CN102584923B - Method for extracting compounds from Chondrus ocelltus - Google Patents
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Abstract
The invention relates to a method for extracting compounds from Chondrus ocelltus, and belongs to the technical field of medical plant chemical extraction processes. A method for separating and preparing a monomer component from Chondrus ocelltus comprises the following steps: extracting Chondrus ocelltus with ethanol, carrying out extraction of the extract with petroleum ether, ethyl acetate and n-butanol, subjecting the n-butanol extract to silica gel column chromatography, eluting with a mixture of chloroform, methanol and water at a ratio of 7:3:0.1, collecting section by fractioning according to color and Rf value, combining same parts, concentrating under reduced pressure to obtain seven fractions C1-C7, wherein C2 is subjected to silica gel column chromatography again and eluting with a mixture of chloroform, methanol and water at a ratio of 9:2:0.1 to obtain five fractions, and C2-C4 are loaded on an Sephadex LH-20 column and eluting with a mixture of chloroform and methanol at a ratio of 1:1 to obtain white powered material adenosine triphosphate with a purity higher than 98%.
Description
Technical field
The present invention relates to a kind of extracting method that extracts compound from red algae carrageen, belong to medical herb chemical extraction Technology field.
Background technology
Carrageen, rhodophyta ，Shan algae section, Chondrus, Intertidal Algae, is commonly called as extra large auricularia auriculajudae." Chinese Sea medicine dictionary " recorded<sup TranNum="74">[2]</sup>: carrageen all edible, be used as medicine, have and relax bowel and the effect of blood detumescence, pain relieving myogenic, cure mainly the diseases such as chronic constipation, fracture, wound.In carrageen, contain multiple antibiotic and antiviral composition, not only can preventing cold, and can eradicate large-scale transmissible disease, Type B influenza and mumps virus are had to stronger inhibition ability.Along with to the going deep into of the pharmacology activity research of natural product, the many-sided physiologically active of carrageen is found, and has caused Chinese scholars and R&D personnel's extensive concern.
Carrageen is a kind of important economical alga, mainly for the production of carrageenin (also claiming carrageenin).But up to the present, the research of carrageen activeconstituents is only limited to some single compounds that the routine analysis of basal component and early stage separation are obtained.Therefore be necessary the chemical composition of carrageen to carry out more deep research.
Summary of the invention
The object of the present invention is to provide a kind of compound Triphosaden and extracting method extracting from red algae carrageen, the present invention further studies the chemical composition of carrageen, first more same season different location the difference of nutritive ingredient of carrageen, by modern separation means, the physiologically active substance in carrageen is extracted separated, adopt Modern spectroscopy technology to carry out Structural Identification to extract, and carry out antibiotic and immunocompetent research, the development and utilization that purport is carrageen provides certain foundation.
The present invention is achieved by the following technical solutions
The compound extracting from red algae carrageen, special character is this compound called after: Triphosaden, it has the chemical formula of following structure:
From red algae carrageen, extract a method for Triphosaden, its special character is to comprise the following steps:
(1), by red algae carrageen powder be placed in 3-5 doubly the solvent cold soaking of its quality extract, guarantee that the solvent quality concentration after soaking is 80%-90%, filter and remove algae-residue, united extraction liquid, evaporated under reduced pressure solvent, obtains deep green oily medicinal extract;
(2), successively with sherwood oil, ethyl acetate and n-butanol extraction extract concentrated solution;
(3), by n-butyl alcohol phase extract by adopting silica gel column chromatography, with chloroform: methyl alcohol: water=7:3:0.1 carries out wash-out, utilizes TLC thin-layer chromatography to follow the tracks of and detects, according to Rf and color, carry out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7, gets C2 standby;
(4), getting C2 uses silica gel column chromatography, use chloroform: methyl alcohol: water=9:2:0.1, obtains C2-1, C2-2, C2-3, C2-4, C2-5 again; Through a large amount of screening, get C2-4 with Sephadex LH-20 post through chloroform: methyl alcohol=1:1 wash-out, wherein C2-4c, uses chloroform repetitive scrubbing, obtains white powder material.
