CN107296877A - A kind of preparation method of Longstamen Onion Bulb group saponine - Google Patents
A kind of preparation method of Longstamen Onion Bulb group saponine Download PDFInfo
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- CN107296877A CN107296877A CN201710431325.9A CN201710431325A CN107296877A CN 107296877 A CN107296877 A CN 107296877A CN 201710431325 A CN201710431325 A CN 201710431325A CN 107296877 A CN107296877 A CN 107296877A
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- China
- Prior art keywords
- saponin
- onion bulb
- longstamen onion
- concentration
- aqueous solution
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- Pending
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- 241000304531 Allium macrostemon Species 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims description 14
- SYXUBXTYGFJFEH-UHFFFAOYSA-N oat triterpenoid saponin Chemical compound CNC1=CC=CC=C1C(=O)OC1C(C=O)(C)CC2C3(C(O3)CC3C4(CCC5C(C)(CO)C(OC6C(C(O)C(OC7C(C(O)C(O)C(CO)O7)O)CO6)OC6C(C(O)C(O)C(CO)O6)O)CCC53C)C)C4(C)CC(O)C2(C)C1 SYXUBXTYGFJFEH-UHFFFAOYSA-N 0.000 title claims description 8
- 229930182490 saponin Natural products 0.000 claims abstract description 127
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 125
- -1 spirostanol saponin Chemical class 0.000 claims abstract description 83
- 150000007949 saponins Chemical class 0.000 claims abstract description 71
- GMBQZIIUCVWOCD-UQHLGXRBSA-N Isosarsasapogenin Natural products O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)C[C@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 GMBQZIIUCVWOCD-UQHLGXRBSA-N 0.000 claims abstract description 56
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- 238000010828 elution Methods 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- 239000003960 organic solvent Substances 0.000 claims abstract description 31
- 239000000284 extract Substances 0.000 claims abstract description 25
- 239000002250 absorbent Substances 0.000 claims abstract description 18
- 230000002745 absorbent Effects 0.000 claims abstract description 18
- 235000017709 saponins Nutrition 0.000 claims description 121
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- 239000000243 solution Substances 0.000 claims description 62
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- 238000010521 absorption reaction Methods 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 9
- 101100313763 Arabidopsis thaliana TIM22-2 gene Proteins 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 244000295724 Allium chinense Species 0.000 claims description 3
- 235000016790 Allium chinense Nutrition 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 50
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 40
- 239000000741 silica gel Substances 0.000 description 40
- 229910002027 silica gel Inorganic materials 0.000 description 40
- 150000005856 steroid saponins Chemical class 0.000 description 30
- 238000011161 development Methods 0.000 description 28
- 230000018109 developmental process Effects 0.000 description 28
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 24
- 239000003480 eluent Substances 0.000 description 22
- 238000000605 extraction Methods 0.000 description 18
- 150000003431 steroids Chemical class 0.000 description 17
- SIHHLZPXQLFPMC-UHFFFAOYSA-N chloroform;methanol;hydrate Chemical compound O.OC.ClC(Cl)Cl SIHHLZPXQLFPMC-UHFFFAOYSA-N 0.000 description 14
- 238000009835 boiling Methods 0.000 description 13
- 239000011148 porous material Substances 0.000 description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 11
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- FZRCKLPSHGTOAU-UHFFFAOYSA-N 6-amino-1,4-dimethylcyclohexa-2,4-diene-1-carbaldehyde Chemical compound CC1=CC(N)C(C)(C=O)C=C1 FZRCKLPSHGTOAU-UHFFFAOYSA-N 0.000 description 5
- 229960000583 acetic acid Drugs 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- QIQOZKOHFKBLRO-UHFFFAOYSA-N chloroform;propan-2-ol;hydrate Chemical compound O.CC(C)O.ClC(Cl)Cl QIQOZKOHFKBLRO-UHFFFAOYSA-N 0.000 description 2
- UCPFREPFIWVFSJ-UHFFFAOYSA-N chloroform;propan-2-one;hydrate Chemical compound O.CC(C)=O.ClC(Cl)Cl UCPFREPFIWVFSJ-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 230000003637 steroidlike Effects 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 210000000707 wrist Anatomy 0.000 description 1
Classifications
-
- 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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8962—Allium, e.g. garden onion, leek, garlic or chives
-
- 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
- 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
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Mycology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Microbiology (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Biotechnology (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a kind of method that the separation total furostanol saponin of Longstamen Onion Bulb and the total spirostanol saponin of Longstamen Onion Bulb are extracted from Longstamen Onion Bulb, the main total furostanol saponin of Longstamen Onion Bulb being made up of furostanol saponin is obtained with the aqueous solution elution of low-concentration organic solvent after longstamen onion bulb extract is adsorbed with macroporous absorbent resin, then the main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin is obtained with the aqueous solution elution of high levels of organic solvents.
