CN1550779A - Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus - Google Patents
Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus Download PDFInfo
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- CN1550779A CN1550779A CNA2004100349305A CN200410034930A CN1550779A CN 1550779 A CN1550779 A CN 1550779A CN A2004100349305 A CNA2004100349305 A CN A2004100349305A CN 200410034930 A CN200410034930 A CN 200410034930A CN 1550779 A CN1550779 A CN 1550779A
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Abstract
Separating unit of chromatograph comprises following parts and steps: solvent system for preparing component stationary phase, mobile phase; pumping prepared stationary phase or pressing it in air pressure mode to working drum of main unit and filling up the drum with the stationary phase; running the main unit and pumping soluble crude extract of camptothecin in prearranged flux and mobile phase; based on detected spectrogram, collecting monomolecular camptothecin component from mobile phase. The two-phase solvent system is composed of hydrocarbon alkylogen, fatty alcohol and water or buffer solution of potassium phosphate under normal temperature and pressure. Upper phase is stationary phase and lower phase is mobile phase. Features of the invention are: easy of operation, small capacity of organic solvent, high efficiency. Content of product of pure monomolecular camptothecin is as high as 98%.
Description
Technical field
The present invention relates to natural medicinal plant camplotheca acuminata deep processing field, relate in particular to a kind of planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device.
Background technology
Camptothecine (Camptothecin writes a Chinese character in simplified form CPT) is a kind of five-membered ring alkaloid that extracts from the non-irrigated nelumbium camplotheca acuminata of China distinctive Nyssaceae (Nyssaceae) (Camptotheca acuminata), is topmost alkaloid in the camplotheca acuminata.Since separation, structure determination and the powerful antitumor activity of Wall reported first in 1966 about the alkaloid camptothecine, people have produced keen interest to the research of alkaloid camptothecine.Clinical application research shows, this Alkaloid has stronger cytotoxic activity, can be by acting on DNA topoisomerase I (topoisomerase I, topo I) suppress dna replication dna, transcribe and mitosis, and topo I is a kind of and the closely-related a kind of enzyme of cell division, the generation of blocking-up this kind of enzyme can stop the growth of cancer cell, can be used for treating multiple malignant tumour, as osteocarcinoma, liver cancer, carcinoma of urinary bladder and leukaemia etc.
At present, it is domestic that directly the extraction process of acquisition alkaloid camptothecine crude extract is comparatively simple from the natural plants camplotheca acuminata, in general, the purity of crude extract product is lower, though by column chromatography and recrystallizing and refining, its purity can further improve, even can be up to about 98%, but yield descends significantly, and owing to adopted chromatographic column, equipment investment is bigger, operate loaded down with trivial details, also can make during column chromatography camptothecine easily by irreversible adsorption on column packing and lose, and because the instability of camptothecine, on solid packing, also degradation reaction can take place, thereby separation efficiency is lower.For the camplotheca acuminata resource of development and utilization China's abundant better, the extracting method of separating common camptotheca fruit alkali cpd is effectively had higher requirement.
Summary of the invention
The object of the present invention is to provide a kind of planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device.
Planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device has the main frame casing, rotatable a plurality of host work drums reach the polytetrafluoroethylene (PTFE) that links with the work drum and lead in/out pipe, side of each work drum is also disposing and rotatablely is being used for separating that strand leads in/out pipe separates the strand framework, lead in/out pipe and separate the strand framework with each work drum and side thereof and be connected in series successively, and draw outside the machine by the host center axle at last.The power output shaft of main frame fixed frame and motor connects and drives the main frame fixed frame rotates, rotating speed of motor can be controlled by frequency-variable controller, the bearing of central shaft is located on the main frame fixed frame, spigot shaft coaxle direct geared and each work drum rotating shaft coaxle gear are shared toe joint, and spigot shaft coaxle gear and each are separated strand framework rotating shaft coaxle gear and then connect by a carrier gear.
