CN102070594A - Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol - Google Patents
Separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol Download PDFInfo
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- CN102070594A CN102070594A CN 200910201848 CN200910201848A CN102070594A CN 102070594 A CN102070594 A CN 102070594A CN 200910201848 CN200910201848 CN 200910201848 CN 200910201848 A CN200910201848 A CN 200910201848A CN 102070594 A CN102070594 A CN 102070594A
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Abstract
The invention discloses a high-speed counter-current chromatography separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol monomers. The method comprises the following steps of: preparing a crude agilawood extract serving as a sample introduction substance; preparing a two-phase solvent system of a stationary phase and a mobile phase; filling the stationary phase in a counter-current chromatograph separation column; rotating a main machine, and pumping the mobile phase into the column; introducing a sample by using a sample introduction valve; and receiving target components according to ultraviolet detection absorption peaks. The solvent system consists of four components (A, B, C and D), wherein the component A is normal paraffin, cycloparaffin or halogenated hydrocarbon; the component B is halogenated hydrocarbon; the component C is fatty alcohol or fatty ketone; and the component D is water. The upper phase is the stationary phase, and the lower phase is the mobile phase. By the method, high-purity agarotetrol and 4'-methoxy agarotetrol can be obtained, and the purity can reach over 97 percent; and the method can ensure high-peak resolution, has high separation amount, mild separation environment and high reclamation rate of target compounds, and is simple and convenient to operate and easy to popularize and use.
Description
Technical field
The present invention relates to a kind of agalloch eaglewood tetrol and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, relate in particular to a kind of application high-speed countercurrent chromatography (HSCCC) separate prepare high purity agalloch eaglewood tetrol and 4 '-method of methoxyl group agalloch eaglewood tetrol.
Technical background
Agalloch eaglewood is the resiniferous timber of thymelaeceae plant Lignum Aquilariae Resinatum Aquilaria sinensis (Lour.) Gilg, be called homemade agalloch eaglewood, aquilaria sinensis, lignum aquilariae resinatum, its flavor is hot, bitter, slightly warm in nature, the effect of tool promoting the circulation of QI to relieve pain, warming middle-JIAO to arrest vomiting, helping inspiration to relieve asthma is used for the vexed pain of chest abdominal distension, gastrofrigid vomiting hiccup, the circulation of vital energy in the wrong direction of suffering from a deficiency of the kidney and breathes heavily urgency.
Homemade agalloch eaglewood The Chemical Constituents just begins starting up to the eighties, its chemical ingredients can be divided into 3 classes substantially, it is sesquiterpenoids composition, aromatic component and 2-(2-styroyl) chromone class, wherein 2-(2-styroyl) chromone class material has anti-allergic effects in various degree, is one of its activeconstituents.Contain multiple 2-(2-styroyl) chromone derivative in the agalloch eaglewood alcohol extract, wherein 4 '-content of methoxyl group agalloch eaglewood tetrol and agalloch eaglewood tetrol is higher, with the quality grade of agalloch eaglewood substantial connection is arranged, and can be used as the index composition of agalloch eaglewood quality control.
Agalloch eaglewood tetrol and 4 '-two compounds of methoxyl group agalloch eaglewood tetrol are structurally very similar, and therefore traditional separation method is difficult to it is directly separated, and 4 '-methoxyl group agalloch eaglewood tetrol generally obtains with the isolated in form of its derivative.