Description
Technical field
The present invention relates to the preparation side for the method, especially Longstamen Onion Bulb group saponine that separation saponin component is extracted from Longstamen Onion Bulb
Method, belongs to Chinese medicine or Natural Medicine Chemistry research field.
Background technology
Longstamen Onion Bulb refers to liliaceous plant Allium macrostemon Allium macrostemon Bge. dry bulb.Summer, season in autumn two adopts
Dig, clean, remove fibrous root, steam thoroughly or put and scald saturating in boiling water, dry.With activating yang and removing abstruction, stagnant function is led in promoting the circulation of qi；For the obstruction of qi in the chest
It is pained, wrist abdomen feeling of fullness distending pain, weight after rush down dysentery.
Up to the present people get a variety of steroid saponins, including furan steroid type steroid saponin and spiral shell steroid type steroidal from Longstamen Onion Bulb
Saponin(e, these saponin(es are the principle active components of Longstamen Onion Bulb.The furan steroid type steroid saponin and spiral shell steroid type steroid saponin contained in Longstamen Onion Bulb,
Not only had any different in chemical constitution, physicochemical property, and also have difference in terms of bioactivity and toxicity.Therefore from Chinese onion
Prepare the mixture of furan steroid type steroid saponin and the mixture of spiral shell steroid type steroid saponin respectively in white, then further according to they
Bioactivity, which goes to develop corresponding medical usage, to be one and significantly works.But up to the present still not from
The mixture of furan steroid type steroid saponin and the total furan steroid soap of mixture i.e. Longstamen Onion Bulb of spiral shell steroid type steroid saponin are prepared in Longstamen Onion Bulb respectively
Glycosides and the document report for preparing total spirostanol saponin.The most common method for extracting separation saponin component from Longstamen Onion Bulb at present is big
Macroporous adsorbent resin method.Longstamen Onion Bulb is added water to cook into extraction, extract solution crosses macroporous absorbent resin absorption and (or uses ethanol water
Adsorbed after refluxing extraction, extract solution recycling design after macroporous absorbent resin), with ethanol, methanol, acetone etc. after being eluted with water
The aqueous solution is eluted, eluent recycling design, obtains the mixture of saponin component in Longstamen Onion Bulb, i.e. Longstamen Onion Bulb total saposins.So
The total saposins of acquisition are the mixtures of furan steroid type steroid saponin and spiral shell steroid type steroid saponin in Longstamen Onion Bulb.
The content of the invention
Longstamen Onion Bulb of the present invention refers not only to liliaceous plant Allium macrostemon Allium macrostemon Bge. drying squama
Stem, also including its Fresh Bulbs, fresh or dry aerial parts, in addition to fresh or dry herb.
Mixture and the mixture of spiral shell steroid type steroid saponin of the present invention the furan steroid type steroid saponin got from Longstamen Onion Bulb
The total furostanol saponin of Longstamen Onion Bulb and the total spirostanol saponin of Longstamen Onion Bulb are referred to as, both Longstamen Onion Bulb group saponine is referred to as, both are added together
Mixture be referred to as Longstamen Onion Bulb total saposins.
The present invention provides a kind of new method of extraction separation Longstamen Onion Bulb group saponine from Longstamen Onion Bulb and answering for Longstamen Onion Bulb group saponine
With.