Detachment process of the present invention is to carry out continuously in the host work drum of centrifugal partition chromatograph instrument, easy to operation, the organic solvent charge capacity is few, it need not any solid-state stilt or carrier, compare the problems such as sample absorption loss, contamination and sex change that do not exist solid-state carrier to cause with column chromatography isochromatic spectrum method.The host work drum can need to be provided with, to regulate the different capabilities of separating column as the separating column of distribution chromatography by separation; Under the main frame operation conditions, a plurality of work drums rotate around the host center axle simultaneously with planetary, thereby have enlarged column capacity.In addition, adopt lead in/out pipe pass the host center axle is connected with the work drum and work drum with separate the mutual strand mode of separating that is connected in series of strand pipe, the technological deficiency of having avoided easy leakage of employing rotary seal joint and sample to be infected with.The camptothecin component of being extracted, through concentrating under reduced pressure, recrystallization, dual water washing, freeze-drying, can obtain the high-purity unimolecule camptothecine product of no solvent residue and residues of pesticides at last, its effective content is up to more than 98%, is a kind of separation efficiency height, extracting method easy and simple to handle.
This method is applicable to separates the highly purified unimolecule camptothecine of preparation from the camptothecine crude extract of all size, the preparation amount of its single device can be up to two hectograms.
Description of drawings
Accompanying drawing is planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device synoptic diagram.
Among the figure, 1 main frame casing, 2 host center axles, 3 host works drum, 4 lead in/out pipe, 5 and separate strand framework, 6 main frame fixed frames, 7 three phase electric machines, 8 frequency-variable controllers, 9 motor fixing frames, 10,11,12 central shaft bearings, 13 are separated strand pipe rotating shaft bearing, 14 work drum rotating shaft bearings, 15,17 spigot shaft coaxle gears, 16 work drum rotating shaft coaxle gears, 18 carrier gears, 19 and are separated strand framework rotating shaft coaxle gear, 20 lower margins.
Embodiment
Planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device comprises that main frame casing 1, the polytetrafluoroethylene (PTFE) that rotatable a plurality of host work drums 3 reach and the work drum links lead in/out and manage 4, side of each work drum is also disposing and rotatablely is being used for separating that strand leads in/out pipe separates strand framework 5, lead in/out pipe and separate the strand framework with each work drum and side thereof and be connected in series successively, and draw outside the machine by host center axle 2 at last.Main frame fixed frame 6 connects and the rotation of drive main frame fixed frame with the power output shaft of motor 7, and rotating speed of motor can be by frequency-variable controller 8 controls.The bearing 11,12 of central shaft is located on the main frame fixed frame, spigot shaft coaxle gear 15 direct and each drum rotating shaft coaxle gear 16 shared toe joint of working, spigot shaft coaxle gear 17 is separated strand framework rotating shaft coaxle gear 19 with each and is then passed through a carrier gear 18 connections.
Under the main frame running status, the angular velocity that the host work that rotates around its central shaft rouses is 2 ω, separates the strand framework and just makes counter-rotation around central shaft by the angular velocity of ω.
Work drum configuration quantity is 2～8, adopts polytetrafluoroethylene (PTFE) pipe, stainless-steel tube or the copper tube multiple wraps of all size, is designed to the work drum column capacity of different capabilities according to the big I of winding pipe caliber.