Agalloch eaglewood tetrol and 4 '-structural formula of methoxyl group agalloch eaglewood tetrol is as follows:
Agalloch eaglewood tetrol and 4 '-chemical structural formula of methoxyl group agalloch eaglewood tetrol
(High-speed Counter-current Chromatography HSCCC) is a kind of novel liquid-liquid chromatograph separation method that grows up the nineties in 20th century to high-speed countercurrent chromatography.Its principle is the centrifugal force that utilizes borded pile to produce when planetary motion, immiscible two-phase is constantly mixed, keep a phase (solid phase) wherein simultaneously, utilize constant flow pump to import another phase (moving phase) continuously, the solute that enters borded pile with moving phase distributes between two-phase repeatedly, press the order of partition ratio, quilt is wash-out successively.The elder generation that allocation proportion is big in moving phase is by wash-out, otherwise, solid mutually in big back of allocation proportion by wash-out.Be different from traditional liquid phase chromatography, the HSCCC analytical procedure is not used solid phase carrier, thereby has avoided effective constituent by shortcomings such as the irreversible adsorption of solid phase carrier and peak shape hangovers; But sample crude extract direct injection is separated, and can separate by efficient, quick and big preparation amount, and separation and purification can be finished synchronously with preparation, and organic solvent consumption is few, free of losses, pollution-free.Based on above advantage, no matter the HSCCC chromatographic instrument is as analysis mode instrument or preparation type instrument, on natural product, have wide development prospect and actual application value, it can extract the effective constituent of different qualities from the natural raw product of complexity, for the development of natural drug provides favourable condition.At present, Chinese scholars is utilized effective constituents such as flavones, alkaloid, anthraquinone derivatives, saponin in the successful separation and Extraction natural drug of HSCCC.Therefore, HSCCC is the very close effective constituent of structure--the better means of 2-(2-styroyl) chromone derivative of separating in the agalloch eaglewood.
Before the present invention, also not occur use high-speed countercurrent chromatography (HSCCC) isolate high purity agalloch eaglewood tetrol and 4 '-the open report of methoxyl group agalloch eaglewood tetrol.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of high purity agalloch eaglewood tetrol and 4 '-highspeed counter-current chromatographic separation process for preparing of methoxyl group agalloch eaglewood tetrol.
In order to solve the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A kind of high purity agalloch eaglewood tetrol and 4 '-highspeed counter-current chromatographic separation process for preparing of methoxyl group agalloch eaglewood tetrol, this method comprises the steps:
(1) preparation agalloch eaglewood crude extract is as the sample introduction thing;
(2) preparation constitutes the two phase solvent system of stationary phase, moving phase, this solvent system is by four component A, B, C, D forms, the A component is normal paraffin, naphthenic hydrocarbon or halogenated alkane, and the B component is a halogenated alkane, and the C component is Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketone, the D component is a water, behind this solvent system mixing standing demix, more than be stationary phase mutually, is moving phase mutually down;
(3) make in the high-speed counter-current chromatograph separator column and be full of stationary phase;
(4) main frame is rotated, then moving phase is pumped in the post, or stationary phase and moving phase are pumped in the post simultaneously, main frame is rotated;
(5) by the sampling valve sample introduction, according to ultraviolet detection absorption peak receiving target component, after separating, can obtain agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.
In the step (2), described normal paraffin is normal heptane or normal hexane; Described naphthenic hydrocarbon is hexanaphthene; Described halogenated alkane is tetracol phenixin or chloroform; Described Fatty Alcohol(C12-C14 and C12-C18) is methyl alcohol, ethanol or Virahol, and described aliphatic ketone is an acetone.
A in the described solvent system, B, C, the volume ratio of four components of D is followed successively by (0-1): (1-4): (1-4): (1-3), for example 0.2: 3.8: 2.6: 2.4 or 1: 3: 3: 2 etc.Solvent system is preferred: the A component is normal hexane or tetracol phenixin, and the B component is a chloroform, and the C component is a methyl alcohol, and the D component is a water.When wherein A component ratio became 0, solvent system can be changed into chloroform-methanol-aqueous systems.Preferred chloroform-methanol-aqueous systems of solvent system and preferred volume ratio are 4: 2.6: 2.4, more than be stationary phase mutually, is moving phase mutually down.
By volume each solution is placed separating funnel, shake up standing demix.Ready to balance will be gone up phase (stationary phase) and separate with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, column volume 119ml, sample introduction circle are 10ml,
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Before the moving phase sample introduction, earlier be full of whole pillar with stationary phase, the adjustment engine speed is 600-999rpm, with the flow velocity of 1-3mL/min moving phase is pumped in the post; Perhaps stationary phase and flow pumps in the post simultaneously, treat that solvent is full of whole pillar after, the adjustment engine speed is 600-999rpm.
