CN105688443B - A kind of chromatogram purification piece-rate system and isolation and purification method - Google Patents
A kind of chromatogram purification piece-rate system and isolation and purification method Download PDFInfo
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- CN105688443B CN105688443B CN201610081486.5A CN201610081486A CN105688443B CN 105688443 B CN105688443 B CN 105688443B CN 201610081486 A CN201610081486 A CN 201610081486A CN 105688443 B CN105688443 B CN 105688443B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
- B01D15/426—Specific type of solvent
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Abstract
The present invention provides a kind of chromatogram purification piece-rate system, and the system includes：First colvent inlet, the first chromatography pump, the first chromatographic column, the first detector, the second colvent inlet, the second chromatography pump, the second chromatographic column, the second detector, the first collection port, the second collection port, the 3rd collection port, the first triple valve, the second triple valve；First colvent inlet connects the entrance of the first chromatographic column by the first chromatography pump；The outlet of first chromatographic column connects the first interface of the first triple valve by the first detector；The second interface of first triple valve connects the first collection port, the first interface of the 3rd the second triple valve of orifice of the first triple valve；The second interface of second triple valve connects the second collection port, the entrance of the 3rd the second chromatographic column of orifice of the second triple valve；Second colvent inlet connects the entrance of the second chromatographic column by the second chromatography pump；The outlet of second chromatographic column connects the 3rd collection port by the second detector.Chromatogram purification piece-rate system of the present invention is simple and easy to do, improves and isolates and purifies effect and separation purity.
Description
Technical field
The present invention relates to preparing chromatograph in industry field, specifically, is related to a kind of chromatogram purification piece-rate system and separation is pure
Change method.
Background technology
The main purpose of preparing chromatograph in industry is that pure material is obtained from mixture, separated more using chromatographic technique,
Collect, to obtain one or more chromatogram pure materials.
At present, the method for traditional chromatographic isolation, comprises the following steps：(1) cleaning balance chromatographic column；(2) dissolving is configured
Good sample injection chromatographic column；(3) switching mobile phase is eluted, and collection prepares spectrogram；(4) target is found on spectrogram is prepared
Start to receive target product after product；(5) product detects the purity of target product after rolling.This traditional chromatography separating method is relatively suitable
Relatively low product is required for easily separated or product quality, but the production that the product or quality requirement for more difficult separation are higher
Product, because purity does not reach defined requirement, this method does not apply to simultaneously.
For such a situation, a kind of scheme that prior art provides is to increase the length of chromatographic column and improve the number of plates.But
The program causes sample residence time in post elongated, and chromatographic peak spreads increasing in post, cross section increase, reduces separation effect
Fruit, and chromatogram column length increase also causes production cost to greatly improve.
Another scheme is to do separating for several times to underproof product.Program technique is relatively complicated, poor for stability
Product, repeatedly post processing may cause product degraded and impurity increase, and cost can also improve.
A kind of it is, thus, sought for more efficiently purifying of product that product or quality requirement for more difficult separation is higher
Piece-rate system.
The content of the invention
In order to overcome above-mentioned technical problem, the invention provides a kind of chromatogram purification piece-rate system, improve and isolate and purify
Effect, technique is simple and cost is relatively low.
The present invention also provides a kind of method isolated and purified using the chromatogram purification piece-rate system.
To achieve these goals, the invention provides a kind of chromatogram purification piece-rate system, including：
First colvent inlet, the first chromatography pump, the first chromatographic column, the first detector, the second colvent inlet, the second chromatography
Pump, the second chromatographic column, the second detector, the first collection port, the second collection port, the 3rd collection port, the first triple valve, the second threeway
Valve；
First colvent inlet connects the entrance of the first chromatographic column by the described first chromatography pump；
The outlet of first chromatographic column connects the first interface of first triple valve by the first detector；
The second interface of first triple valve connects first collection port, and the 3rd interface of first triple valve connects
Lead to the first interface of second triple valve；
The second interface of second triple valve connects second collection port, and the 3rd interface of second triple valve connects
Lead to the entrance of second chromatographic column；
Second colvent inlet connects the entrance of the second chromatographic column by the described second chromatography pump；
The outlet of second chromatographic column connects the 3rd collection port by the second detector.
