CN109867650A - A kind of preparation method for extracting allelochemical Salcolin A from highland barley stalk - Google Patents
A kind of preparation method for extracting allelochemical Salcolin A from highland barley stalk Download PDFInfo
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Abstract
The invention discloses a kind of from highland barley stalk extracts the preparation method of allelochemical Salcolin A.Including including material disintegrating, pure water ultrasonic wave extraction, enrichment desaccharification, HPLC preparation, recrystallization.Using pure water ultrasonic extraction, murder by poisoning and pollution caused by organic solvent extracts are avoided；Enrichment desaccharification technique is first eluted with water using D101 macroreticular resin on concentrate is extracted, and alcohol eluen processing is collected in again with methanol elution.The impurity such as sugared part macromolecular in extract can be effectively removed through this process, improve separative efficiency and reduce raw material investment.HPLC preparation can shorten very big disengaging time, and repeatability is strong, reduces the investment of manpower and material resources.The Salcolin A purity that preparation method provided by the invention obtains is and easy to operate up to 95% or more, can greatly save the usage amount of toxic solvent, save manpower, save the time.
Description
Technical field
The invention belongs to allelopathy active material technical fields, and in particular to one kind extracts allelopathic object from highland barley stalk
The preparation method of matter Salcolin A.
Background technique
Farmland weed is one of the major issue in agricultural production, fights for the resources such as light, water, fertilizer with crop and becomes shadow
The important factor for ringing crop yield and quality, brings about great losses to agricultural production.For a long time mainly using chemical weed control
Means control the harm of weeds, not only pollute environment using herbicide, but also weeds are also easy to produce drug resistance, the food peace of initiation
Entirely, the adverse effect of anti-(resistance to) pharmacological property of public health, natural environment and weeds etc. has increasingly caused the concern of people.Plant
Allelopathy (Allelopathy) refer to a kind of plant to the specific chemical substance of Environment release (allelochemical,
Allelochemical the ecological phenomenon of the growth and development of the other plants of surrounding) is influenced.Made using the allelopathic between plant
With can by discharged into environment allelochemical and with weed competition living environment, and then sprouting and growth to weed seed
Inhibiting effect is generated, the environmental problem of pesticide residue etc. will not be brought using allelopathy control weeds.In order to protect people
The sustainable development of the environment that class is survived and agricultural, developing and using for chemical herbicide will be strictly by environment and ecological system
About.New herbicide is developed using natural products, has shown powerful vitality, natural products herbicide is gradually by people
Attention, plant allelochemicals be find new bio source herbicide lead compound important channel.
Highland barley (hullessbarley) is the special crop of Qinghai-Tibet Platean, is that a kind of Cereal of grass family Hordeum is made
Object, because the separation of the glume shell inside and outside and the bare grain for it, therefore also known as naked barley.Applicant's early period by a large amount of research work at home
Highland barley is reported for the first time outside with allelopathy, the main allelochemical of highland barley, form of expression of highland barley allelopathy etc., simultaneously
Confirm that Salcolin A (tricin 4'-O- (threo- β-guaiacylglyceryl) ether) is main highland barley suppression grassization
Feel substance, is to receptor wild avena sativa root long allelopathic index when being 100 μ g/mL for examination concentration by biological activity test
0.63.In addition Salcolin A has inhibiting effect to Growth of Microcystis aeruginosa, and 503nhibiting concentration (5d) is respectively 6.02 × 10- 5mol l-1.Salcolin A structure novel, isomers be more, diverse biological activities, has in scientific research and agriculture application field
Bright prospects.But chemical structure is complicated, chiral carbon is more, it is difficult to which chemical synthesis, its source is still relied on from plant at present
Middle separation obtains.
It is considerably less now concerning the method for extraction and purification of Salcolin A, using highland barley as the method for extraction and purification of raw material sources
Basic blank.Method is also only that laboratory micro extracts separation at present, and no Standard Operating Procedure, amount to obtain is mostly at more than ten milligrams
And it is unsecured.Specific method is: material disintegrating, and --- 95% industrial methanol refluxing extraction --- extracting solution concentration --- is organic molten
Agent extracts (or organic solvent refluxing extraction), and --- silica gel column chromatography (normal phase column and reversed-phase column) --- HPLC preparation --- is tied again
It is brilliant.In organic solvent extraction (or organic solvent refluxing extraction) technique, usually using petroleum ether, methylene chloride, chloroform, acetic acid
The toxic organic solvents such as ethyl ester, methanol are extracted or are extracted, and in silica gel column chromatography technique, the most commonly used is use wet column method
It is separated, i.e., fills chromatographic column with the silica white after organic solvent impregnates, sample is added to filling chromatographic column top, then use
Different organic solvents are eluted, and fraction collection eluent is chromatographed repeatedly, finally prepared with HPLC, and recrystallization is until obtain
Obtain sterling.Entire technique is cumbersome, time-consuming, and the time that preparation personnel contact with toxic solvent is long, serious to damage preparation personnel's
Health generates a large amount of poisonous and hazardous organic solvents, serious to environmental hazard.
