description 6
- 201000001421 hyperglycemia Diseases 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000010172 mouse model Methods 0.000 description 5
- HIMXGTXNXJYFGB-UHFFFAOYSA-N alloxan Chemical compound O=C1NC(=O)C(=O)C(=O)N1 HIMXGTXNXJYFGB-UHFFFAOYSA-N 0.000 description 4
- 229930003944 flavone Natural products 0.000 description 4
- 235000011949 flavones Nutrition 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- -1 Flavone compound Chemical class 0.000 description 3
- 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 3
- 208000008589 Obesity Diseases 0.000 description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 238000003304 gavage Methods 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 235000020824 obesity Nutrition 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
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- 238000002425 crystallisation Methods 0.000 description 2
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- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 150000002212 flavone derivatives Chemical class 0.000 description 2
- 235000013402 health food Nutrition 0.000 description 2
- 241000411851 herbal medicine Species 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000012109 statistical procedure Methods 0.000 description 2
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 201000004569 Blindness Diseases 0.000 description 1
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000758791 Juglandaceae Species 0.000 description 1
- 241000305527 Juglans cathayensis Species 0.000 description 1
- 235000014075 Juglans mandschurica Nutrition 0.000 description 1
- 108010092277 Leptin Proteins 0.000 description 1
- 206010029164 Nephrotic syndrome Diseases 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 241000130764 Tinea Species 0.000 description 1
- 208000002474 Tinea Diseases 0.000 description 1
- 206010067584 Type 1 diabetes mellitus Diseases 0.000 description 1
- VSQUZVLNMULDCY-UHFFFAOYSA-N [O].C1=CC=NC=C1 Chemical compound [O].C1=CC=NC=C1 VSQUZVLNMULDCY-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 230000003113 alkalizing effect Effects 0.000 description 1
- 238000000540 analysis of variance Methods 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003527 anti-angiogenesis Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 230000002567 autonomic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 description 1
- 229940093265 berberine Drugs 0.000 description 1
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 208000016097 disease of metabolism Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- IXZISFNWUWKBOM-ARQDHWQXSA-N fructosamine Chemical compound NC[C@@]1(O)OC[C@@H](O)[C@@H](O)[C@@H]1O IXZISFNWUWKBOM-ARQDHWQXSA-N 0.000 description 1
- 208000004104 gestational diabetes Diseases 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
- 208000037890 multiple organ injury Diseases 0.000 description 1
- 208000009928 nephrosis Diseases 0.000 description 1
- 231100001027 nephrosis Toxicity 0.000 description 1
- 238000001543 one-way ANOVA Methods 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 208000008128 pulmonary tuberculosis Diseases 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/32—2,3-Dihydro derivatives, e.g. flavanones
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/52—Juglandaceae (Walnut family)
Abstract
The present invention relates to a kind of preparation method and purposes of the Hickory Leaves pinostrobin with hypoglycemic effect, the mass percent containing pinostrobin is more than 90%.The Hickory Leaves pinostrobin can significantly reduce the blood sugar level of diabetic mice, have significant curative effect for diabetes particularly II types glycosuria, available for prevent and treat diabetes be major function medicine and health product.
Description
Technical field
The present invention relates to pharmaceutical technology field, the system of more particularly to a kind of Hickory Leaves pinostrobin with hypoglycemic effect
Preparation Method and purposes.
Background technology
Diabetes are by the excessive caused metabolic disease of glucose in blood accumulation, critical immunologic function.Also because of its disease
Therewith and extremely, diabetic holds hidden infection multi-infection as caused by flu, pneumonia, pulmonary tuberculosis to the trouble of the longer human body of journey very much
Disease, and be difficult to cure.Serious possibility causes whole body multiple organ injury, the complication, harmful to human such as blindness, nephrosis occurs
Health.Diabetes typically divide the diabetes of type 1 diabetes, diabetes B, gestational diabetes mellitus and other specific types.In glycosuria
In patient, the ratio shared by diabetes B is about 95%.With the raising for carrying out Living consumption this year, diabetic
Quantity also greatly increase, this also results in a large amount of hypoglycemic drugs and come out therewith, but at present clinically common medicine for treating diabetes
Thing is generally chemical synthesis class medicine, although determined curative effect, also there is more adverse reaction simultaneously.Natural drug, is through modern times doctor
Animal drugs, autonomic drug and mineral drug with certain pharmacological activity that medicine body system proves etc..
