CN106518940A - Method for purifying vincoside lactam - Google Patents
Method for purifying vincoside lactam Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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Abstract
The invention provides a method for purifying vincoside lactam and belongs to the technical field of purification of natural plant monomers. According to the method, firstly, a common camptotheca fruit is extracted with an ethanol water solution, a common camptotheca fruit crude extract is obtained, vincoside lactam in the common camptotheca fruit crude extract is purified by the aid of three-zone simulated moving bed chromatography separation, a vincoside lactam extracting liquid is obtained and then is treated after being concentrated and crystalized, and high-purity vincoside lactam is obtained. The method can be used for purifying vincoside lactam efficiently on a large scale, stable, continuous and automatic operation is realized in the simulated moving bed chromatography separation process, a solid phase and a mobile phase can be repeatedly utilized, and the purification cost is reduced.
Description
Technical field
The invention belongs to natural plants monomer purification technical field, more particularly to a kind of method of purification vincoside-lactam.
Background technology
Fructus Camptothecae Acuminatae is the fruit of China endemic tree Fructus seu radix camptothecae acuminatae (Fructus Camptothecae Acuminatae), and since ancient times, Fructus seu radix camptothecae acuminatae (Fructus Camptothecae Acuminatae) is important medical material among the people, and can be complete
Strain medication, for treating pernicious treatment poison, tumor.Main chemical compositions in Fructus Camptothecae Acuminatae include：Camptothecine, 10-hydroxycamptothecine,
11- methoxycamptothecines, deoxocamptothecin, venoterpine, betulinic acid and vincoside-lactam.Research discovery, vincoside-lactam and camptothecine
Class compound has active anticancer, and vincoside-lactam also has antibacterial, antiviral, antiinflammatory, paroxysmal pain, antipyretic purposes.
By vincoside-lactam is extracted in Fructus Camptothecae Acuminatae, it is worth with important practical.The method for extracting separation vincoside-lactam at present is mainly
Column chromatography, such as：Ou Lailiang et al. (CN 1295239C, 2007) by Fructus Camptothecae Acuminatae ethanol solution percolation or ethanol solution 25-80
DEG C heat is extracted, extracting solution adsorbs in being passed through the resin column equipped with macroporous adsorbent resin (AL-2 adsorbent resiies), uses ethanol water
The step such as washing and desorbing, effluent concentrated by rotary evaporation and recrystallization obtains wedding fruits glycoside product；Wang Ruifang et al. (applied chemistry, 2005,
22(1)：24-29) with macropore super high cross-linked adsorbing resin (Rf18) and its methylamine (Rs3), the N- methyl vinyl aminations of synthesis
(Rs4), diformazan amination (Rs5), column chromatography for separation is carried out to camptothecine and vincoside-lactam after front three amination (Rs6)；Shi Weiguo et al.
(CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2008,32 (21)：2487-2489) with polyamide separation and purification 10-hydroxycamptothecine and vincoside-lactam；King
Auspicious virtue et al. (applied chemistry, 2009,26 (5)：593-596) Fructus Camptothecae Acuminatae is carried by the nano adsorption resin from different structure
The camptothecine and vincoside-lactam (CPT and VCS-LT) taken in liquid carries out chromatography.The technique that existing column chromatography purifies vincoside-lactam
Batch process is, eluant consumption is big, it is impossible to continuous to produce automatically.
Simulated moving bed chromatography (abbreviation SMBC) is the high efficiency separation means for purifying compound.Simulated moving bed chromatography is in system
On the basis of standby chromatograph, continuous operating mechanism is introduced, the separation of automatization and scale can be carried out.