According to detector ultraviolet spectrogram, the identical sample of each separating obtained chromatographic peak is collected and merged identical component, obtain the monomeric substance Triphosaden that purity is greater than 98%.
The concrete steps of said extracted process are as follows:
(1), red algae carrageen powder is placed in to the doubly solvent normal temperature cold soaking 7-10 days of its quality of 3-5, guarantee that the solvent quality concentration after soaking is 80%-90%, change solvent 3-5 time continuously, carry out 3-5 extraction;
Described solvent is ethanol; Normal temperature is generally 20-30 ℃;
(2) extract, in step 1 filters removes algae-residue, merges the extracting solution of above-mentioned 3-5 time, evaporated under reduced pressure solvent, and the alcohol in evaporated under reduced pressure extracting solution, obtains deep green oily medicinal extract;
(3), first deep green oily medicinal extract that step 2 is obtained add aqueous suspension, then use and the sherwood oil normal temperature extraction of suspension equivalent 4-8 time, merging sherwood oil phase, concentrating under reduced pressure obtains deep green medicinal extract;
(4), the water of step 3 gained adds again and the ethyl acetate normal temperature of water equivalent extraction 4-8 time, combined ethyl acetate phase, concentrating under reduced pressure obtains brown color medicinal extract;
(5), the water of step 4 gained adds again and the propyl carbinol normal temperature of water equivalent extraction 4-8 time, merging propyl carbinol phase, concentrating under reduced pressure obtains yellow medicinal extract;
(6), get 100-200 object silica gel, activate 25-35 minute at 110 ℃ ± 5 ℃, mix with sherwood oil, the ultrasonic bubble that degass, then wet method packs in chromatography column, pillar size: 50 * 600mm, dress post height: 400mm, standing 60-80 hour;
(7), collect the n-butyl alcohol phase extract in step 5, with dissolve with methanol, with the 60-100 order silica gel mixed sample of three times of its quality, dry method loading, respectively with chloroform: methyl alcohol: water=7:3:0.1 carries out gradient elution, with 50mL test tube Fractional Collections, every pipe is collected 45mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7;
C1: 1-6 manages merging; C2: 7-19 manages merging; C3: 20-34 manages merging; C4: 35-47 manages merging; C5: 48-61 manages merging; C6: 62-72 manages merging; C7: 73-89 manages merging;
(8), get silica gel 200-300 order, according to wet method dress post after the process activation of step 6, pillar size: 20 * 400mm, dress post height: 280mm;
(9), get the separating obtained fraction C2 of step 7, with dissolve with methanol, by 60 ~ 100 order silica gel mixed samples of three times of its quality, dry method loading, with chloroform: methyl alcohol: water=9:2:0.1 carries out gradient elution, with 20mL test tube Fractional Collections, every pipe is collected 18mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains five kinds of mixture fraction C2-1, C2-2, C2-3, C2-4, C2-5;
C2-1: 1-3 manages merging; C2-2: 4-12 manages merging; C2-3: 13-21 manages merging; C2-4: 22-29 manages merging; C2-5: 30-39 manages merging;
(10), get Sephadex LH-20 gel dress post, pillar specification: 15 * 800mm; Dress post height: 700mm, gets the separating obtained fraction C2-4 of step 9, uses chloroform: methyl alcohol=1:1 dissolves, loading;
Through chloroform: methyl alcohol=1:1 wash-out, with 10mL test tube Fractional Collections, every pipe is collected 5mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, wherein 10-17 pipe is C2-4c, and adularescent solid is separated out, and uses chloroform repetitive scrubbing, obtaining white powder material, is Triphosaden after testing.
The method for separating and preparing of monomer component in red algae carrageen of the present invention, by carrageen extraction using alcohol, extract is successively used sherwood oil, ethyl acetate, n-butanol extraction, by n-butyl alcohol phase extract by adopting silica gel column chromatography, with chloroform: methyl alcohol: water=7:3:0. 1 carries out wash-out, according to color and Rf value, carry out Fractional Collections, merge same section, concentrating under reduced pressure obtains seven fraction: C1-C7.Wherein C2 uses silica gel column chromatography again, chloroform: methyl alcohol: water=9:2:0.1, obtains five fractions.Wherein C2-4 with Sephadex LH-20 post through chloroform: methyl alcohol=1:1 wash-out, obtain white powder material Triphosaden, purity is higher than 98%.