As described in the background section, the most common method for extracting separation saponin component from Longstamen Onion Bulb at present is macropore
Adsorption resin method.That is Longstamen Onion Bulb adds water to cook extraction, and extract solution crosses macroporous absorbent resin absorption (or with ethanol, methanol, acetone
Deng aqueous solution refluxing extraction, extract solution reclaim organic solvent after after macroporous absorbent resin adsorb), with ethanol, methanol, acetone
Deng the aqueous solution eluted, eluent recycling design, obtain Longstamen Onion Bulb total saposins.Typically directly used in above-mentioned elution process
The ethanol water elution of higher concentration, so whole saponin(es are eluted, what is obtained is Longstamen Onion Bulb total saposins.We are by grinding
Study carefully discovery, if adjusting the concentration of ethanol (or methanol, acetone) relatively low, i.e., (compared with the aqueous solution of the ethanol of low concentration
As 30%) eluted, the composition eluted is the furan steroid type steroid saponin in Longstamen Onion Bulb, and spiral shell steroid type steroid saponin is still adsorbed
On macroporous absorbent resin.Find to be eluted with 20% to 40% ethanol water after conscientious careful research, will elute
The composition got off carries out TLC inspections, and it is the furan steroid type steroid saponin in Longstamen Onion Bulb to find the composition eluted, by furan steroid type steroidal
After saponin(e elution completely, eluted with the ethanol water more than 45%, the composition eluted is subjected to TLC inspections, finds to wash
The composition taken off is the spiral shell steroid type steroid saponin in Longstamen Onion Bulb.It is again seen that with concentration of volume percent be more than 15% to less than
The composition eluted during 40% methanol aqueous solution elution is the furan steroid type steroid saponin in Longstamen Onion Bulb, with the methanol more than 40%
The composition that the aqueous solution is eluted when eluting is the spiral shell steroid type steroid saponin in Longstamen Onion Bulb；It is less than with more than 15% to 40% acetone water
The composition that solution is eluted when eluting is the furan steroid type steroid saponin in Longstamen Onion Bulb, when being eluted with the aqueous acetone solution more than 40%
The composition eluted is the spiral shell steroid type steroid saponin in Longstamen Onion Bulb；With more than 17% to the normal propyl alcohol or isopropanol water less than 40%
The composition that solution is eluted when eluting is the furan steroid type steroid saponin in Longstamen Onion Bulb, with the normal propyl alcohol or isopropanol water more than 40%
The composition that solution is eluted when eluting is the spiral shell steroid type steroid saponin in Longstamen Onion Bulb.
The studies above result shows, the organic molten of low concentration is first used after Longstamen Onion Bulb water extract is adsorbed with macroporous absorbent resin
The aqueous solution elution of agent can obtain the main total furostanol saponin of Longstamen Onion Bulb being made up of furostanol saponin, after after furostanol saponin elution completely
The main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin can be obtained by using the aqueous solution elution of the organic solvent of high concentration instead.No
The busy difference of concentration that same organic solvent and different macroporous absorbent resins are required, but difference is little.
Described macroporous absorbent resin be selected from AB-8, D4020, D101, D102, D103,860021, HP20 one kind or it
Two or more hybrid resin.
Described organic solvent be selected from ethanol, methanol, acetone, normal propyl alcohol, isopropanol or they one or both of or
Two or more mixed solvents.
The aqueous solution of described low-concentration organic solvent refers to the organic solvent that concentration of volume percent is less than or equal to 40%
The aqueous solution, the aqueous solution of described high levels of organic solvents is the water-soluble of the organic solvent that concentration of volume percent is more than 40%
Liquid.