The content of the invention
The purpose of the present invention is the deficiency for the presence of vincoside-lactam method is isolated and purified in prior art, there is provided Yi Zhongti
The method of pure vincoside-lactam.The method extracts Fructus Camptothecae Acuminatae crude extract with ethanol water first, recycles three band Simulation moving bed colors
Vincoside-lactam in spectrum separating-purifying Fructus Camptothecae Acuminatae crude extract, obtains vincoside-lactam extract, then after extract is concentrated and crystallized
Process obtains highly purified vincoside-lactam.The method can be with scale, efficiently purify vincoside-lactam, and simulated moving bed chromatography point
Sane, continuous, automatic running is realized from process, fixing phase and mobile phase can be recycled, and reduce cost for purification.
A kind of method of purification vincoside-lactam, comprises the steps：
(1) Fructus Camptothecae Acuminatae crude extract is prepared, i.e.,：Raw material pre-treatment
After Fructus Camptothecae Acuminatae raw material is smashed, leached 1-3 time with solvent, obtain leaching liquid；After leaching liquid is concentrated, plus ethanol or water
And ethanol, make that the mixeding liquid volume is the leaching liquid volume 1/5～1/20, and in the mixed liquor ethanol volume basis
Content is 60～100%, and the precipitation produced in removing mixed liquor obtains filtrate；Water and ethanol dilution filtrate are used again, obtain Fructus Camptothecae Acuminatae thick
Extract enters sample liquid；
The solid-liquid ratio of the Fructus Camptothecae Acuminatae raw material and solvent is 1g: 10mL～1g: 20mL；The volume hundred of ethanol in the solvent
Content is divided to be 50～100%, balance of water；
The Fructus Camptothecae Acuminatae crude extract enter vincoside-lactam in sample liquid concentration be 0.1～3mg/mL, the volumn concentration of ethanol
For 40～65%；
(2) vincoside-lactam is purified with SMBC
1) SMBC separation conditions are as follows：
Chromatographic column：3～10；
Fixing phase：Octadecylsilane chemically bonded silica ODS, 10～60 μm；
Operational mode：Three band SMBC are set, and three bands include elution band, refined band and absorption band, and a is elution band chromatographic column number
Mesh, 1≤a≤2；B is refined band chromatographic column number, 1≤b≤4；C is absorption band chromatographic column number, and 1≤c≤4, operational mode are used
A-b-c is represented；
Flowing phase composition：Mobile phase P of elution band is ethanol and the mixed solution or ethanol of water, ethanol in mobile phase P
Volumn concentration is 50～100%；Mobile phase D of refined band and absorption band is ethanol and the mixed solution of water, the body of ethanol
Product percentage composition is 50～70%；
Flow rate of mobile phase：In refined band and absorption band, eluent D flow velocity QDFor 1～10 times of column volume, i.e., 1 per hour
～10BV/h, as eluent D flow velocity QDUnit is mL/min, and chromatograph column radius r units are cm, and column's length L units are cm
When, then 1 BV/h is equivalent to 60QD/(πr2L)；Enter sample liquid F flow velocity QFFor 0.1QD～1.0QD, raffinate R flow velocity QR=QD+QF；
In elution band, eluent P flow velocity QpFor 0.5QD～2QD, extract E flow velocity QE=Qp；
Switching time TS：8～20min；
Simulation moving bed operation temperature：Room temperature；
2) SMBC separation processes are as follows：
SMBC separation is carried out under above-mentioned SMBC working condition, Fructus Camptothecae Acuminatae crude extract sample introduction is continuously pumped into by material liquid entrance
Liquid, SMBC automatic control systems press switching time TSAlong mobile phase direction by eluent entrance, extract export, material liquid entrance
Next root chromatogram column is moved to successively simultaneously with the position of raffinate outlet, removes various front impurity from raffinate R outlets, from extraction
Take liquid E outlets and obtain vincoside-lactam extract；
(3) post processing is carried out to extract
Vincoside-lactam extract will be contained and be concentrated into muddiness, stratification will discard upper strata milky white liquid, with distilled water to lower floor
Precipitation is cleaned, until cleanout fluid is colourless；Wedding fruits glycoside product is obtained to lower sediment recrystallization with ethanol again.