In a kind of optional embodiment, the system also includes flowmeter, and the flowmeter is connected to described first
Between the first interface of detector and first triple valve.
In a kind of optional embodiment, first colvent inlet is 2 to 5 road entrances, second colvent inlet
For 2 to 5 road entrances.
In a kind of optional embodiment, flow is provided between first colvent inlet and the first chromatography pump
Valve.
In a kind of optional embodiment, flow is provided between second colvent inlet and the second chromatography pump
Valve.
In a kind of optional embodiment, the first chromatography pump and the second chromatography pump be respectively plunger pump or every
Membrane pump.
In a kind of optional embodiment, first chromatographic column and second chromatographic column include post sieve plate, distribution
Device, pressing plate and column jecket, the post sieve plate, the distributor and the pressing plate are bonded successively to be arranged in the column jecket.
In a kind of optional embodiment, the post sieve plate includes sieve plate seat, several deck units；
The sieve plate seat is provided with that some shapes are identical and the through hole of equidistantly distributed, several described deck units and institute
State through hole to be engaged, be placed in the through hole.
Present invention also offers a kind of method isolated and purified using above-mentioned chromatogram purification piece-rate system, including it is as follows
Step：
1) the first chromatographic column is first injected a sample into；
2) elution mobile phase is pumped into the first chromatographic column by the first chromatography pump through the first colvent inlet again, proceeds by and wash
It is de-, and record-keeping system is for one-dimensional spectrogram；
3) the first triple valve opens first interface and second interface, closes the 3rd interface, and preceding miscellaneous Fraction collection enters first
Collection port；
4) when there are target components during record-keeping system is for spectrogram, the first triple valve is subjected to switch switching, second is closed and connects
Mouthful, the 3rd interface is opened, and the first interface and the 3rd interface of the second triple valve are opened, close the second triple valve second connects
Mouthful, the first chromatographic column connects with the second chromatographic column, and target components are transported to the second chromatographic column, and record-keeping system is for the second spectrogram；
5) terminate when the first detector detects target components, when rear miscellaneous component occurs, close the 3rd of the second triple valve
Interface, the connection between the first chromatographic column and the second chromatographic column is disconnected, and open first, second interface of the second triple valve, will
Miscellaneous component inputs the second collection port afterwards；
6) while by elution mobile phase by the second chromatography infusion enter the second chromatographic column, carry out two dimensional separation purifying, will be pure
Target components after change are received into the 3rd collection port.
In a kind of optional embodiment, before being isolated and purified and after isolating and purifying, to the first chromatographic column and the
Two chromatographic columns are cleaned respectively and Balance Treatment.
Chromatogram purification piece-rate system described in the embodiment of the present invention, including the first colvent inlet, the first chromatography pump, the first color
Compose post, the first detector, the second colvent inlet, the second chromatography pump, the second chromatographic column, the second detector, the first collection port, second
Collection port, the 3rd collection port, the first triple valve, the second triple valve.First colvent inlet connects the first color by the first chromatography pump
Compose the entrance of post；The outlet of first chromatographic column connects the first interface of the first triple valve, the first triple valve by the first detector
Second interface connect the first collection port, the first interface of the 3rd the second triple valve of orifice of the first triple valve, the two or three
The second interface of port valve connects the second collection port, and the entrance of the 3rd the second chromatographic column of orifice of the second triple valve, second is molten
Agent entrance connects the entrance of the second chromatographic column by the second chromatography pump, and the outlet of the second chromatographic column connects institute by the second detector
State the 3rd collection port.Chromatogram purification piece-rate system of the present invention and isolation and purification method improve the product of more difficult separation or quality will
The separation purity of higher product is sought, product yield is high, and technique is simple, easy to control, and cost is relatively low, is protected more suitable for object
Stay the impurity separation that the time is nearer.