Dry Longstamen Onion Bulb 1kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 2h, 1.5h, 1h, and merging is carried
Liquid is taken, is filtered, concentration is crossed the absorption of D4020 large pore resin absorption columns, is washed with deionized water to colourless, with the 15% of 6 times of column volumes
Ethanol solution elution, lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagents
(50ml acetic acid dissolves 0.5ml anisaldehydes, plus sulfuric acid 1ml) and E reagents (1% paradime thylaminobenzaldehyde ethanol solution：Dense salt
Acid (4：1) check, steroid saponin spot as a result do not occur, illustrate that 15% ethanol solution can not be by furostanol saponin and spiral shell steroid soap
Glycosides is eluted (to furan steroid, spiral shell steroid all displaing yellows, E reagents only show pink colour to A reagents to furan steroid)；Then with 17% ethanol solution
Elution, puts lamellae, with chloroform-methanol-water (7 after eluent is concentrated:4:0.7) system is deployed, and uses A reagent colour developments, silica gel
There are several yellow spottings in plate, uses E reagent colour developments, and several pink colour spots, and yellow spotting and pink colour spot occurs in silica gel plate
Point can be corresponded to completely, and illustrating 17% ethanol solution can elute furostanol saponin and can not elute down spirostanol saponin
Come.Again respectively with the 23% of 6 times of column volumes, 25%, 27%, 29%, 31%, 33%, 35%, 37%, 39%, 40% ethanol
Solution is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagent colour developments,
There are several yellow spottings in silica gel plate, uses E reagent colour developments, and several pink colour spots, and yellow spotting and powder occurs in silica gel plate
Color spot point can be corresponded to completely, illustrate 17%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%, 39%, 40%
Ethanol solution furostanol saponin can be eluted and spirostanol saponin can not be eluted.Again with 41%, 43%, 45% ethanol
Solution is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-methanol-water (10:4:0.5) system is deployed, and uses A reagent colour developments,
There are several yellow spottings in silica gel plate, uses E reagent colour developments, and pink colour spot occurs in silica gel plate, illustrates when concentration of alcohol is more than
Furostanol saponin and spirostanol saponin are eluted together when 41%.
Longstamen Onion Bulb 1kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively that 3h, 2h, 1h merge extract solution, mistake
Filter, concentration, the absorption of AB-8 large pore resin absorption columns is crossed, be washed with deionized water to colourless, 15% methanol with 6 times of column volumes is molten
Liquid is eluted, and lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, with A reagents (50ml vinegar
Acid dissolves 0.5ml anisaldehydes, plus sulfuric acid 1ml) and E reagents (1% paradime thylaminobenzaldehyde methanol solution：Concentrated hydrochloric acid (4：1)
Check, steroid saponin spot as a result do not occur, furostanol saponin and spirostanol saponin can not be eluted by illustrating 15% methanol solution
Get off (to furan steroid, spiral shell steroid all displaing yellows, E reagents only show pink colour to A reagents to furan steroid)；Then eluted with 17% methanol solution,
Lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagent colour developments, and silica gel plate occurs
Several yellow spottings, use E reagent colour developments, several pink colour spots occurs in silica gel plate, and yellow spotting and pink colour spot can
Completely corresponding, illustrating 17% methanol solution can elute furostanol saponin and can not elute spirostanol saponin.Divide again
Not with the 19% of 6 times of column volumes, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%, 39%, 40%
Methanol solution is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, aobvious with A reagents
There are several yellow spottings in color, silica gel plate, uses E reagent colour developments, and several pink colour spots occurs in silica gel plate, and yellow spotting and
Pink colour spot can be corresponded to completely, illustrate 17%, 19%, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%,
37%th, furostanol saponin can be eluted and can not elute spirostanol saponin by 39%, 40% methanol solution.Use again
41%th, 43%, 45% methanol solution is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-methanol-water (10:4:0.5) system
System expansion, uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, silica gel plate pink colour spot occurs, said
It is bright to elute furostanol saponin and spirostanol saponin together when methanol concentration is more than 41%.
Longstamen Onion Bulb 1kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively that 3h, 2h, 1h merge extract solution, mistake
Filter, concentration, the absorption of HP20 large pore resin absorption columns is crossed, be washed with deionized water to colourless, 15% acetone with 6 times of column volumes is molten
Liquid is eluted, and lamellae is put after eluent is concentrated, with chloroform-acetone-water (7:4:0.7) system is deployed, with A reagents (50ml vinegar
Acid dissolves 0.5ml anisaldehydes, plus sulfuric acid 1ml) and E reagents (1% paradime thylaminobenzaldehyde methanol solution：Concentrated hydrochloric acid (4：1)
Check, steroid saponin spot as a result do not occur, furostanol saponin and spirostanol saponin can not be eluted by illustrating 15% acetone soln
Get off (to furan steroid, spiral shell steroid all displaing yellows, E reagents only show pink colour to A reagents to furan steroid)；Then eluted with 17% acetone soln,
Lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagent colour developments, and silica gel plate occurs
Several yellow spottings, use E reagent colour developments, several pink colour spots occurs in silica gel plate, and yellow spotting and pink colour spot can
Completely corresponding, illustrating 17% acetone soln can elute furostanol saponin and can not elute spirostanol saponin.Divide again
Not with the 19% of 6 times of column volumes, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%, 39%, 40%
Acetone soln is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-acetone-water (7:4:0.7) system is deployed, aobvious with A reagents
There are several yellow spottings in color, silica gel plate, uses E reagent colour developments, and several pink colour spots occurs in silica gel plate, and yellow spotting and
Pink colour spot can be corresponded to completely, illustrate 17%, 19%, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%,
37%th, furostanol saponin can be eluted and can not elute spirostanol saponin by 39%, 40% acetone soln.Use again
41%th, 43%, 45% acetone soln is eluted, and silica gel plate is put after eluent is concentrated, with chloroform-methanol-water (10:4:0.5) system
System expansion, uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, silica gel plate pink colour spot occurs, said
It is bright to elute furostanol saponin and spirostanol saponin together when acetone concentration is more than 41%.