The development of society makes people increasingly pay close attention to the negative effect of chemicals, and under this background, Chinese herbal medicine is undoubtedly
With the advantage do not replaced.Therefore, exploitation both caters to market with the Chinese herbal medicine for preventing and treating diabetes and its complication
Demand has good social benefit again.
Ob/ob mouse are that leptin gene knocks out a kind of congenital obesity mouse obtained, its pathogenic process and mankind's fertilizer
It is fat similar, it is one of more common heredity obese model, is also commonly used for type-II diabetes animal experiment study.
Chinese walnut is a kind of Juglandaceae deciduous tree, and its leaf is more in the harvesting of the season of summer and autumn two, be used as medicine with it is clearing heat and detoxicating, kill
The antipruritic effect of worm.Be mainly used in toe it is wet itch and skin tinea card treatment etc..Research finds to contain in Hickory Leaves extract
A large amount of anti-oxidation active substances, such as flavones, the effects such as with anti-aging, antitumor, anti-angiogenesis.Flavone compound is
One of medicinal plant main active, with wide spectrum pharmacological activity and low toxicity, research shows that Hickory Leaves pinostrobin can
Reduce model ob/ob mouse blood sugar level, available for prevent and treat hyperglycaemia, particularly diabetes B be major function medicine
And health food.
The content of the invention
It is an object of the invention to provide a kind of preparation side of the Hickory Leaves extract pinostrobin with hypoglycemic effect
Method, while there is provided its purposes.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of Hickory Leaves extract pinostrobin with hypoglycemic effect, the mass percent containing pinostrobin 90% with
On.
A kind of preparation method of the Hickory Leaves pinostrobin with hypoglycemic effect, the preparation method includes following step
Suddenly：
(1) Hickory Leaves are placed in baking oven and dry, pulverize sieving, the alcohol reflux for adding 75-95% is extracted, each 30-120
Minute, repeat 1-3 times, filtering, merging filtrate；
(2) filtrate of step (1) is concentrated, 0.7mL, 1mol/L sodium hydroxide solution is added per 4mL filtrates, is added again after mixing
Addition polymerization acid amides is sufficiently mixed, and be concentrated under reduced pressure upper prop, with 4-12BV/h flow velocity, successively with water, 20% ethanol, 40% ethanol,
60% ethanol elution, every kind of solvent elutes 6-10 times of column volume, collects the eluent of 60% ethanol, is concentrated under reduced pressure into dry mountain
Walnut Leave extract；
(3) ratio of 5-35mL methanol is added to add according to every 1g Hickory Leaves crude extract the Hickory Leaves crude extract of step (2)
Enter methanol, and with petroleum ether 1:1 ratio is extracted, and is repeated 3-10 times, then that petroleum ether extraction liquid is dense in 30-50 DEG C of decompression
Drying is reduced to, Hickory Leaves yellow crude extract is produced；
(4) by the Hickory Leaves yellow crude extract of step (3) with 1g:8-12mL ratio, adds 60vol%-90% ethanol
The aqueous solution, is dissolved in 70-90 DEG C of water-bath, after dissolving terminates, is put in rapidly in 4 DEG C of refrigerators, is placed 12-24h, is tied
Crystalline substance, filter paper filtering, obtains Hickory Leaves pinostrobin crystal, pinostrobin content is more than 90%.
Preferably, oven drying temperature is 30-80 DEG C in step (1).
Preferably, step (1) sieving sieve mesh is 40-100 mesh.
Preferably, extraction conditions are 60-120 DEG C of normal pressure in step (1).
Preferably, 70-95% ethanol waters consumption is to add 10mL per 1g Hickory Leaves crushed materials in step (1)
Preferably, the consumption of polyamide is the filtrate addition 5g polyamide after being alkalized per 100mL in step (2).