Brief description of the drawings
Fig. 1 is the structural representation of chromatogram purification piece-rate system provided in an embodiment of the present invention；
Fig. 2 is chromatographic column structure figure provided in an embodiment of the present invention；
Fig. 3 is the structure chart of post sieve plate provided in an embodiment of the present invention；
Fig. 4 a are the chromatogram isolated and purified using existing chromatogram purification piece-rate system to sample；
Fig. 4 b are the product chromatogram after being isolated and purified using existing chromatogram purification piece-rate system to sample；
Fig. 5 a are one-dimensional chromatogram when being isolated and purified using chromatogram purification piece-rate system of the present invention to sample；
Fig. 5 b are two-dimensional chromatogram when being isolated and purified using chromatogram purification piece-rate system of the present invention to sample；
Fig. 5 c are the product chromatogram after being isolated and purified using chromatogram purification piece-rate system of the present invention to sample；
Fig. 6 is the partial structural diagram of chromatogram purification piece-rate system provided in an embodiment of the present invention.
Embodiment
Below with reference to the accompanying drawings embodiments of the invention are illustrated.Retouched in the accompanying drawing of the present invention or a kind of embodiment
The element and feature that the element and feature stated can be shown in one or more other accompanying drawings or embodiment are combined.Should
Work as attention, for purposes of clarity, eliminated in accompanying drawing and explanation known to unrelated to the invention, those of ordinary skill in the art
Part or processing expression and description.
The present invention is described further below in conjunction with the accompanying drawings.
The embodiments of the invention provide a kind of chromatogram purification piece-rate system, as shown in figure 1, the system includes：First solvent
Entrance 101, first chromatographs pump 102, the first chromatographic column 103, the first detector 104, the second colvent inlet 105, second chromatography pump
106th, the second chromatographic column 107, the second detector 108, the first collection port 109, the second collection port 110, the 3rd collection port 111,
One triple valve 112, the second triple valve 113.
First colvent inlet 101 connects the entrance of the first chromatographic column 103 by the first chromatography pump 102.
The outlet of first chromatographic column 103 connects the first interface of the first triple valve 112 by the first detector.
The second interface of first triple valve 112 connects the first collection port 109, the 3rd orifice of the first triple valve 112
The first interface of second triple valve 113.
The second interface of second triple valve 113 connects the second collection port 110, the 3rd orifice of the second triple valve 113
The entrance of second chromatographic column 107.
Second colvent inlet 105 connects the entrance of the second chromatographic column 107 by the second chromatography pump 106.
The outlet of second chromatographic column 107 connects the 3rd collection port 111 by the second detector 108.
Optionally, the system also includes flowmeter 114, and flowmeter 114 is connected to the first detector and the first triple valve 112
First interface between.Flowmeter 114 is used to detect flow rate of liquid, can be specifically mass flowmenter, volume flowmeter etc..
First colvent inlet 101 is specifically as follows 2 to 5 road entrances, and 3 road entrances are shown as in Fig. 1.Second colvent inlet 105
For 2 to 5 road entrances, 3 road entrances are shown as in Fig. 1.Each entrance institute in the first colvent inlet 101, the second solution inlet 105
Path on valve is set, by valve regulated from every road entrance inject chromatographic column liquid inventory.
Figure 6 illustrates the annexation of the first triple valve, each interface of the second triple valve.Wherein the first triple valve
There are three interfaces, respectively first interface 1121, second interface 1122, the 3rd interface 1123.Second triple valve has three interfaces,
Respectively first interface 1131, second interface 1132, the 3rd interface 1133.
The connection flow gauge 114 of first interface 1121 of first triple valve, second interface 1122 connect the first collection port 109,
3rd interface 1123 connects the first interface 1131 of the second triple valve.The connection of second interface 1,132 second of second triple valve is collected
Mouth 110, the 3rd interface 1133 connect the second chromatographic column 107.
Optionally, it can be specifically plunger pump or membrane pump that the first chromatography pump 102 and second, which chromatographs pump 106, be not limited to one
Platform is used, and more chromatography pumps can be set to be used cooperatively on path.Chromatograph pump flow can 10ml/min to 100L/min it
Between change, pressure highest tolerance 20MPa.