Engine speed is high more, and the stationary phase retention rate is high more, but rotating speed is high more, easy more generation emulsion.When rotating speed in the 800-999r/min scope, separating effect is better, changes rotating speed in this scope, and the result is not had too big influence, so preferred 900r/min.
Flow rate of mobile phase is more little, and the stationary phase retention value is high more, good separating effect.When flow velocity in the 1.0-1.5mL/min scope, separating effect is better, when flow velocity is 1.2mL/min, resolution the best is so preferable flow rate is 1.2mL/min.
The present invention is fit to temperature 20-30 ℃.In the said temperature scope, when temperature was low, appearance time slightly shifted to an earlier date, and separation efficiency changes little, and peak shape is not had much influences.
In the step (3), when being full of stationary phase and balance in the described high-speed counter-current chromatograph separator column, control stationary phase retention value is 0.4-0.8, and preferred stationary phase retention value is 0.72.
Agalloch eaglewood tetrol and 4 through collecting after the disposable separation of system '-methoxyl group agalloch eaglewood tetrol evaporate to dryness after, 4 '-methoxyl group agalloch eaglewood tetrol is a yellow powder powder solid, the agalloch eaglewood tetrol is colourless plate crystal behind the methanol solvate recrystallization.
The present invention has following beneficial effect: the present invention since use high-speed countercurrent chromatography separate agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol, and adopt the processing condition of preferred solvent system, adjustment engine speed and flow velocity, separation efficiency is improved, obtain highly purified agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol; While separated object rate of recovery height, theory reaches 100%, and the present invention is actual to be reached more than 90%; And method for separating and preparing of the present invention is suitable for the agalloch eaglewood crude extract of various technology approach preparations, energy guarantees higher peak shape resolution, fractional dose is big, isolating environment is gentle, save solvent, easy and simple to handle, the agalloch eaglewood tetrol and 4 that obtains at last '-methoxyl group agalloch eaglewood tetrol solid detects through HPLC, and purity is all more than 97%.
Description of drawings
Fig. 1 is that the HSCCC-UV of the embodiment of the invention 1 detects collection of illustrative plates;
Fig. 2 is that the HSCCC-UV of the embodiment of the invention 2 detects collection of illustrative plates;
Fig. 3 is that the HSCCC-UV of the embodiment of the invention 3 detects collection of illustrative plates;
Fig. 4 is that the HSCCC-UV of the embodiment of the invention 4 detects collection of illustrative plates;
Fig. 5 is that the HSCCC-UV of the embodiment of the invention 5 detects collection of illustrative plates;
Fig. 6 is that the HSCCC-UV of the embodiment of the invention 6 detects collection of illustrative plates;
Fig. 7 is that the HSCCC-UV of the embodiment of the invention 7 detects collection of illustrative plates.
Embodiment
The invention will be further elaborated by the following examples:
Embodiment 1
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL 95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose normal heptane-chloroform-methanol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 0.5: 3.5: 2.8: 2.2 volume ratios placed separating funnel with above-mentioned solvent composition, shook up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 20 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 80mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 900rpm, with the flow velocity of 2.0mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 1, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 97%.
Embodiment 2
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL 95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose normal hexane-chloroform-methanol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 0.3: 3.7: 2.6: 2.4 volume ratios placed separating funnel with above-mentioned solvent composition, shook up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 20 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 30mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 900rpm, with the flow velocity of 1.0mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 2, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 98%.
Embodiment 3
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose tetracol phenixin-chloroform-acetone-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 0.2: 3.8: 3.2: 1.8 volume ratios were disposed at above-mentioned solvent composition in the separating funnel, shook up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 20 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 150mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 900rpm, with the flow velocity of 1.2mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 3, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 97%.
Embodiment 4
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose chloroform-methanol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 4: 2.6: 2.4 volume ratios above-mentioned solvent composition is disposed in the separating funnel, shakes up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 20 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 150mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 900rpm, with the flow velocity of 1.2mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 4, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 99%.
Embodiment 5
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose hexanaphthene-chloroform-Virahol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 1: 3: 3: 2 volume ratios were disposed at above-mentioned solvent composition in the separating funnel, shook up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 30 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 50mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 600rpm, with the flow velocity of 3.0mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 5, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target fraction evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 98%.