The present invention further studies the chemical composition of carrageen, by modern separation means, the physiologically active substance in carrageen is extracted separated, adopt Modern spectroscopy technology to carry out Structural Identification to extract, and carry out antibiotic and immunocompetent research, for the development and utilization of carrageen provides certain foundation.
Accompanying drawing explanation
Fig. 1: the solvent of red algae carrageen ethanol extraction distributes schematic diagram;
Fig. 2: the separation process figure of red algae carrageen propyl carbinol phase extract.
Embodiment
Referring to accompanying drawing, provide the specific embodiment of the present invention, be used for formation of the present invention to be further described.
Embodiment 1
(1), red algae carrageen powder is placed in to the solvent normal temperature cold soaking 10 days of 3 times of its quality, guarantee that the solvent quality concentration after soaking is 85%, change continuously solvent 4 times, carry out 4 times and extract;
Described solvent is ethanol; Normal temperature is generally 20-30 ℃;
(2) extract, in step 1 filters removes algae-residue, merges the extracting solution of above-mentioned 4 times, evaporated under reduced pressure solvent, and the alcohol in evaporated under reduced pressure extracting solution, obtains deep green oily medicinal extract;
(3), first deep green oily medicinal extract that step 2 is obtained add aqueous suspension, then uses and the sherwood oil normal temperature extraction of suspension equivalent 6 times, merges sherwood oil phase, concentrating under reduced pressure obtains deep green medicinal extract;
(4), the water of step 3 gained adds again and the ethyl acetate normal temperature of water equivalent extraction 6 times, combined ethyl acetate phase, concentrating under reduced pressure obtains brown color medicinal extract;
(5), the water of step 4 gained adds again and the propyl carbinol normal temperature of water equivalent extraction 6 times, merges propyl carbinol phase, concentrating under reduced pressure obtains yellow medicinal extract;
(6), get 100-200 object silica gel, activate 30 minutes at 110 ℃ ± 5 ℃, mix with sherwood oil, the ultrasonic bubble that degass, then wet method packs in chromatography column, pillar size: 50 * 600mm, dress post height: 400mm, standing 60-80 hour;
(7), collect the n-butyl alcohol phase extract in step 5, with dissolve with methanol, with the 60-100 order silica gel mixed sample of three times of its quality, dry method is splined in the chromatography column of step (6), respectively with chloroform: methyl alcohol: water=7:3:0.1 carries out gradient elution, with 50mL test tube Fractional Collections, every pipe is collected 45mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7;
C1: 1-6 manages merging; C2: 7-19 manages merging; C3: 20-34 manages merging; C4: 35-47 manages merging; C5: 48-61 manages merging; C6: 62-72 manages merging; C7: 73-89 manages merging;
(8), get silica gel 200-300 order, according to wet method dress post after the process activation of step 6, pillar size: 20 * 400mm, dress post height: 280mm;
(9), get the separating obtained fraction C2 of step 7, with dissolve with methanol, with 60 ~ 100 order silica gel mixed samples of three times of its quality, dry method is splined in the chromatography column of step (8), with chloroform: methyl alcohol: water=9:2:0.1 carries out gradient elution, with 20mL test tube Fractional Collections, every pipe is collected 18mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains five kinds of mixture fraction C2-1, C2-2, C2-3, C2-4, C2-5;
C2-1: 1-3 manages merging; C2-2: 4-12 manages merging; C2-3: 13-21 manages merging; C2-4: 22-29 manages merging; C2-5: 30-39 manages merging;
(10), get Sephadex LH-20 gel dress post, pillar specification: 15 * 800mm; Dress post height: 700mm, gets the separating obtained fraction C2-4 of step 9, uses chloroform: methyl alcohol=1:1 dissolves, loading;
Through chloroform: methyl alcohol=1:1 wash-out, with 10mL test tube Fractional Collections, every pipe is collected 5mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, wherein 10-17 pipe is C2-4c, and adularescent solid is separated out, and uses chloroform repetitive scrubbing, obtaining white powder material, is Triphosaden.