Optionally, the first chromatographic column 103 can be high-pressure chromatographic column or mesolow chromatographic column.
Product stream artificial situation of first monitoring in real time of detector 104 after the separation of the first chromatographic column 103, optionally, the
One detector 104 can be UV-detector, electric conductivity detector, PH detector, shunting connection differential refraction detector, evaporative light
Scatter detector etc..Pressure highest is resistant to 20MPa.
The process that overall purifies and separates are carried out using chromatogram purification piece-rate system of the present invention is as follows：
1) the first chromatographic column is first injected a sample into；
2) elution mobile phase is pumped into the first chromatographic column by the first chromatography pump through the first colvent inlet again, proceeds by and wash
It is de-, and record-keeping system is for one-dimensional spectrogram；
3) the first triple valve opens first interface and second interface, closes the 3rd interface, and preceding miscellaneous Fraction collection enters first
Collection port；
4) when there are target components during record-keeping system is for spectrogram, the first triple valve is subjected to switch switching, second is closed and connects
Mouthful, the 3rd interface is opened, and the first interface and the 3rd interface of the second triple valve are opened, close the second triple valve second connects
Mouthful, the first chromatographic column connects with the second chromatographic column, and target components are transported to the second chromatographic column, and record-keeping system is for the second spectrogram；
5) terminate when the first detector detects target components, when rear miscellaneous component occurs, close the 3rd of the second triple valve
Interface, the connection between the first chromatographic column and the second chromatographic column is disconnected, and open first, second interface of the second triple valve, will
Miscellaneous component inputs the second collection port afterwards；
6) while by elution mobile phase by the second chromatography infusion enter the second chromatographic column, carry out two dimensional separation purifying, will be pure
Target components after change are received into the 3rd collection port.
Specifically, as shown in figure 1, the method for the purifies and separates, comprises the following steps：
(1) cleaning balance is carried out to the first chromatographic column 103 and the second chromatographic column 107 first.
By the switching of the valve on the multientry path of the first colvent inlet and the second colvent inlet, can select not
Same solvent carries out sample introduction, elution, balance, cleaning etc. and operated.
(2) inject a sample into the first chromatographic column 103.
(3) solvent (mobile phase) of first colvent inlet 101 and then using the first chromatography pump 102 is pumped into the first chromatographic column
103.First chromatographic column 103 is eluted, and record-keeping system is for spectrogram.
Now the first triple valve 112 opens first interface and second interface, closes the 3rd interface, the first chromatographic column 103 with
First collection port 109 communicates.Preceding miscellaneous component is taken in the first collection port 109.
(4) when finding target components on preparing spectrogram, start to receive target components.
When the first detector 104 detects the first flex point, i.e., when target components occur, the first triple valve 112 is opened
Concern is changed, and closes its second interface, opens the 3rd interface, and opens the first interface and the 3rd interface of the second triple valve 113, is closed
The second interface of the second triple valve 113 is closed, the first chromatographic column 103 communicates with the second chromatographic column 107, and target components are transported to
Two chromatographic columns 107.
(5) when the first detector 104 detects target components Second Inflexion Point, i.e., target components terminate, rear miscellaneous component occurs
When, mobile phase is injected into the second chromatographic column 107 by the second chromatography pump 106 from the second colvent inlet 105, target components are carried out
Two dimension purifying.
A two-port valve can be connected on the path of second chromatography pump 106 to the second chromatographic column 107, opens the two-port valve, liquid
Body is pumped into the second chromatographic column 107.
Meanwhile the 3rd interface of the second triple valve 113 is closed, first, second interface of the second triple valve 113 is opened, is made
First chromatographic column 103 is communicated with the second collection port 110, and rear miscellaneous component is inputted into the second collection port 110.
(6) the first chromatographic column of cleaning and regeneration 103.And product is detected by the second detector 108, after product is detected,
Product is received into the 3rd collection port 111.
In actual scene, in order to improve efficiency, the chromatographic column of cleaning and regeneration first and reception two processes of product are entered simultaneously
OK.