Embodiment 6
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose chloroform-alcohol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 1: 1: 1 volume ratio above-mentioned solvent composition is disposed in the separating funnel, shakes up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 20 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 70mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 800rpm, with the flow velocity of 1.0mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 6, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 98%.
Embodiment 7
It is meal that agalloch eaglewood is pulverized, and gets the 100g meal and adds 1000mL95% ethanol, behind refluxing extraction 3 hours, the each 3h, filter, and the rotation evaporate to dryness, it is standby to get brownish black medicinal extract.
From solvent system, choose chloroform-methanol-water half countercurrent chromatography instrument separate the preparation agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.By 4: 4: 3 volume ratios above-mentioned solvent composition is disposed in the separating funnel, shakes up the back standing demix.Ready to balance will be gone up phase (stationary phase) and separate 25 ℃ of experiment condition temperature with following (moving phase) mutually after for some time.Adopt TBE-300A type high-speed counter-current chromatograph, be furnished with
KTA purifier P-900 pump, UV detector, HX-1050 constant temperature circulator.Taking by weighing 150mg sample introduction thing is dissolved in the 10mL moving phase stand-by.Before the sample introduction, be full of whole separator column with stationary phase, the adjustment engine speed is 999rpm, with the flow velocity of 1.2mL/min moving phase is pumped in the post until setting up running balance, by the sampling valve sample introduction; UV value according to 254nm detects collection of illustrative plates, receiving target composition then.The HSCCC-UV collection of illustrative plates as shown in Figure 7, wherein, peak I is 4 '-methoxyl group agalloch eaglewood tetrol, peak ∏ is the agalloch eaglewood tetrol.Behind the target components evaporate to dryness, the agalloch eaglewood tetrol gets clear crystal after recrystallizing methanol, and two materials are through the detection of HPLC-UV, and purity is more than 97%.
Claims (9)
- A high purity agalloch eaglewood tetrol and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that this method adopts high-speed countercurrent chromatography, comprises the steps:(1) preparation agalloch eaglewood crude extract is as the sample introduction thing;(2) preparation constitutes the two phase solvent system of stationary phase, moving phase, this solvent system is by four component A, B, C, D forms, the A component is normal paraffin, naphthenic hydrocarbon or halogenated alkane, and the B component is a halogenated alkane, and the C component is Fatty Alcohol(C12-C14 and C12-C18) or aliphatic ketone, the D component is a water, behind this solvent system mixing standing demix, more than be stationary phase mutually, is moving phase mutually down;(3) make in the high-speed counter-current chromatograph separator column and be full of stationary phase;(4) main frame is rotated, then moving phase is pumped in the post, or stationary phase and moving phase are pumped in the post simultaneously, main frame is rotated;(5) by the sampling valve sample introduction, according to ultraviolet detection absorption peak receiving target component, after separating, can obtain agalloch eaglewood tetrol and 4 '-methoxyl group agalloch eaglewood tetrol.
- 2. high purity agalloch eaglewood tetrol as claimed in claim 1 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that in the step (2), described normal paraffin is normal heptane or normal hexane; Described naphthenic hydrocarbon is hexanaphthene; Described halogenated alkane is tetracol phenixin or chloroform; Described Fatty Alcohol(C12-C14 and C12-C18) is methyl alcohol, ethanol or Virahol, and described aliphatic ketone is an acetone.
- 3. high purity agalloch eaglewood tetrol according to claim 1 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that: in the step (2), A in the described solvent system, B, C, the volume ratio of four components of D is followed successively by (0-1): (1-4): (1-4): (1-3).
- According to each described high purity agalloch eaglewood tetrol and 4 of claim 1 to 3 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that: in the step (2), described solvent system is by following A, B, C, the D component is formed: the A component is normal hexane or tetracol phenixin, and the B component is a chloroform, the C component is a methyl alcohol, and the D component is a water.
- 5. high purity agalloch eaglewood tetrol as claimed in claim 1 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that, in step (4) and the step (5), the rotating speed of described main frame is controlled between the 600-999rpm/min, separation temperature is 20-30 ℃, and flow rate of mobile phase is controlled at 1.0-3.0mL/min.