Embodiment 2
(1), red algae carrageen powder is placed in to the solvent normal temperature cold soaking 10 days of 5 times of its quality, guarantee that the solvent quality concentration after soaking is 85%, change continuously solvent 5 times, carry out 5 times and extract;
Described solvent is ethanol; Normal temperature is generally 20-30 ℃;
(2) extract, in step 1 filters removes algae-residue, merges the extracting solution of above-mentioned 5 times, evaporated under reduced pressure solvent, and the alcohol in evaporated under reduced pressure extracting solution, obtains deep green oily medicinal extract;
(3), first deep green oily medicinal extract that step 2 is obtained add aqueous suspension, then uses and the sherwood oil normal temperature extraction of suspension equivalent 8 times, merges sherwood oil phase, concentrating under reduced pressure obtains deep green medicinal extract;
(4), the water of step 3 gained adds again and the ethyl acetate normal temperature of water equivalent extraction 8 times, combined ethyl acetate phase, concentrating under reduced pressure obtains brown color medicinal extract;
(5), the water of step 4 gained adds again and the propyl carbinol normal temperature of water equivalent extraction 8 times, merges propyl carbinol phase, concentrating under reduced pressure obtains yellow medicinal extract;
(6), get 100-200 object silica gel, activate 35 minutes at 110 ℃ ± 5 ℃, mix with sherwood oil, the ultrasonic bubble that degass, then wet method packs in chromatography column, pillar size: 50 * 600mm, dress post height: 400mm, standing 60-80 hour;
(7), collect the n-butyl alcohol phase extract in step 5, with dissolve with methanol, with the 60-100 order silica gel mixed sample of three times of its quality, dry method is splined in the chromatography column of step (6), respectively with chloroform: methyl alcohol: water=7:3:0.1 carries out gradient elution, with 50mL test tube Fractional Collections, every pipe is collected 45mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7;
C1: 1-6 manages merging; C2: 7-19 manages merging; C3: 20-34 manages merging; C4: 35-47 manages merging; C5: 48-61 manages merging; C6: 62-72 manages merging; C7: 73-89 manages merging;
(8), get silica gel 200-300 order, according to wet method dress post after the process activation of step 6, pillar size: 20 * 400mm, dress post height: 280mm;
(9), get the separating obtained fraction C2 of step 7, with dissolve with methanol, with 60 ~ 100 order silica gel mixed samples of three times of its quality, dry method is splined in the chromatography column of step (8), with chloroform: methyl alcohol: water=9:2:0.1 carries out gradient elution, with 20mL test tube Fractional Collections, every pipe is collected 18mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains five kinds of mixture fraction C2-1, C2-2, C2-3, C2-4, C2-5;
C2-1: 1-3 manages merging; C2-2: 4-12 manages merging; C2-3: 13-21 manages merging; C2-4: 22-29 manages merging; C2-5: 30-39 manages merging;
(10), get Sephadex LH-20 gel dress post, pillar specification: 15 * 800mm; Dress post height: 700mm, gets the separating obtained fraction C2-4 of step 9, uses chloroform: methyl alcohol=1:1 dissolves, loading;
Through chloroform: methyl alcohol=1:1 wash-out, with 10mL test tube, collect, every pipe is collected 5mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, wherein 10-17 pipe is C2-4c, and adularescent solid is separated out, and uses chloroform repetitive scrubbing, obtaining white powder material, is Triphosaden.