D101 macroporous absorbent resin is a kind of polymer absorbant with the synthesis of porous spongy structure artificial, by tree
Van der Waals force between rouge skeleton and the molecule being adsorbed, by the huge specific surface area of resin carry out physical absorption reach from
The purpose of the water-soluble poor organic substance of separation and Extraction in aqueous solution.D101 resin is a kind of non-polar adsorbent, general to use
In Chinese herbal medicine the extraction of saponins with separate, have many advantages, such as easy to operate, cost is relatively low, resin can Reusability.
Summary of the invention
The purpose of the present invention is to provide a kind of extraction purifications from highland barley stalk more easy, efficient, environmentally friendlyly
The relatively large number of preparation method of Salcolin A (tricin 4'-O- (threo- β-guaiacylglyceryl) ether),
Long, the serious damage system with the low efficiency, time-consuming, expense material, preparation personnel and the toxic organic solvents time of contact that solve current method
The problems such as health and environmental pollution of standby personnel.
The present invention is realized especially by following technical scheme:
A kind of preparation method for extracting allelochemical Salcolin A from highland barley stalk, comprising the following steps:
1) material disintegrating is ground into powder after fresh highland barley stalk is removed moisture removal；
2) pure water ultrasonic wave extraction takes highland barley stalk powder to dissolve in pure water, through ultrasound filtration up to extracting solution；
3) enrichment desaccharification, extracting solution is adsorbed through D101 macroporous adsorption resin chromatography, is successively eluted using water and methanol, is received
Collect meoh eluate, is concentrated under reduced pressure into paste, obtains paste extract；
4) prepared by HPLC
Gradient elution, paste extract water and a small amount of methanol sufficiently dissolve loading, collect eluent, pass through thin-layer chromatography
Chromatography detection, the component for the appearance point that mutually exists together with Salcolin A standard items Rf value, both slightly propose component；
Isocratic elution, by runic component, loading, chromatography show 4 main chromatographic peaks altogether after completely dissolution, and retention time exists
The component of the 4th chromatographic peak, the Rf surveyed in silica gel thin-layer chromatography with Salcolin A standard items are collected between 18-24min
Value is compared, and both obtains the higher component of Salcolin A content；
Polishing purification, by the higher component of Salcolin A content loading after completely dissolution, with mobile phase: A: B=70: 30
(v/v) it elutes, after retention time is greater than 20min, collects the component of maximum chromatographic peak, obtain the elution of high-purity Salcolin A
Liquid；
5) it recrystallizes, thin-layer chromatography detection and the eluent that Salcolin A standard items Rf value mutually exists together is concentrated under reduced pressure
Afterwards, it is sufficiently dissolved with methanol, filtrate is statically placed in 4 DEG C of refrigerators, and filtering out crystallization is Salcolin A sterling.
Further, the mass volume ratio of highland barley stalk powder and pure water is 1:2-5 in step (2).
Further, extracting solution and D101 macroporous absorbent resin volume ratio are 2-5:1 in step (3).
Further, condition of gradient elution described in step (4) are as follows: A phase: H2O (0.1%TFA)；B phase: acetonitrile；Flow velocity
25ml/min, chromatographic column selection C-18 prepare column (21.2mm × 150mm × 5um)；UV detector 254nm, Mobile phase B are initial
Ratio is that 10%, 0-10min Mobile phase B ratio rises to 30%, 10-10.2min Mobile phase B ratio and rises to 90%, is kept
Mobile phase B ratio is down to 10% in 3.3min, subsequent 2min, restores initial proportion, keeps baseline stability.
Further, isocratic condition described in step (4) are as follows: A phase: H2O contains 0.1%TFA；B phase: acetonitrile；Chromatography
Column selection C-18 prepares column (21.2mm × 150mm × 5um)；UV detector 254nm, with mobile phase A: B=50: 50 (v/v),
Flow velocity 25mL/min, monitoring time 30-35min.