Longstamen Onion Bulb 1kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively that 3h, 2h, 1h merge extract solution, mistake
Filter, concentrate, crossing the absorption of HP20 large pore resin absorption columns, being washed with deionized water to colourless, with 15% isopropanol of 6 times of column volumes
Solution is eluted, and lamellae is put after eluent is concentrated, with chloroform-isopropanol-water (7:4:0.7) system is deployed, and uses A reagents
(50ml acetic acid dissolves 0.5ml anisaldehydes, plus sulfuric acid 1ml) and E reagents (1% paradime thylaminobenzaldehyde methanol solution：Dense salt
Acid (4：1) check, steroid saponin spot as a result do not occur, illustrate that 15% aqueous isopropanol can not be by furostanol saponin and spiral shell steroid
Saponin(e is eluted (to furan steroid, spiral shell steroid all displaing yellows, E reagents only show pink colour to A reagents to furan steroid)；Then with 17% isopropanol
Solution is eluted, and lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagent colour developments,
There are several yellow spottings in silica gel plate, uses E reagent colour developments, and several pink colour spots, and yellow spotting and powder occurs in silica gel plate
Color spot point can be corresponded to completely, illustrated 17% aqueous isopropanol and can be eluted furostanol saponin and can not wash spirostanol saponin
Take off.Again respectively with the 19% of 6 times of column volumes, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%,
39%th, 40% aqueous isopropanol elution, puts silica gel plate, with chloroform-isopropanol-water (7 after eluent is concentrated:4:0.7) system
System expansion, uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, several pink colours occurs in silica gel plate
Spot, and yellow spotting and pink colour spot can correspond to completely, illustrate 17%, 19%, 21%, 23%, 25%, 27%, 29%,
31%th, furostanol saponin can be eluted and can not be by spirostanol saponin by 33%, 35%, 37%, 39%, 40% aqueous isopropanol
Elute.Again with 41%, 43%, 45% aqueous isopropanol elute, put silica gel plate after eluent is concentrated, with chloroform-methanol-
Water (10:4:0.5) system is deployed, and uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, silica gel plate
There is pink colour spot, illustrate to elute furostanol saponin and spirostanol saponin together when isopropyl alcohol concentration is more than 41%.