(1), red algae carrageen powder 30kg is placed in to the solvent normal temperature cold soaking 7 days of 4 times of its quality, guarantee that the solvent quality concentration after soaking is 90%, change continuously solvent 4 times, carry out 4 times and extract;
Described solvent is ethanol; Normal temperature is generally 20-30 ℃;
(2) extract, in step 1 filters removes algae-residue, merges the extracting solution of above-mentioned 4 times, evaporated under reduced pressure solvent, and the alcohol in evaporated under reduced pressure extracting solution, obtains deep green oily medicinal extract;
(3), first deep green oily medicinal extract that step 2 is obtained add aqueous suspension, then uses and the sherwood oil normal temperature extraction of suspension equivalent 6 times, merges sherwood oil phase, concentrating under reduced pressure obtains deep green medicinal extract;
(4), the water of step 3 gained adds again and the ethyl acetate normal temperature of water equivalent extraction 6 times, combined ethyl acetate phase, concentrating under reduced pressure obtains brown color medicinal extract;
(5), the water of step 4 gained adds again and the propyl carbinol normal temperature of water equivalent extraction 6 times, merges propyl carbinol phase, concentrating under reduced pressure obtains yellow medicinal extract;
(6), get 100-200 object silica gel, activate 25-35 minute at 110 ℃ ± 5 ℃, mix with sherwood oil, the ultrasonic bubble that degass, then wet method packs in chromatography column, pillar size: 50 * 600mm, dress post height: 400mm, standing 60-80 hour;
(7), collect the n-butyl alcohol phase extract in step 5, with dissolve with methanol, with the 60-100 order silica gel mixed sample of three times of its quality, dry method is splined in the chromatography column of step (6), respectively with chloroform: methyl alcohol: water=7:3:0.1 carries out gradient elution, with 50mL test tube Fractional Collections, every pipe is collected 45mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7;
C1: 1-6 manages merging; C2: 7-19 manages merging; C3: 20-34 manages merging; C4: 35-47 manages merging; C5: 48-61 manages merging; C6: 62-72 manages merging; C7: 73-89 manages merging;
(8), get silica gel 200-300 order, according to wet method dress post after the process activation of step 6, pillar size: 20 * 400mm, dress post height: 280mm;
(9), get the separating obtained fraction C2 of step 7, with dissolve with methanol, 60 ~ 100 order silica gel mixed samples by three times of its quality, dry method is splined in the chromatography column of step (8), with chloroform: methyl alcohol: water=9:2:0.1 carries out gradient elution, with 20mL test tube, carry out Fractional Collections, every pipe is collected 18mL, utilizing TLC thin-layer chromatography to follow the tracks of detects, according to Rf and color, carry out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains five kinds of mixture fraction C2-1, C2-2, C2-3, C2-4, C2-5;
C2-1: 1-3 manages merging; C2-2: 4-12 manages merging; C2-3: 13-21 manages merging; C2-4: 22-29 manages merging; C2-5: 30-39 manages merging;
(10), get Sephadex LH-20 gel dress post, pillar specification: 15 * 800mm; Dress post height: 700mm, gets the separating obtained fraction C2-4 of step 9, uses chloroform: methyl alcohol=1:1 dissolves, loading;
Through chloroform: methyl alcohol=1:1 wash-out, with 10mL test tube, collect, every pipe is collected 5mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, wherein 10-17 pipe is C2-4c, and adularescent solid is separated out, and uses chloroform repetitive scrubbing, obtaining white powder material, is Triphosaden.
A kind of compound Triphosaden (ATP) extracting from red algae carrageen of the present invention is a kind of coenzyme.Be improved the effect of body metabolism, participate in the metabolism of body fat, protein, sugar, nucleic acid and Nucleotide, be again the main source of energy i (in vivo) simultaneously.Be applicable to the disease that cellular enzymes goes down and causes after cell injury.Animal experiment finds that this product has obvious effect to myocardial cell's electric physiology, the flow of calcium ions that can suppress slow reacting cell, blocking-up and the forward conduction that extends atrioventricular nodal reentry loop, heavy dose of still turning back property of accessory pathway capable of blocking, there is vagal effect of enhancing, available supraventricular tachycardia.ATP may be used as the energy of nanotechnology and irrigation.Artificial cardiac pacemaker may benefit from this technology and no longer need battery that power is provided.