- 6. high purity agalloch eaglewood tetrol as claimed in claim 5 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that described engine speed is 900rpm/min, separation temperature is 20 ℃, flow rate of mobile phase is 1.2mL/min.
- 7. high purity agalloch eaglewood tetrol as claimed in claim 4 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that, in the step (2), described solvent system is by following B, C, and the D component is formed: the B component is a chloroform, the C component is a methyl alcohol, and the D component is a water.
- 8. high purity agalloch eaglewood tetrol as claimed in claim 7 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that, B in the described solvent system, C, the volume ratio of D component was followed successively by 4: 2.6: 2.4.
- 9. high purity agalloch eaglewood tetrol as claimed in claim 1 and 4 '-method for separating and preparing of methoxyl group agalloch eaglewood tetrol, it is characterized in that: after step (5) is finished, will through agalloch eaglewood tetrol and 4 that separation obtains '-the component evaporate to dryness of methoxyl group agalloch eaglewood tetrol after, 4 '-methoxyl group agalloch eaglewood tetrol is a yellow powder powder solid, the agalloch eaglewood tetrol is colourless plate crystal behind the methanol solvate recrystallization.
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| CN108057035A (en) * | 2018-02-08 | 2018-05-22 | 中国科学院昆明植物研究所 | Application of the agalloch eaglewood tetrol in the drug for preparing prevention and treatment nerve degenerative diseases |
| CN110240585A (en) * | 2019-06-10 | 2019-09-17 | 上海诗丹德标准技术服务有限公司 | A kind of preparation method of agalloch eaglewood tetrol |
| CN112630339A (en) * | 2020-12-18 | 2021-04-09 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN113861135A (en) * | 2021-10-29 | 2021-12-31 | 北京中科沉香科技股份有限公司 | Aquilaria sinensis tetrol, pharmaceutical composition thereof, and preparation method and application thereof |
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| US5169984A (en) * | 1990-09-10 | 1992-12-08 | The United States Of America As Represented By The Department Of Health And Human Services | Synthesis and characterization of N-bromoacetyl-3,3'5-triiodo-L-thyronine using high speed countercurrent chromatography |
| CN1136024C (en) * | 1999-06-14 | 2004-01-28 | 北京市新技术应用研究所 | Highspeed counter-current chromatographic separation process for preparing high purity catechin |
| CN1323776A (en) * | 2001-05-31 | 2001-11-28 | 北京天纯维通生物技术有限公司 | Prepn. of resveratrol and resveratrol glycoside |
| CN1594261A (en) * | 2004-06-22 | 2005-03-16 | 上海同田生化技术有限公司 | Preparation method of high purity physcion and chrysophanol |
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| CN103145677A (en) * | 2013-02-27 | 2013-06-12 | 中山火炬职业技术学院 | Method for separating active ingredients from aquilaria sinensis lamina by utilizing high-speed countercurrent chromatography |
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| CN108057035A (en) * | 2018-02-08 | 2018-05-22 | 中国科学院昆明植物研究所 | Application of the agalloch eaglewood tetrol in the drug for preparing prevention and treatment nerve degenerative diseases |
| CN110240585A (en) * | 2019-06-10 | 2019-09-17 | 上海诗丹德标准技术服务有限公司 | A kind of preparation method of agalloch eaglewood tetrol |
| CN110240585B (en) * | 2019-06-10 | 2023-08-22 | 上海诗丹德标准技术服务有限公司 | Preparation method of agilawood tetraol |
| CN112630339A (en) * | 2020-12-18 | 2021-04-09 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN112630339B (en) * | 2020-12-18 | 2022-07-26 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN113861135A (en) * | 2021-10-29 | 2021-12-31 | 北京中科沉香科技股份有限公司 | Aquilaria sinensis tetrol, pharmaceutical composition thereof, and preparation method and application thereof |
| CN113861135B (en) * | 2021-10-29 | 2024-01-30 | 北京中科沉香科技股份有限公司 | Radix aucklandiae tetrol and pharmaceutical composition thereof, and preparation method and application thereof |
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