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
The column capacity of the polytetrafluoroethylene (PTFE) pipe of multiple wraps is about 12 liters in the host work drum of the centrifugal partition chromatograph instrument of present embodiment.Solvent system adopts methenyl choloride (chloroform): methyl alcohol: water=5: 2: 1, camptothecine content is about 20% (HPLC) in the camptothecine crude extract.Get methenyl choloride (chloroform) 150L, methyl alcohol 60L, water 30L, mixing in the mixing kettle of 300L, behind the standing demix, two-phase is separately standby up and down.Above as stationary phase, last flow velocity with 50ml/min pumped into or be pressed into and be full of the host work drum with the air pressure mode.Take by weighing camptothecine crude extract 160 grams,, filter standby with the following phase solution dissolving of 1000mL.Open the centrifugal partition chromatograph instrument, adjust engine speed 400rpm, pumping into down phase (down as moving phase) with the flow of 8mL/min then made total system set up mobile equilibrium in 1 hour, pump into the camptothecine crude extract of above-mentioned dissolving again with the flow of 50ml/min, treat to use instead behind the sample introduction remaining following phase and with the camptothecin component in the flow wash-out host work drum of 8mL/min.In the moving phase of wash-out, collect camptothecin component according to detecting spectrogram, and determine the time period of its outflow.The camptothecin component of separated and collected through the decompression precipitation concentrate, recrystallization, dual water washing, freeze-drying, can get unimolecule camptothecine 26g at last, its HPLC purity is up to more than 98%.
Embodiment 2
The column capacity of the polytetrafluoroethylene (PTFE) pipe of multiple wraps is about 25 liters in the host work drum of the centrifugal partition chromatograph instrument of present embodiment.Solvent system adopts methenyl choloride (chloroform): phenixin: methyl alcohol: water=2: 2: 3: 1, and camptothecine content is about 40% (HPLC) in the camptothecine crude extract.Get methenyl choloride (chloroform) 40L, phenixin 40L, methyl alcohol 60L, water 20L, mixing in the mixing kettle of 300L, behind the standing demix, two-phase is separately standby up and down.Above as stationary phase, last flow velocity with 80ml/min pumped into or be pressed into and be full of the host work drum with the air pressure mode.Take by weighing camptothecine crude extract 250 grams,, filter standby with the following phase solution dissolving of 2000mL.Open the centrifugal partition chromatograph instrument, adjust engine speed 400rpm, pump into the camptothecine crude extract of above-mentioned dissolving then with the flow of 20mL/min, it is constant to keep flow behind the sample introduction, pumps into down the camptothecin component in phase (down as moving phase) the wash-out host work drum.In the moving phase of wash-out, regularly collect camptothecin component according to detecting spectrogram, the determining of its delivery time section with embodiment 1.Equally, the camptothecin component of separated and collected gets the about 75g of unimolecule camptothecine at last through a series of aftertreatments, and its HPLC purity is up to more than 98%.
Embodiment 3
The column capacity of the polytetrafluoroethylene (PTFE) pipe of multiple wraps is about 32 liters in the host work drum of the centrifugal partition chromatograph instrument of present embodiment.Solvent system adopts methenyl choloride (chloroform): methyl alcohol: 0.07mol/L buffer solution of potassium phosphate=3: 3: 1, camptothecine content is about 50% (HPLC) in the camptothecine crude extract.Get methylene chloride 180L, methyl alcohol 180L, water 60L, mixing in the mixing kettle of 500L, behind the standing demix, two-phase is separately standby up and down.Above as stationary phase, last flow velocity with 80ml/min pumped into or be pressed into and be full of the host work drum with the air pressure mode.Take by weighing camptothecine crude extract 400 grams,, filter standby with the following phase solution dissolving of 2500mL.Open the centrifugal partition chromatograph instrument, adjust engine speed 350rpm, pump into the camptothecine crude extract of above-mentioned dissolving then with the flow of 30mL/min, it is constant to keep flow behind the sample introduction, pumps into down the camptothecin component in phase (down as moving phase) the wash-out host work drum.In the moving phase of wash-out, regularly collect camptothecin component according to detecting spectrogram, the determining of its delivery time section with embodiment 1.Equally, the camptothecin component of collection gets the about 140g of unimolecule camptothecine at last through a series of aftertreatments, and its HPLC purity is up to more than 98%.
Embodiment 4
The column capacity of the polytetrafluoroethylene (PTFE) pipe of multiple wraps is about 40 liters in the host work drum of the centrifugal partition chromatograph instrument of present embodiment.Solvent system adopts methenyl choloride (chloroform): methyl alcohol: 0.15mol/L buffer solution of potassium phosphate=3: 3: 1, camptothecine content is about 50% (HPLC) in the camptothecine crude extract.