A kind of purposes of the Hickory Leaves pinostrobin with hypoglycemic effect, by the Hickory Leaves pinostrobin of above-mentioned preparation with
The auxiliary material approved on medicament or food, using Modern preparations technology, is made capsule, piece based on Hickory Leaves pinostrobin
The various formulations such as agent, powder, oral liquid, soft capsule, pill, gel, sustained release preparation and health food.
Beneficial effects of the present invention：The present invention prepares its primary extract by raw material of Juglandaceae Hickory Leaves, and through further
Purifying obtains the Hickory Leaves pinostrobin with hypoglycemic effect, and this method is simple and easy to apply, and further expands Hickory Leaves
Application, with very huge market potential and economic value.
Embodiment
Below by specific embodiment, the present invention is further detailed explanation, but the present invention is not limited to these implementations
Example.
Embodiment 1
Hickory Leaves are crushed in 40 DEG C of drying, cross 40 mesh sieves, weigh powder 100g, add the ethanol solution of 1L volumetric concentrations 85%
Refluxing extraction, 2 times, extraction conditions are 80 DEG C of normal pressure, and each 60min, merging filtrate adds 0.7mL, 1mol/L per 4mL filtrates
Sodium hydroxide solution alkalization 12h, after alkalization by sample solution per 100mL add 5g polyamide (100-200 mesh) ratio mix
Uniformly, drying, upper chromatographic column (15mm × 350mm i.d), successively with 10BV water, 20% ethanol, 40% second are concentrated under reduced pressure into
Alcohol, 60% ethanol elution, collect 60% ethanol eluate, are concentrated under reduced pressure into drying, obtain Hickory Leaves crude extract.
The ratio that above-mentioned Hickory Leaves crude extract is added into 5mL methanol according to every 1g Hickory Leaves crude extract is dissolved,
It is again with isometric petroleum ether extraction 10 times, petroleum ether product at reduced pressure rotary evaporated to dryness is dry, obtain Hickory Leaves yellow and slightly carry
Thing.Hickory Leaves yellow crude extract is dissolved in 90 DEG C, in 80% ethanol, filtered while hot, and filtrate is put in rapidly to 4 DEG C of refrigerators
In, place 12h, crystallization.Crystal solution filter paper is filtered, Hickory Leaves extract pinostrobin crystal is obtained, pinostrobin content exists
More than 90%.
Embodiment 2
Hickory Leaves are placed in 35 DEG C of oven dryings, crushed, 80 mesh sieves are crossed, Hickory Leaves powder 200g is weighed, 2L volumes are added
The alcohol reflux of concentration 95% is extracted, and extraction conditions are 60 DEG C of normal pressure, and 2 times, each 30min, merging filtrate is added per 4mL filtrates
0.7mL, 1mol/L sodium hydroxide solution alkalization 12h, 5g polyamide (100-200 is added per 100mL after alkalization by sample solution
Mesh) ratio be well mixed, be concentrated under reduced pressure into drying, upper chromatographic column (15mm × 350mm i.d), successively with 10BV water, 20%
Ethanol, 40% ethanol, 60% ethanol elution, collect 60% ethanol eluate, are concentrated under reduced pressure into drying, obtain Hickory Leaves and slightly carry
Thing.
The ratio that above-mentioned Hickory Leaves crude extract is added into 20mL methanol according to every 1g Hickory Leaves crude extract is dissolved,
It is again with isometric petroleum ether extraction 10 times, petroleum ether product at reduced pressure rotary evaporated to dryness is dry, obtain Hickory Leaves yellow and slightly carry
Thing.Hickory Leaves yellow crude extract is dissolved in 90 DEG C, in 80% ethanol, filtered while hot, and filtrate is put in rapidly to 4 DEG C of refrigerators
In, place 12h, crystallization.Crystal solution filter paper is filtered, Hickory Leaves extract pinostrobin crystal is obtained, pinostrobin content exists
More than 90%.