Longstamen Onion Bulb 1kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively that 3h, 2h, 1h merge extract solution, mistake
Filter, concentrate, crossing the absorption of HP20 large pore resin absorption columns, being washed with deionized water to colourless, with 15% normal propyl alcohol of 6 times of column volumes
Solution is eluted, and lamellae is put after eluent is concentrated, with chloroform-normal propyl alcohol-water (7:4:0.7) system is deployed, and uses A reagents
(50ml acetic acid dissolves 0.5ml anisaldehydes, plus sulfuric acid 1ml) and E reagents (1% paradime thylaminobenzaldehyde methanol solution：Dense salt
Acid (4：1) check, steroid saponin spot as a result do not occur, illustrate that 15% normal propyl alcohol solution can not be by furostanol saponin and spiral shell steroid
Saponin(e is eluted (to furan steroid, spiral shell steroid all displaing yellows, E reagents only show pink colour to A reagents to furan steroid)；Then with 17% normal propyl alcohol
Solution is eluted, and lamellae is put after eluent is concentrated, with chloroform-methanol-water (7:4:0.7) system is deployed, and uses A reagent colour developments,
There are several yellow spottings in silica gel plate, uses E reagent colour developments, and several pink colour spots, and yellow spotting and powder occurs in silica gel plate
Color spot point can be corresponded to completely, illustrated 17% normal propyl alcohol solution and can be eluted furostanol saponin and can not wash spirostanol saponin
Take off.Again respectively with the 19% of 6 times of column volumes, 21%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%,
39%th, 40% normal propyl alcohol solution elution, puts silica gel plate, with chloroform-normal propyl alcohol-water (7 after eluent is concentrated:4:0.7) system
System expansion, uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, several pink colours occurs in silica gel plate
Spot, and yellow spotting and pink colour spot can correspond to completely, illustrate 17%, 19%, 21%, 23%, 25%, 27%, 29%,
31%th, furostanol saponin can be eluted and can not be by spirostanol saponin by 33%, 35%, 37%, 39%, 40% normal propyl alcohol solution
Elute.Again with 41%, 43%, 45% normal propyl alcohol solution elute, put silica gel plate after eluent is concentrated, with chloroform-methanol-
Water (10:4:0.5) system is deployed, and uses A reagent colour developments, several yellow spottings occurs in silica gel plate, uses E reagent colour developments, silica gel plate
There is pink colour spot, illustrate to elute furostanol saponin and spirostanol saponin together when normal propyl alcohol concentration is more than 41%.
First used to obtain after the total furostanol saponin of the higher Longstamen Onion Bulb of purity adsorbs longstamen onion bulb extract with macroporous absorbent resin
The aqueous solution elution of organic solvent of the concentration of volume percent less than 15% removes impurity, is then more than with concentration of volume percent
The 15% total furostanol saponin of Longstamen Onion Bulb being mainly made up of to the aqueous solution elution acquisition of the organic solvent less than 40% furostanol saponin, is treated
The aqueous solution elution of organic solvent after furostanol saponin elution completely with concentration of volume percent more than 40% obtains main by spiral shell
The total spirostanol saponin of Longstamen Onion Bulb of steroid saponin(e composition.
Can also be by longstamen onion bulb extract macroporous absorbent resin for the purposes of obtaining the higher total furostanol saponin of Longstamen Onion Bulb of purity
The buck for being first 9-13 with pH value before the aqueous solution elution of organic solvent after absorption with concentration of volume percent less than 15%
Solution is eluted, and is washed to neutrality, and then the aqueous solution of the organic solvent with concentration of volume percent less than 15% is eluted, subsequently
With concentration of volume percent be more than 15% to the organic solvent less than 40% the aqueous solution elution obtain purity it is higher it is main by
The total furostanol saponin of Longstamen Onion Bulb of furostanol saponin composition, the aqueous solution for being finally more than 40% organic solvent with concentration of volume percent is washed
It is de- to obtain the main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin.
Alkali described herein can utilize alkali metal or the hydroxide of alkaline-earth metal, preferably sodium hydroxide or hydrogen-oxygen
Change potassium or calcium hydroxide, the pH value of aqueous alkali is 9-13.The Longstamen Onion Bulb group saponine that above-mentioned preparation method is obtained can be used for system
Standby pharmaceutical composition, health food and prepare monomer saponin.
The beneficial effects of the present invention are furostanol saponin and spirostanol saponin are separated with macroporous absorbent resin and ethanol,
Simple with method, operation is easy, good separating effect, and solvent is recycled, the advantages of not causing environmental pollution.
Embodiment
Embodiment 1
Dry Longstamen Onion Bulb 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 3h, 2h, 1h, merges and extracts
Liquid, is filtered, concentration, crosses the absorption of D101 large pore resin absorption columns, with 35% ethanol solution that furostanol saponin elution is complete, then is used
85% ethanol solution elutes spirostanol saponin completely, and solvent is recovered under reduced pressure, and dries, and obtains total 24.2 grams of the furostanol saponin of Longstamen Onion Bulb, Chinese onion
27.0 grams of the total spirostanol saponins of Bai.Bioactivity research result shows that the above-mentioned total furostanol saponin of Longstamen Onion Bulb and the total spirostanol saponin of Longstamen Onion Bulb are equal
With platelet aggregation inhibitory activity, and the activity spirostanol saponin more total than Longstamen Onion Bulb of the total furostanol saponin of Longstamen Onion Bulb is strong.