Get methenyl choloride (chloroform) 180L, methyl alcohol 180L, water 60L, mixing in the mixing kettle of 500L, behind the standing demix, two-phase is separately standby up and down.Above as stationary phase, last flow velocity with 80ml/min pumped into or be pressed into and be full of the host work drum with the air pressure mode.Take by weighing camptothecine crude extract 480 grams,, filter standby with the following phase solution dissolving of 3000mL.As follows embodiment 3.Can get the about 175g of unimolecule camptothecine at last, its HPLC purity is up to more than 98%.
Embodiment 5
The column capacity of the copper tube of multiple wraps is about 40 liters in the host work drum of the centrifugal partition chromatograph instrument of present embodiment.Solvent system adopts methylene chloride: methyl alcohol: water=5: 4: 1, camptothecine content is about 50% (HPLC) in the camptothecine crude extract.Get methenyl choloride (chloroform) 400L, methyl alcohol 320L, water 80L, mixing in the mixing kettle of 1000L, behind the standing demix, two-phase is separately standby up and down.Above as stationary phase, last flow velocity with 100ml/min pumped into or be pressed into and be full of the host work drum with the air pressure mode.Take by weighing camptothecine crude extract 550 grams,, filter standby with the following phase solution dissolving of 3500mL.As follows embodiment 3.Can get the about 200g of unimolecule camptothecine at last, its HPLC purity is up to more than 98%.
Claims (4)
1. planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device, [little rotatable a plurality of host work drums [3] reach the teflon that links with the work drum and lead in/out pipe [4] to it is characterized in that it having the main frame casing, side of each work drum is also disposing and rotatablely is being used for separating that strand leads in/out pipe separates strand framework [5], lead in/out pipe and separate the strand framework with each work drum and side thereof and be connected in series successively, and draw outside the machine by host center axle [2] at last.Main frame fixed frame [6] connects and the rotation of drive main frame fixed frame with the power output shaft of motor [7], rotating speed of motor can be controlled by frequency-variable controller [8], the bearing of central shaft [11], [12] are located on the main frame fixed frame, direct and the shared toe joint of each drum rotating shaft coaxle gear [16] of working of spigot shaft coaxle gear [15], spigot shaft coaxle gear [17] is separated strand framework rotating shaft coaxle gear [19] with each and is then passed through a carrier gear [18] connection.
2. a kind of planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device according to claim 1 is characterized in that said host work drum configuration quantity is 2～8.
3. a kind of planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device according to claim 1 is characterized in that said work drum adopts polyfluortetraethylene pipe, stainless-steel tube or copper tube multiple wraps.
4. a kind of planetary multi-layer helical pipe centrifugal partition chromatograph instrument tripping device according to claim 1, it is characterized in that under the main frame running status, the angular velocity that the host work that rotates around its central shaft rouses is 2 ω, separates the strand framework and just makes counter-rotation around central shaft by the angular velocity of ω.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100349305A CN1550779A (en) | 2002-03-18 | 2002-03-18 | Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100349305A CN1550779A (en) | 2002-03-18 | 2002-03-18 | Planetary multi-layer helix-tube centrifugal distribution chromatograph separation apparatus |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02111094 Division CN1373131A (en) | 2002-03-18 | 2002-03-18 | Process and apparatus for extracting and separating high-purity monomolecular camptothecine |
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| CN1550779A true CN1550779A (en) | 2004-12-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103987463A (en) * | 2011-09-28 | 2014-08-13 | 动力提取有限公司 | Improvements to centrifuge apparatus. |
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2002
- 2002-03-18 CN CNA2004100349305A patent/CN1550779A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103987463A (en) * | 2011-09-28 | 2014-08-13 | 动力提取有限公司 | Improvements to centrifuge apparatus. |
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