Embodiment 3
Hickory Leaves are placed in baking oven 80 DEG C and dry, pulverize 100 mesh sieves, Hickory Leaves powder 300g is weighed, 3L bodies are added
The alcohol reflux of product concentration 75% is extracted, and extraction conditions are 120 DEG C of normal pressure, 120 minutes every time, are repeated 1 times, and is filtered, and merges filter
Liquid；
(2) filtrate of step (1) is concentrated, added per 4mL filtrates after 0.7mL, 1mol/L sodium hydroxide solution, alkalization 12h
Add polyamide again to be sufficiently mixed, the filtrate addition 5g polyamide after alkalizing per 100mL；Be concentrated under reduced pressure upper prop, with 12BV/h's
Flow velocity, successively with water, 20% ethanol, 40% ethanol, 60% ethanol elution, every kind of solvent elutes 6-10 times of column volume, collects
The eluent of 60% ethanol, is concentrated under reduced pressure into dry Hickory Leaves crude extract；
(3) ratio of 35mL methanol is added to add according to every 1g Hickory Leaves crude extract the Hickory Leaves crude extract of step (2)
Methanol, and with petroleum ether 1:1 ratio is extracted, and is repeated 3 times, and is then concentrated under reduced pressure into petroleum ether extraction liquid in 30-50 DEG C
Dry, produce Hickory Leaves yellow crude extract；
(4) by the Hickory Leaves yellow crude extract of step (3) with 1g:12mL ratio, adds 90% ethanol water, 70
Dissolved, after dissolving terminates, be put in rapidly in 4 DEG C of refrigerators in DEG C water-bath, placed 24h, crystallized, filter paper filtering is obtained
Hickory Leaves pinostrobin crystal, pinostrobin content is more than 90%.
Pinostrobin content assaying method is referring to 5 flavone aglycones in the high effective liquid chromatography for measuring Hickory Leaves such as Shen Yong
Content [J] Pharmaceutical Analysis magazines, 05 phase in 2013.
Hickory Leaves pinostrobin causes the Effect study of hyperglycaemia mouse model to alloxan
1. experimental method：
By male ICR mouse 50,6 groups, wherein blank control group 10, each 8 of remaining each group, by 40 models are randomly divided into
Tail vein injection alloxan solution 80mg/kg, which makes, after mouse fasting 12h touches (Normal group injection normal saline), 5d
After survey blood glucose, work as blood glucose>Modeling success during 11.1mmol/L.Then model mice is randomly divided into 5 groups, respectively hyperglycaemia mould
Type group, Hickory Leaves pinostrobin 50mg/kg low dose groups, 100mg/kg middle dose groups, 200mg/kg high dose groups, 50mg/kg
Melbine positive drug group.Normal group and model group give 0.5%CMC-Na gavages during experiment, and remaining each group is by administration
Dosage gavage, 1 time/d, continuous 14d.After 14d, each group mouse blood sugar, body weight and Serum Fructosamine are determined, and record.Experiment knot
Fruit carries out statistical procedures using the statistical softwares of SPSS 18.0.Experimental data is represented with average ± standard deviation, using list
Analysis of variance, thinks there is significant difference during P ＜ 0.05.
2. experimental result
As a result one 1, table 2 is shown in Table, understands that Hickory Leaves pinostrobin can significantly reduce mouse's blood sugar content in table, it is phonetic to four oxygen
Pyridine causes hyperglycaemia mouse model to have remarkable effect.
Influence of the Hickory Leaves pinostrobin of table 1 to hyperglycemia model mouse
Note：Compared with normal group,**P<0.01；Compared with model group,#P<0.05,##P<0.01。
Influence of the Hickory Leaves general flavone different dosing dosage of table 2 to hyperglycaemia mouse weight
Note：Compared with normal group,**P<0.01；Compared with model group,#P<0.05。
Effect study of the Hickory Leaves pinostrobin to ob/ob Mice model of obesity
1. experimental method
8 week old ob/ob male mices 40 are taken, adaptability is raised l weeks, and mouse then is randomly divided into Hickory Leaves pinostrobin
50mg/kg low dose groups, 100mg/kg middle dose groups, 200mg/kg high dose groups, 50mg/kg berberine positive drug groups, and with
C57 mouse are used as Normal group, 1 times/day of gavage of each group mouse.Continuous 28d.After 28d, determine each group mouse blood sugar and remember
Record.Experimental result carries out statistical procedures using the statistical softwares of SPSS 18.0.Experimental data is with average ± standard deviation table
Show, using one-way analysis of variance, think there is significant difference during P ＜ 0.05.