Further, polishing purification described in step (4) takes off condition are as follows: A phase: H2O contains 0.1%TFA；B phase: acetonitrile；Color
Spectrum column selection C-18 prepares column (21.2mm × 150mm × 5um)；UV detector 254nm, with mobile phase A: B=70: 30 (v/
V) it elutes.
The invention has the benefit that
(1) firstly, according to target substance Salcolin A (tricin 4'-O- (threo- β-guaiacylglyceryl)
Ether the characteristics of) belonging to allelochemical, being obtained by flooding, this method use pure water ultrasonic wave extraction in extraction
Method, greatly avoid time-consuming, consuming funds, process caused by being extracted using organic solvent be cumbersome, preparation personnel with it is toxic molten
The problems such as agent contact for a long time, pollution environment.
(2) secondly, using extracting solution and D101 macroporous absorbent resin volume ratio for 2- in extract desaccharification process of enriching
5:1 adsorbs extracting solution through D101 macroporous adsorption resin chromatography, first uses the water elution of 2-4 column volume, then with 3-5 cylinder
Long-pending methanol elution, collects meoh eluate, is concentrated under reduced pressure into paste, obtains paste extract.It can effectively remove through this process
Remove the impurity such as sugared part in extract, Salcolin A (tricin4'-O- (threo- β-in extract-enriched
Guaiacylglyceryl) ether) etc. water-soluble poor organic principle, improve in column chromatography procedure the bearing capacity of silica gel and
Separative efficiency obtains target component Salcolin A (tricin 4'-O- (threo- β-guaiacylglyceryl) ether)
To effective enrichment, the use using toxic organic solvents in organic solvent extraction or organic solvent Effect of Alcohol Extracting Procedureto Total is avoided,
Greatly shorten the time of process flow.
(3) again, this method carries out the separation of target compound by preparation or semi-preparative liquid chromatography, with Salcolin
A (tricin 4'-O- (threo- β-guaiacylglyceryl) ether) is guiding, and thin-layer chromatography tracing detection, comparison is now
There is method to increase mechanization intelligent operation, repeatability is strong, process flow can normalizing operation, reduce making for organic solvent
With, significantly improve separative efficiency.
It (4), can be from highland barley young crops or highland barley stalk using the method for the present invention finally, the present inventor is proved by test of many times
Middle extraction purification to high-purity Salcolin A (tricin4'-O- (threo- β-guaiacylglyceryl) ether), it is pure
Degree (being detected using HPLC) can be used for various bioactivity research up to 95% or more, the simple, preparation process with preparation method
Toxic organic solvents usage amount is few, preparation personnel and toxic solvent time of contact are short, repeatable strong, standard process flow is grasped
Make, protect the advantages that environment.
Detailed description of the invention
Fig. 1 is slightly to mention component isocratic elution chromatogram in HPLC preparation.
Specific embodiment
Below in conjunction with specific embodiment of the present invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
A kind of specific preparation method that allelochemical Salcolin A is extracted from highland barley stalk provided by the invention, leads to
Cross following steps completion:
One, material disintegrating: fresh highland barley stalk is taken to be dried or set in drying box after 45 DEG C of -55 DEG C of drying, with cutting section
1-3cm or plant pulverizer are ground into powder；
Two, pure water ultrasonic wave extraction: take a certain amount of powder in reflux flask, by sample and Extraction solvent quality volume
Than pure water is added for 1:2-5, shakes up, sample is all compressed under liquid level, is placed in ultrasonic cleaner, every 2h ultrasound
It is filtered after 15min, 1-3d up to extracting solution；
Three, enrichment desaccharification: being 2-5:1 by extracting solution and D101 macroporous absorbent resin volume ratio, and extracting solution is big through D101
Macroporous adsorbent resin chromatographic adsorption is first used the water elution of 2-4 column volume, then is eluted with the methanol of 3-5 column volume, and methanol is collected
Eluent is concentrated under reduced pressure into paste, obtains paste extract；
Four, prepared by HPLC: point three steps preparation
(1) gradient elution, paste extract water and a small amount of methanol sufficiently dissolve loading.It will preparation liquid phase mobile phase selection
A phase: H2O (0.1%TFA)；B phase: acetonitrile；Flow velocity 25ml/min (according to preparation column capacity), chromatographic column selection C-18 prepare column
(21.2mm×150mm×5um)；UV detector 254nm, Mobile phase B initial proportion are 10%, 0-10min Mobile phase B ratio
It rises to 30%, 10-10.2min Mobile phase B ratio and rises to 90%, keep 3.3min, Mobile phase B ratio is down in subsequent 2min
10%, restore initial proportion, keeps baseline stability.Eluent 25-35mL/ parts is collected, is detected by thin-layer chromatography chromatography, according to
Every part of eluent is carried out thin-layer chromatography detection, merged by the Rf value that Salcolin A standard items are surveyed in silica gel thin-layer chromatography
Mutually exist together the component of appearance point with Salcolin A standard items Rf value, both slightly propose component.