A kind of method of above-mentioned purification vincoside-lactam, can substitute ethanol as solvent or mobile phase with methanol.
It is of the invention compared with existing preparative hplc isolation technics, which significantly has the beneficial effect that：
1st, in the present invention, pre-treatment of the ethanol-water solution to Fructus Camptothecae Acuminatae raw material fully can be removed into sample liquid insoluble matter, it is ensured that
The stable operation of SMBC, the extract obtained by SMBC can obtain highly purified vincoside-lactam in conjunction with post processing, and purity is higher than
98%.
2nd, the present invention being capable of scale, sane, continuous, automatic, the efficiently purification happiness from Fructus Camptothecae Acuminatae using SMBC technologies
Fruit glycosides, in the extract of SMBC, product recovery rate is higher than 90% higher than 99%, HPLC purity, and fixing phase and mobile phase can be anti-
It is multiple to utilize, cost for purification is reduced, belongs to environmental protection separation process.
Description of the drawings
In Fig. 1, embodiment 1, Fructus Camptothecae Acuminatae enters the HPLC spectrograms of sample liquid.
Three band SMBC systems in Fig. 2, embodiment 1.
The three HPLC spectrograms with SMBC raffinates in Fig. 3, embodiment 1.
The three HPLC spectrograms with SMBC extracts in Fig. 4, embodiment 1.
The HPLC spectrograms of post-treated wedding fruits glycoside product in Fig. 5, embodiment 1.
The crystal scanning electron microscope (SEM) photograph of post-treated wedding fruits glycoside product in Fig. 6, embodiment 1.
Specific embodiment
A kind of method of purification vincoside-lactam, comprises the steps：
(1) prepare Fructus Camptothecae Acuminatae crude extract
After Fructus Camptothecae Acuminatae raw material is smashed, leached 1-3 time with solvent, obtain leaching liquid；After leaching liquid is concentrated, plus ethanol or water
And ethanol, make that the mixeding liquid volume is the leaching liquid volume 1/5～1/20, and in the mixed liquor ethanol volume basis
Content is 60～100%, and the precipitation produced in removing mixed liquor obtains filtrate；Water and ethanol dilution filtrate are used again, obtain Fructus Camptothecae Acuminatae thick
Extract enters sample liquid；
The solid-liquid ratio of the Fructus Camptothecae Acuminatae raw material and solvent is 1g: 10mL～1g: 20mL, and in solvent, the volume basis of ethanol contain
Measure as 50～100%, balance of water；
The Fructus Camptothecae Acuminatae crude extract enter vincoside-lactam in sample liquid concentration be 0.1～3mg/mL, the volumn concentration of ethanol
For 40～65%；
(2) vincoside-lactam is purified with SMBC
1) SMBC separation conditions are as follows：
Chromatographic column：3～10；
Fixing phase：Octadecylsilane chemically bonded silica ODS, 10～60 μm；
Operational mode：Three band SMBC are set, and three bands include elution band, refined band and absorption band, and a is elution band chromatographic column number
Mesh, 1≤a≤2；B is refined band chromatographic column number, 1≤b≤4；C is absorption band chromatographic column number, and 1≤c≤4, operational mode are used
A-b-c is represented；
Flowing phase composition：Mobile phase P of elution band is ethanol and the mixed solution or ethanol of water, ethanol in mobile phase P
Volumn concentration is 50～100%；Mobile phase D of refined band and absorption band is ethanol and the mixed solution of water, the body of ethanol
Product percentage composition is 50～70%；
Flow rate of mobile phase：In refined band and absorption band, eluent D flow velocity QDFor 1～10 times of column volume, i.e., 1 per hour
～10BV/h, as eluent D flow velocity QDUnit is mL/min, and chromatograph column radius r units are cm, and column's length L units are cm
When, then 1 BV/h is equivalent to 60QD/(πr2L)；Enter sample liquid F flow velocity QFFor 0.1QD～1.0QD, raffinate R flow velocity QR=QD+QF；
In elution band, eluent P flow velocity QpFor 0.5QD～2QD, extract E flow velocity QE=Qp；
Switching time TS：8～20min；
Simulation moving bed operation temperature：Room temperature；