Embodiment 2
Dry Longstamen Onion Bulb aerial part 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 3h, 2h, 1h,
Merge extract solution, filter, concentration crosses the absorption of D101 large pore resin absorption columns, eluted furostanol saponin with 35% ethanol solution
Completely, then with 85% ethanol solution spirostanol saponin is eluted completely, solvent is recovered under reduced pressure, dried, obtain the total furostanol saponin of Longstamen Onion Bulb
22.3 grams, 24.5 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Embodiment 3
Dry Longstamen Onion Bulb herb 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively that 3h, 2h, 1h merge
Extract solution, is filtered, concentration, is crossed the absorption of AB-8 large pore resin absorption columns, is washed with deionized water to colourless, with 35% ethanol solution
Furostanol saponin elution is complete, then eluted spirostanol saponin completely with 85% ethanol solution, solvent is recovered under reduced pressure, dries, obtains
23.2 grams of the total furostanol saponin of Longstamen Onion Bulb, 26.6 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Embodiment 4
Take fresh Longstamen Onion Bulb aerial part 10kg to be homogenized, with 10 times of water boiling and extractions 3 times, decocting time be respectively 3h, 2h,
1h, merges extract solution, filters, and ethanol is reclaimed in concentration, the absorption of AB-8 large pore resin absorption columns is crossed after being diluted with water, with 35%
Ethanol solution elutes furostanol saponin completely, then is eluted spirostanol saponin completely with 85% ethanol solution, and solvent is recovered under reduced pressure, and does
It is dry, obtain total 24.2 grams of the furostanol saponin of Longstamen Onion Bulb, 27.0 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Embodiment 5
Take fresh Longstamen Onion Bulb 12kg to smash to pieces, extracted 3 times with 10 times of 85% alcohol reflux, extraction time is respectively 3h, 2h, 1h,
Merge extract solution, ethanol is reclaimed in filtering, the absorption of D101 large pore resin absorption columns is crossed after being diluted with water, with 35% ethanol solution
Furostanol saponin elution is complete, then eluted spirostanol saponin completely with 85% ethanol solution, solvent is recovered under reduced pressure, dries, obtains
30.2 grams of the total furostanol saponin of Longstamen Onion Bulb, 34.0 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Embodiment 6
Dry Longstamen Onion Bulb 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 3h, 2h, 1h, merges and extracts
Liquid, is filtered, concentration, crosses the absorption of D101 large pore resin absorption columns, is first eluted, discarded with 10% methanol solution of 6 times of column volumes,
Then furostanol saponin is eluted completely with 30% methanol solution, then eluted spirostanol saponin completely with 85% methanol solution, subtracted
Recycling design is pressed, is dried, 21.3 grams of the total furostanol saponin of Longstamen Onion Bulb of higher purity, 22.6 grams of the total spirostanol saponin of Longstamen Onion Bulb is obtained.
Embodiment 7
Dry Longstamen Onion Bulb 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 3h, 2h, 1h, merges and extracts
Liquid, is filtered, concentration, crosses the absorption of D102 large pore resin absorption columns, first with pH value for 10 sodium hydrate aqueous solution be eluted to it is colourless,
Discard；It is washed with water to neutrality, then is eluted with 10% ethanol solution of 6 times of column volumes, is discarded；Then with 30% ethanol solution
Furostanol saponin elution is complete, then eluted spirostanol saponin completely with 80% ethanol solution, solvent is recovered under reduced pressure, dries, obtains
19.8 grams of the total furostanol saponin of Longstamen Onion Bulb of higher purity, 21.4 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Embodiment 8
Dry Longstamen Onion Bulb aerial part 3kg is taken to crush, with 10 times of water boiling and extractions 3 times, decocting time is respectively 3h, 2h, 1h,
Merge extract solution, filter, the absorption of HP20 large pore resin absorption columns is crossed in concentration, with pH value for 13 sodium hydroxide be washed to it is colourless,
Neutrality is washed to again, is eluted, discarded with 12% acetone soln of 6 times of column volumes；Then with 35% acetone soln by furan steroid
Saponin(e elution is complete, then is eluted spirostanol saponin completely with 75% acetone soln, and solvent is recovered under reduced pressure, dries, Longstamen Onion Bulb is obtained total
24.3 grams of furostanol saponin, 26.8 grams of the total spirostanol saponin of Longstamen Onion Bulb.