(2) preparation liquid phase mobile phase is selected A phase: H by runic component loading after completely dissolution by isocratic elution2O
(0.1%TFA)；B phase: acetonitrile；Chromatographic column selection C-18 prepares column (21.2mm × 150mm × 5um)；UV detector 254nm,
With mobile phase: A: B=50: 50 (v/v), flow velocity 25mL/min, monitoring time 30-35min, chromatography show 4 main chromatographies altogether
Peak, retention time collect the component of the 4th chromatographic peak between 18-24min, and the detection of thin-layer chromatography chromatography is marked with Salcolin A
The Rf value that quasi- product are surveyed in silica gel thin-layer chromatography is compared, and both obtains the higher component of Salcolin A content.
(3) polishing purification, by the higher component of Salcolin A content loading after completely dissolution, instrument condition with (two),
With mobile phase: A: B=70: 30 (v/v) elution is collected the component of maximum chromatographic peak, can be obtained after retention time is greater than 20min
Obtain the eluent of high-purity Salcolin A.
Five, it recrystallizes: thin-layer chromatography detection is only mutually existed together the merging of appearance point with Salcolin A standard items Rf value
It after eluent is concentrated under reduced pressure, is sufficiently dissolved, is filtered, filtrate is statically placed in 4 DEG C of refrigerators, after precipitation to be crystallized, filters out knot with methanol
Crystalline substance is Salcolin A (tricin4'-O- (threo- β-guaiacylglyceryl) ether) sterling.
Wherein, the highland barley in step (1) can be any for green (blueness) seedling of highland barley or highland barley fresh straw.
If step (4) cannot obtain the eluent of high-purity Salcolin A, can carried out once with (four) (3) method
Polishing purification.
Embodiment 1
Water-removing of learning from else's experience dries the fresh highland barley stalk 5Kg after 2d, cuts section 3cm or so and is respectively placed in 2L wide-mouth bottle, is added
500mL distilled water suppresses stalk in blade face hereinafter, seal with sealed membrane, and it is several to reserve ventilation hole, is placed in ultrasonic cleaning
Every 2h ultrasound 15min in device, ultrasound 4 times altogether, double-layer filter paper filtered off with suction is after 3d up to extracting solution, every bottle of about 380-400mL.
400mL extracting solution is taken to cross the chromatographic column (column diameter 7cm, long 100cm) equipped with 1500g D101 macroreticular resin, loading flow velocity every time
About 10mL/min first with the water elution of 2 column volumes, then is eluted with the methanol of 4 column volumes, is collected meoh eluate, close
And 3 eluents, 45 DEG C are concentrated under reduced pressure into paste, amount to obtain paste 145g.Liquid chromatogram Shimadzu LC-20AT, chromatographic column:
Phenomenex LUNA C-18 (21.2mm × 150mm × 5um), flow velocity: 25ml/min, mobile phase select A phase: H2O
(0.1%TFA), B phase: acetonitrile；UV detector 254nm, Mobile phase B initial proportion are 10%, 0-10min Mobile phase B ratio
It rises to 30%, 10-10.2min Mobile phase B ratio and rises to 90%, keep 3.3min, Mobile phase B ratio is down in subsequent 2min
10%, restore initial proportion, keeps baseline stability (Fig. 1).Eluent 25mL/ parts is collected, collects merge 12 components altogether, press
1-12 numbers, are detected, the R surveyed in silica gel thin-layer chromatography according to SalcolinA standard items by thin-layer chromatography chromatographyfValue,
Every part of eluent is subjected to thin-layer chromatography detection, is merged and SalcolinA standard items RfValue mutually exists together the component of appearance point, and No. 7
Group, which is divided into, slightly proposes component, and revolving to medicinal extract obtains 7.3g.It, will preparation liquid phase mobile phase selection by runic component loading after completely dissolution
A phase: H2O (0.1%TFA)；B phase: acetonitrile；Chromatographic column selection C-18 prepares column (21.2mm × 150mm × 5um)；Ultraviolet detection
Device 254nm, with mobile phase: A: B=50: 50 (v/v), flow velocity 25mL/min, monitoring time 35min, totally 4 main chromatographic peaks,
Collect the component of 4th chromatographic peak of the retention time between 18.1-18.6min, the detection of thin-layer chromatography chromatography and SalcolinA
The R that standard items are surveyed in silica gel thin-layer chromatographyfValue is compared, and both obtains the higher component of SalcolinA content, revolving to leaching
Cream 138mg.Polishing purification, by the higher component of SalcolinA content loading after completely dissolution, instrument condition is constant, with flowing
Phase: A: B=70: 30 (v/v) elution collects the component of retention time 21.5-21.9min maximum chromatographic peak, can get high-purity
The eluent of SalcolinA.Thin-layer chromatography detection is only washed mutually existing together with SalcolinA standard items Rf value merging for appearance point
It after de- liquid is concentrated under reduced pressure, is sufficiently dissolved, is filtered, filtrate is statically placed in 4 DEG C of refrigerators, after precipitation to be crystallized, filters out crystallization with methanol
As Salcolin A (tricin4'-O- (threo- β-guaiacylglyceryl) ether) sterling weighs 108.7mg, liquid
Phase chromatography detects purity 96.57%.