2) SMBC separation processes are as follows：
SMBC separation is carried out under above-mentioned SMBC working condition, Fructus Camptothecae Acuminatae crude extract sample introduction is continuously pumped into by material liquid entrance
Liquid, SMBC automatic control systems press switching time TSAlong mobile phase direction by eluent entrance, extract export, material liquid entrance
Next root chromatogram column is moved to successively simultaneously with the position of raffinate outlet, removes various front impurity from raffinate R outlets, from extraction
Take liquid E outlets and obtain vincoside-lactam extract；
(3) post processing is carried out to extract
Vincoside-lactam extract will be contained and be concentrated into muddiness, stratification will discard upper strata milky white liquid, with distilled water to lower floor
Precipitation is cleaned, until cleanout fluid is colourless；Wedding fruits glycoside product is obtained to lower sediment recrystallization with ethanol again.
A kind of method of above-mentioned purification vincoside-lactam, can substitute ethanol as solvent or mobile phase with methanol.
The detection method method of vincoside-lactam is：
High performance liquid chromatograph：Agilent 1200；Analysis chromatographic column：Extend-C18,5 μm, 150mm × 4.6mm
I.D.；Mobile phase：V (methanol): V (water)=60: 40；Detection wavelength：256nm flow velocitys：1.2mL/min；Column temperature：25℃.By liking
Fruit glycosides standard substance are demarcating the content of prepare liquid vincoside-lactam.
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1st, prepare Fructus Camptothecae Acuminatae crude extract
The Fructus Camptothecae Acuminatae raw material of 100g crushing is taken, adds 1L ethanol, supersonic leaching 2 times at 60 DEG C to leach 60min every time,
Obtain leaching liquid；Then leaching liquid is concentrated into into 75mL, plus 25mLH2O, stratification remove the precipitation that the mixed liquor is produced,
Take filtrate；Filtrate is diluted with water-ethanol (volume ratio 5: 5), obtain Fructus Camptothecae Acuminatae crude extract enters sample liquid, wherein, vincoside-lactam concentration is
0.56mg/mL, its chromatographic purity are 23.79%, see Fig. 1.
2nd, vincoside-lactam is purified with SMBC from Fructus Camptothecae Acuminatae crude extract
1) SMBC separation conditions are as follows：
Chromatographic column：6, diameter 1cm, long 20cm；
Fixing phase：Octadecylsilane chemically bonded silica ODS, 20～30 μm；
Operational mode：1-3-2, i.e. elution band：1 root chromatogram column；Refined band：3 root chromatogram columns；Absorption band：2 root chromatogram columns,
As shown in Figure 2；
Flowing phase composition：Mobile phase P of elution band is 95% ethanol；Refined band and absorption band mobile phase D be ethanol with
The mixed solution of water, the volumn concentration of ethanol is 60%；
Flow rate of mobile phase：In elution band, eluent P flow velocity QpFor 1.5mL/min, extract E flow velocity QE=Qp；In essence
In band processed and absorption band, eluent D flow velocity QDFor 1.53mL/min, enter sample liquid F flow velocity QFFor 0.29mL/min, raffinate R flow velocitys
QR=QD+QF；
Switching time：9.3min；
Simulation moving bed operation temperature：Room temperature；
2) SMBC separation processes are as follows：
SMBC separation is carried out under above-mentioned SMBC working condition, entering for Fructus Camptothecae Acuminatae crude extract is pumped into by material liquid entrance continuously
Sample liquid, SMBC automatic control systems press switching time TSEluent entrance, extract are exported along mobile phase direction, material liquid enters
The position of mouth and raffinate outlet is moved to next root chromatogram column simultaneously successively, removes various front impurity from raffinate R outlets, extracts
Extraction raffinate HPLC spectrogram obtains vincoside-lactam extract as shown in figure 3, exporting from extract E, the chromatographic purity of vincoside-lactam in extract
For 91.56%, yield 99.28%, extract HPLC spectrograms are as shown in Figure 4.