Claims (10)
1. a kind of preparation method of Longstamen Onion Bulb group saponine, it is characterised in that used after longstamen onion bulb extract is adsorbed with macroporous absorbent resin
The aqueous solution elution of low-concentration organic solvent obtains the main total furostanol saponin of Longstamen Onion Bulb being made up of furostanol saponin completely, then with height
The aqueous solution elution of concentration organic solvent obtains the main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin.
2. the preparation method described in claim 1, it is characterised in that described macroporous absorbent resin be selected from AB-8, D4020,
D101, D102, D103,860021, HP20 one kind or their two or more hybrid resin.
3. the preparation method described in claim 1, it is characterised in that described organic solvent is selected from ethanol, methanol, acetone, positive third
Alcohol, isopropanol or their two or more mixed solvent.
4. the preparation method described in claim 1, it is characterised in that the aqueous solution of described low-concentration organic solvent is volume hundred
The aqueous solution for dividing specific concentration to be less than or equal to 40%.
5. the preparation method described in claim 1, it is characterised in that the aqueous solution of described high levels of organic solvents is volume hundred
The aqueous solution for dividing specific concentration to be more than 40%.
6. the preparation method described in claim 1, it is characterised in that first used after longstamen onion bulb extract is adsorbed with macroporous absorbent resin
Concentration of volume percent is obtained to the aqueous solution elution of the organic solvent less than 40% more than 15% and is mainly made up of furostanol saponin
The total furostanol saponin of Longstamen Onion Bulb, be then more than with concentration of volume percent 40% organic solvent aqueous solution elution obtain it is main by
The total spirostanol saponin of Longstamen Onion Bulb of spirostanol saponin composition.
7. the preparation method described in claim 1, it is characterised in that first used after longstamen onion bulb extract is adsorbed with macroporous absorbent resin
Concentration of volume percent is less than the aqueous solution elution of 15% organic solvent, is then more than 15% to small with concentration of volume percent
The higher total furostanol saponin of Longstamen Onion Bulb of the main purity being made up of furostanol saponin is obtained in the aqueous solution elution of 40% organic solvent,
Then the aqueous solution elution for being more than 40% organic solvent with concentration of volume percent obtains the main Chinese onion being made up of spirostanol saponin
The total spirostanol saponins of Bai.
8. the preparation method described in claim 1, it is characterised in that it is characterized in that by longstamen onion bulb extract macroporous absorbent resin
The aqueous alkali for being first 9-13 with pH value after absorption is eluted, then is more than 15% to organic less than 40% with concentration of volume percent
The aqueous solution elution of solvent obtains the higher total furostanol saponin of Longstamen Onion Bulb of the main purity being made up of furostanol saponin, finally with volume hundred
The aqueous solution elution for dividing specific concentration to be more than 40% organic solvent obtains the main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin.
9. the preparation method described in claim 1, it is characterised in that it is characterized in that by longstamen onion bulb extract macroporous absorbent resin
The aqueous alkali for being first 9-13 with pH value after absorption is eluted, and the water of 15% organic solvent is then less than with concentration of volume percent
Solution is eluted, then with concentration of volume percent be more than 15% to the organic solvent less than 40% aqueous solution elution obtain it is main by
The higher total furostanol saponin of Longstamen Onion Bulb of purity of furostanol saponin composition, be finally more than with concentration of volume percent 40% organic solvent
Aqueous solution elution obtain the main total spirostanol saponin of Longstamen Onion Bulb being made up of spirostanol saponin.
10. the preparation method described in claim 8 or 9, it is characterised in that described alkali is the hydrogen-oxygen of alkali metal or alkaline-earth metal
Compound.
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| CN109431944A (en) * | 2018-12-26 | 2019-03-08 | 上海应用技术大学 | A kind of longstamen onion bulb extract and its application in anti-oxidation efficacy cosmetics |
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| CN112500448A (en) * | 2020-11-19 | 2021-03-16 | 西安集佰侬生物科技有限公司 | Method for extracting laxogenin from plant of Allium of Liliaceae |
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