Salcolin A (tricin 4'-O- (threo- β-guaiacylglyceryl) is extracted from highland barley stalk
Ether) structural formula of sterling compound is as follows:
Embodiment 2
Take fresh highland barley stalk 5Kg, set in drying box through 45 DEG C -55 DEG C drying after, be ground into powder with plant pulverizer,
Weigh 3.2kg.It is divided into 10 parts to be placed in 1000mL triangular flask, every bottle of addition 600mL distilled water, sufficiently be impregnated, with
Sealed membrane sealing, it is several to reserve ventilation hole, is placed in ultrasonic cleaner every 2h ultrasound 15min, ultrasound 4 times altogether, after 3d
Double-layer filter paper filtered off with suction is up to extracting solution, every bottle of about 400mL.400mL extracting solution is taken to cross equipped with 1500g D101 macropore every time
The chromatographic column (column diameter 7cm, long 100cm) of resin, loading flow velocity is about 10mL/min, first with the water elution of 2 column volumes, then
With the methanol elution of 4 column volumes, meoh eluate is collected, merges 3 eluents, 45 DEG C are concentrated under reduced pressure into paste, amount to
Paste 181g.Liquid chromatogram Chinese nation NS4000, chromatographic column: Phenomenex LUNA C-18 (21.2mm × 150mm ×
5um), flow velocity: 25ml/min, mobile phase select A phase: H2O (0.1%TFA), B phase: acetonitrile；UV detector 254nm, flowing
Phase B initial proportion rises to 30%, 10-10.2min Mobile phase B ratio for 10%, 0-10min Mobile phase B ratio and rises to 90%, protects
3.3min is held, Mobile phase B ratio is down to 10% in subsequent 2min, restores initial proportion, keeps baseline stability.Collect eluent
It 25mL/ parts, collects merge 12 components altogether, by 1-12 numbers, detected by thin-layer chromatography chromatography, according to SalcolinA standard
The R that product are surveyed in silica gel thin-layer chromatographyfEvery part of eluent is carried out thin-layer chromatography detection, merged and SalcolinA standard by value
Product RfValue mutually exists together the component of appearance point, and No. 7 groups, which are divided into, slightly proposes component, and revolving to medicinal extract obtains 8.9g.Runic component is sufficiently molten
Preparation liquid phase mobile phase is selected A phase: H by loading after solution2O (0.1%TFA)；B phase: acetonitrile；Chromatographic column selection C-18 prepares column
(21.2mm×150mm×5um)；UV detector 254nm, with mobile phase: A: B=50: 50 (v/v), flow velocity 25mL/min, prison
Time 40min is surveyed, totally 4 main chromatographic peaks, collects the group of 4th chromatographic peak of the retention time between 18.7-19.3min
Point, the R that the detection of thin-layer chromatography chromatography is surveyed in silica gel thin-layer chromatography with SalcolinA standard itemsfValue is compared, both
The higher component of SalcolinA content, revolving to medicinal extract 118mg.Polishing purification fills the higher component of SalcolinA content
Divide loading after dissolving, instrument condition is constant, with mobile phase: retention time 22.5- is collected in A: B=70: 30 (v/v) elution
The component of 23.1min maximum chromatographic peak can get the eluent of high-purity SalcolinA.By thin-layer chromatography detection only with
SalcolinA standard items Rf value mutually exist together appearance point merging eluent be concentrated under reduced pressure after, sufficiently dissolved with methanol, filter, filter
Liquid is statically placed in 4 DEG C of refrigerators, and after precipitation to be crystallized, filtering out crystallization is Salcolin A (tricin4'-O- (threo- β-
Guaiacylglyceryl) ether) sterling, weigh 88.4mg, liquid chromatographic detection purity 97.05%.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understand without departing from the principles and spirit of the present invention can to these examples carry out it is a variety of variation, modification, replacement and
Modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of preparation method for extracting allelochemical Salcolin A from highland barley stalk, which is characterized in that including following step