3rd, post processing is carried out to extract
Vincoside-lactam extract will be contained and be concentrated into muddiness, stratification will discard upper strata milky white liquid, with distilled water to lower floor
Precipitation is cleaned, until solution is colourless, with ethanol to precipitating three recrystallization, obtains the vincoside-lactam that chromatographic purity is 99.1%
Product, its HPLC spectrogram is as shown in figure 5, the stereoscan photograph of its pattern is shown in Fig. 6.
Embodiment 2
In addition to the description below, other conditions are with step with embodiment 1；
Prepare Fructus Camptothecae Acuminatae crude extract and enter sample liquid：After 100g Fructus Camptothecae Acuminatae is crushed, with the mixing of ethanol and water (volume ratio 7: 3)
At 60 DEG C of solution, supersonic leaching is secondary, and each supersonic leaching 60min, solid-liquid ratio 1: 15 obtain leaching liquid；After leaching liquid dense doing
Plus ethanol and water (volume ratio 7: 3) 100mL, mixed liquor is obtained, the precipitation of mixed liquor is removed, is taken filtrate；With ethanol and water (volume
Than 5: filtrate is diluted 5), obtain Fructus Camptothecae Acuminatae crude extract enters sample liquid, wherein, the concentration of vincoside-lactam is 1.14mg/mL.
Vincoside-lactam extract is obtained from SMBC extracts E outlets, the chromatographic purity and yield of vincoside-lactam are respectively 91.07%
With 99.34%.
Post processing is carried out to extract and obtains the wedding fruits glycoside product that chromatographic purity is 98.80%.
Embodiment 3
In addition to the description below, other conditions are with step with embodiment 1；
Prepare Fructus Camptothecae Acuminatae crude extract and enter sample liquid：After 100g Fructus Camptothecae Acuminatae is crushed, with the mixing of ethanol and water (volume ratio 7: 3)
Solution supersonic leaching is secondary, and each supersonic leaching 60min, solid-liquid ratio 1: 15 obtain leaching liquid；Leaching liquid it is dense it is dry after plus ethanol with
Water (volume ratio 6: 4) 150mL, obtains mixed liquor, removes the precipitation of mixed liquor, obtains filtrate；It is dilute with ethanol and water (volume ratio 6: 4)
Filtrate is released, obtain Fructus Camptothecae Acuminatae crude extract enters sample liquid, wherein, the concentration of vincoside-lactam is 1.0mg/mL.
Chromatographic column：4, diameter 2cm, long 20cm；
Fixing phase：Octadecylsilane chemically bonded silica ODS, 30～40 μm；
Operational mode：1-1-2；
Eluent P flow velocity QpFor 6mL/min, extract E flow velocity QE=Qp；Eluent D flow velocity QDFor 6mL/min, enter sample liquid
F flow velocity QFFor 1.2mL/min, raffinate R flow velocity QR=QD+QF；
Export from SMBC extracts E, obtain vincoside-lactam extract, vincoside-lactam chromatographic purity 91.90%, the response rate
99.50%.
Post processing is carried out to extract and obtains the wedding fruits glycoside product that chromatographic purity is 98.85%.