In poultry farming: 1. for getting fat, the growth promotion of the meat animals such as broiler chicken, meat duck, pig, beef cattle, mutton sheep, fish, shrimp; 2. for drinking water for animals, the food consumption causing because of disease, decline, supplement fast human body energy level; 3. after using this product can impel animal morbidity, get well fast; 4. be applicable to the reparation after hepar damnification that animal causes because of various paathogenic factors such as disease, medicine, toxin, kidney injury, intestinal mucosal injury, uterine tube damage.
Claims (1)
1. from red algae carrageen, extract a method for Triphosaden, it is characterized in that the concrete steps of leaching process are as follows:
(1), red algae carrageen powder is placed in to the doubly solvent normal temperature cold soaking 7-10 days of its quality of 3-5, guarantee that the solvent quality concentration after soaking is 80%-90%, change solvent 3-5 time continuously, carry out 3-5 extraction;
Described solvent is ethanol; Normal temperature is 20-30 ℃;
(2) extract, in step 1 filters removes algae-residue, merges the extracting solution of above-mentioned 3-5 time, evaporated under reduced pressure solvent, and the alcohol in evaporated under reduced pressure extracting solution, obtains deep green oily medicinal extract;
(3), first deep green oily medicinal extract that step 2 is obtained add aqueous suspension, then use and the sherwood oil normal temperature extraction of suspension equivalent 4-8 time, merging sherwood oil phase, concentrating under reduced pressure obtains deep green medicinal extract;
(4), the water of step 3 gained adds again and the ethyl acetate normal temperature of water equivalent extraction 4-8 time, combined ethyl acetate phase, concentrating under reduced pressure obtains brown color medicinal extract;
(5), the water of step 4 gained adds again and the propyl carbinol normal temperature of water equivalent extraction 4-8 time, merging propyl carbinol phase, concentrating under reduced pressure obtains yellow medicinal extract;
(6), get 100-200 object silica gel, activate 25-35 minute at 110 ℃ ± 5 ℃, mix with sherwood oil, the ultrasonic bubble that degass, then wet method packs in chromatography column, pillar size: 50 * 600mm, dress post height: 400mm, standing 60-80 hour;
(7), collect the n-butyl alcohol phase extract in step 5, with dissolve with methanol, with the 60-100 order silica gel mixed sample of three times of its quality, dry method loading, respectively with chloroform: methyl alcohol: water=7:3:0.1 carries out gradient elution, with 50mL test tube Fractional Collections, every pipe is collected 45mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains seven kinds of mixture fraction C1-C7;
C1: 1-6 manages merging; C2: 7-19 manages merging; C3: 20-34 manages merging; C4: 35-47 manages merging; C5: 48-61 manages merging; C6: 62-72 manages merging; C7: 73-89 manages merging;
(8), get silica gel 200-300 order, according to wet method dress post after the process activation of step 6, pillar size: 20 * 400mm, dress post height: 280mm;
(9), get the separating obtained fraction C2 of step 7, with dissolve with methanol, by 60 ~ 100 order silica gel mixed samples of three times of its quality, dry method loading, with chloroform: methyl alcohol: water=9:2:0.1 carries out gradient elution, with 20mL test tube Fractional Collections, every pipe is collected 18mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, concentrating under reduced pressure obtains five kinds of mixture fraction C2-1, C2-2, C2-3, C2-4, C2-5;
C2-1: 1-3 manages merging; C2-2: 4-12 manages merging; C2-3: 13-21 manages merging; C2-4: 22-29 manages merging; C2-5: 30-39 manages merging;
(10), get Sephadex LH-20 gel dress post, pillar specification: 15 * 800mm; Dress post height: 700mm, gets the separating obtained fraction C2-4 of step 9, uses chloroform: methyl alcohol=1:1 dissolves, loading;
Through chloroform: methyl alcohol=1:1 wash-out, with 10mL test tube Fractional Collections, every pipe is collected 5mL, utilizes TLC thin-layer chromatography to follow the tracks of and detects, and according to Rf and color, carries out segmentation, merge the Rf part identical with color, wherein 10-17 pipe is C2-4c, and adularescent solid is separated out, and uses chloroform repetitive scrubbing, obtaining white powder material, is Triphosaden after testing.
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