It is rapid:
1) material disintegrating is ground into powder after fresh highland barley stalk is removed moisture removal；
2) pure water ultrasonic wave extraction takes highland barley stalk powder to dissolve in pure water, through ultrasound filtration up to extracting solution；
3) enrichment desaccharification, extracting solution is adsorbed through D101 macroporous adsorption resin chromatography, is successively eluted using water and methanol, and first is collected
Alcohol eluen is concentrated under reduced pressure into paste, obtains paste extract；
4) prepared by HPLC
Gradient elution, paste extract water and a small amount of methanol sufficiently dissolve loading, collect eluent, pass through thin-layer chromatography chromatography
Detection, the component for the appearance point that mutually exists together with Salcolin A standard items Rf value, both slightly propose component；
Isocratic elution, by runic component, loading, retention time collect component between 18-24min after completely dissolution, with
The Rf value that Salcolin A standard items are surveyed in silica gel thin-layer chromatography is compared, and both obtains higher group of Salcolin A content
Point；
Polishing purification, by the higher component of Salcolin A content loading after completely dissolution, with mobile phase: A: B=70: 30 (v/
V) it elutes, after retention time is greater than 20min, collects the component of maximum chromatographic peak, obtain the eluent of high-purity Salcolin A；
5) it recrystallizes, after thin-layer chromatography detection is concentrated under reduced pressure with the eluent that Salcolin A standard items Rf value mutually exists together, uses
Methanol sufficiently dissolves, and filtrate is statically placed in 4 DEG C of refrigerators, and filtering out crystallization is Salcolin A sterling.
2. a kind of preparation method that allelochemical Salcolin A is extracted from highland barley stalk according to claim 1,
It is characterized in that, the mass volume ratio of highland barley stalk powder and pure water is 1:2-5 in step (2).
3. a kind of preparation method that allelochemical Salcolin A is extracted from highland barley stalk according to claim 1,
It is characterized in that, extracting solution and D101 macroporous absorbent resin volume ratio are 2-5:1 in step (3).
4. a kind of preparation method that allelochemical Salcolin A is extracted from highland barley stalk according to claim 1,
It is characterized in that, condition of gradient elution described in step (4) are as follows: A phase: H2O contains 0.1%TFA；B phase: acetonitrile；Flow velocity 25ml/
Min, chromatographic column selection C-18 prepare column；UV detector 254nm, Mobile phase B initial proportion are 10%, 0-10min Mobile phase B
Ratio rises to 30%, 10-10.2min Mobile phase B ratio and rises to 90%, keeps 3.3min, Mobile phase B ratio drop in subsequent 2min
To 10%, restores initial proportion, keep baseline stability.
5. a kind of preparation method that allelochemical Salcolin A is extracted from highland barley stalk according to claim 1,
It is characterized in that, isocratic condition described in step (4) are as follows: A phase: H2O contains 0.1%TFA；B phase: acetonitrile；Chromatographic column selects C-
18 prepare column；UV detector 254nm, with mobile phase A: B=50: 50 (v/v), flow velocity 25mL/min, monitoring time 30-
35min。
6. a kind of preparation method that allelochemical Salcolin A is extracted from highland barley stalk according to claim 1,
It is characterized in that, polishing purification described in step (4) takes off condition are as follows: A phase: H2O contains 0.1%TFA；B phase: acetonitrile；Chromatographic column selection
C-18 prepares column；UV detector 254nm, with mobile phase A: B=70: 30 (v/v) elution.
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| YOUNG-SUK JUNG: "Anti-inflammatory effect of tricin 4′-O-(threo-β-guaiacylglyceryl) ether,anovel flavonolignan compound isolated from Njavara on in RAW264.7 cells and in ear mice edema", 《TOXICOLOGY AND APPLIED PHARMACOLOGY》 * |
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