Claims (4)
1. it is a kind of purification vincoside-lactam method, it is characterised in that comprise the steps：
(1) prepare Fructus Camptothecae Acuminatae crude extract
After Fructus Camptothecae Acuminatae raw material is smashed, leached 1-3 time with solvent, obtain leaching liquid；After leaching liquid is concentrated, plus ethanol or water and second
Alcohol, make that the mixeding liquid volume is the leaching liquid volume 1/5～1/20, and in the mixed liquor ethanol volumn concentration
For 60～100%；The precipitation produced in removing mixed liquor, obtains filtrate；Water and ethanol dilution filtrate are used again, obtain Fructus Camptothecae Acuminatae crude extract
Enter sample liquid；
(2) vincoside-lactam is purified with simulated moving bed chromatography abbreviation SMBC
1) SMBC separation conditions are as follows：
Chromatographic column：3～10；
Fixing phase：Octadecylsilane chemically bonded silica ODS, 10～60 μm；
Operational mode：Three band SMBC are set, and three bands include elution band, refined band and absorption band, a is elution band chromatographic column number, 1
≤a≤2；B is refined band chromatographic column number, 1≤b≤4；C is absorption band chromatographic column number, 1≤c≤4, operational mode a-b-
C is represented；
Flowing phase composition：Mobile phase P of elution band is ethanol and the mixed solution or ethanol of water, the volume of ethanol in mobile phase P
Percentage composition is 50～100%；Mobile phase D of refined band and absorption band is ethanol and the mixed solution of water, the volume hundred of ethanol
Content is divided to be 50～70%；
Flow rate of mobile phase：In refined band and absorption band, eluent D flow velocity QDFor 1～10 times of column volume per hour, enter sample liquid F stream
Fast QFFor 0.1QD～1.0QD, raffinate R flow velocity QR=QD+QF；In elution band, eluent P flow velocity QpFor 0.5QD～2QD, extraction
Take liquid E flow velocity QE=Qp；
Switching time TS：8～20min；
Simulation moving bed operation temperature：Room temperature；
2) SMBC separation processes are as follows：
SMBC separation is carried out under above-mentioned SMBC working condition, Fructus Camptothecae Acuminatae crude extract is continuously pumped into by material liquid entrance and is entered sample liquid,
SMBC automatic control systems press switching time TSAlong mobile phase direction by eluent entrance, extract export, material liquid entrance and
The position of raffinate outlet is moved to next root chromatogram column simultaneously successively, removes various front impurity from raffinate R outlets, from extraction
Liquid E outlets obtain vincoside-lactam extract；
(3) post processing is carried out to extract
Vincoside-lactam extract is concentrated into into muddiness, stratification discards upper strata milky white liquid, lower sediment entered with distilled water
Row cleaning, until cleanout fluid is colourless；Wedding fruits glycoside product is obtained to lower sediment recrystallization with ethanol again.
2. it is according to claim 1 it is a kind of purification vincoside-lactam method, it is characterised in that in the step (1), Fructus Camptothecae Acuminatae
The solid-liquid ratio of raw material and solvent is 1g: 10mL～1g: 20mL；In the solvent, the volumn concentration of ethanol is 50～100%,
Balance of water.
3. it is according to claim 1 it is a kind of purification vincoside-lactam method, it is characterised in that in the step (1), Fructus Camptothecae Acuminatae
It is 0.1～3mg/mL that crude extract enters the concentration of vincoside-lactam in sample liquid, and the volumn concentration of ethanol is 40～65%.
4. the method for a kind of purification vincoside-lactam according to claims 1 to 3 any one, it is characterised in that replaced by methanol
For ethanol as solvent or mobile phase.
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| CN1634951A (en) * | 2004-11-25 | 2005-07-06 | 南开大学 | Process for extracting camptothecin |
| CN101313914A (en) * | 2007-05-29 | 2008-12-03 | 江苏康缘药业股份有限公司 | Uses and preparations of common camptotheca fruit glycosides of common camptotheca fruit extract |
| CN103936816A (en) * | 2014-04-14 | 2014-07-23 | 辽宁科技大学 | Method for purifying tanshinone IIA in salvia miltiorrhiza crude extract through simulated moving bed chromatography |
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