2. experimental result
Experimental result is shown in Table 3, understands that Hickory Leaves pinostrobin can significantly reduce mouse's blood sugar content in table, to obesity mice
That is type ii diabetes model mice works well.
Influence of the Hickory Leaves pinostrobin of table 3 to ob/ob obese model mouse
Note：Compared with normal group,**P<0.01；Compared with model group,#P<0.05,##P<0.01。
Embodiment described above is a kind of preferably scheme of the present invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (7)
1. a kind of preparation method of the Hickory Leaves pinostrobin with hypoglycemic effect, it is characterised in that the preparation method bag
Include following steps：
(1) Hickory Leaves are placed in baking oven and dry, pulverize sieving, the alcohol reflux for adding 75-95% is extracted, each 30-120
Minute, repeat 1-3 times, filtering, merging filtrate；
(2) filtrate of step (1) is concentrated, 0.7mL, 1mol/L sodium hydroxide solution is added per 4mL filtrates, is added again after mixing
Addition polymerization acid amides is sufficiently mixed, and be concentrated under reduced pressure upper prop, with 4-12BV/h flow velocity, successively with water, 20% ethanol, 40% ethanol,
60% ethanol elution, every kind of solvent elutes 6-10 times of column volume, collects the eluent of 60% ethanol, is concentrated under reduced pressure into dry mountain
Walnut Leave extract；
(3) ratio of 5-35mL methanol is added to add according to every 1g Hickory Leaves crude extract the Hickory Leaves crude extract of step (2)
Enter methanol, and with petroleum ether 1:1 ratio is extracted, and is repeated 3-10 times, then that petroleum ether extraction liquid is dense in 30-50 DEG C of decompression
Drying is reduced to, Hickory Leaves yellow crude extract is produced；
(4) by the Hickory Leaves yellow crude extract of step (3) with 1g:8-12mL ratio, adds 60vol%-90% ethanol
The aqueous solution, is dissolved in 70-90 DEG C of water-bath, after dissolving terminates, is put in rapidly in 4 DEG C of refrigerators, is placed 12-24h, is tied
Crystalline substance, filter paper filtering, obtains Hickory Leaves pinostrobin crystal, pinostrobin content is more than 90%.
2. a kind of preparation method of Hickory Leaves pinostrobin with hypoglycemic effect according to claim 1, its feature
It is, oven drying temperature is 30-80 DEG C in step (1).
3. a kind of preparation method of Hickory Leaves pinostrobin with hypoglycemic effect according to claim 1, its feature
It is, step (1) sieving sieve mesh is 40-100 mesh.
4. a kind of preparation method of Hickory Leaves pinostrobin with hypoglycemic effect according to claim 1, its feature
It is, extraction conditions are 60-120 DEG C of normal pressure in step (1).
5. a kind of preparation method of Hickory Leaves pinostrobin with hypoglycemic effect according to claim 1, its feature
It is, 70-95% ethanol waters consumption is to add 10mL per 1g Hickory Leaves crushed materials in step (1).
6. a kind of preparation method of Hickory Leaves pinostrobin with hypoglycemic effect according to claim 1, its feature
It is, the consumption of polyamide is the filtrate addition 5g polyamide after being alkalized per 100mL in step (2).
7. a kind of purposes of the Hickory Leaves pinostrobin with hypoglycemic effect, it is characterised in that the mountain for preparing claim 1
Walnut Leaves pinostrobin and the auxiliary material approved on medicament or food, using Modern preparations technology, are made with Hickory Leaves pinostrobin
Based on the various formulations such as capsule, tablet, powder, oral liquid, soft capsule, pill, gel, sustained release preparation and health care food
Product.
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| CN109232757A (en) * | 2018-08-31 | 2019-01-18 | 吉首大学 | Walnut Leaves polyoses extract and application |
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