(7) the second chromatographic column 107 is cleaned after product finishes receiving.
Optionally, the first chromatographic column of the chromatogram purification piece-rate system and the second chromatographic column include post sieve plate, distributor, pressure
Plate and column jecket.It is arranged on as shown in Fig. 2 post sieve plate 21, distributor 22 and pressing plate 23 are bonded successively in column jecket 24.Positioned at column jecket 24
The pressing plate 23 of bottom is further secured on blind flange 25.
As shown in figure 3, post sieve plate includes sieve plate seat 31, several deck units 32.Sieve plate seat 31 is provided with some shapes
Identical and equidistantly distributed through hole, several deck units 32 are engaged with through hole, are placed in through hole.Such a structure it is whole
The entirety that deck unit and sieve plate seat are formed has more preferable intensity.
Below by taking a kind of active ingredient product of taxanes plant extracts as an example, to traditional chromatographic fractionation system and this
The effect for the chromatogram purification piece-rate system that inventive embodiments provide is compared.
The active ingredient of the plant extracts is a kind of anticancer preparation raw material, and to some specific cancers, (such as non-leaflet is thin
Born of the same parents' lung cancer) there is good effect, its content in plant is relatively low, and extraction and purifying difficulty are larger, and listing pharmacopoeial requirements at initial stage are pure
Degree is more than 97%, but is found by clinic for many years and laboratory research contrast, wherein the impurity level contained crosses conference production
Raw very big clinical side effects, reduce curative effect of medication.In order to obtain more preferable therapeutic effect, the pharmacopeia purity requirement of the product from
97% has brought up to 98.5%, and inner controlling standard of enterprise is even more to improve to 99.5%.Using the Plant Extracts as treating point
From purification of samples, sample has been subjected to the plant extract and simple process of early stage, and the purity of target product in the sample is 56%, point
It is that product purity reaches more than 99.5% from purification of target.
Comparative example：
Purifies and separates, including following step are carried out to the plant extracts active ingredient product using traditional chromatographic fractionation system
Suddenly：
1) first cleaning balances chromatographic column, and chromatographic column specification is chromatographic column specification ID200x650mm, loads 5 kilograms 10 microns
Octadecylsilane chemically bonded silica filler, use 20L methanol：Water=50：50 (v/v) cleaning balances；
2) 1L methanol will be added with 0.1 kilogram of extract crude product：Water=80:20 (v/v) solution, sample passed through after dissolving
After filter, chromatographic column is injected；
3) and then switching mobile phase carries out gradient elution, and eluting order is first to be pumped into 40L methanol：Water=40：60 (v/v),
60L methanol is pumped into again：Water=52：48 (v/v), collection prepare spectrogram (as shown in fig. 4 a)；
4) start to receive target product after finding target product (shown in Fig. 4 a at 90min) on spectrogram is prepared；
5) product after rolling (92min peaks shown in Fig. 4 a) detection target product purity, as shown in Figure 4 b, through efficient liquid phase
Chromatography (High Performance Liquid Chromatography, HPLC) detection collected by target product purity be
97.2%.
Experimental example：
Purifies and separates, including following step are carried out to the Plant Extracts product using chromatogram purification piece-rate system of the present invention
Suddenly：
1) 5 kilograms of 20 microns of octadecyl silicon are loaded to the first chromatographic column 103 (chromatographic column specification ID200x650mm) first
Alkane bonded silica gel filler simultaneously loads 5 kilograms of 20 microns of octadecyls to the second chromatographic column 107 (chromatographic column specification ID200x650mm)
Silane group silica filler, respectively using 20L methanol：Water=50：50 (v/v) solvents are carried out to the first chromatographic column and the second chromatographic column
Cleaning balance.
2) 0.25 kilogram of extract crude product is added into 1L methanol：Water=80:20 (v/v) solution, sample passed through after dissolving
After filter, inject in the first chromatographic column 103.
3) and then using first pump 102 is chromatographed by the methanol configured of the first colvent inlet 101：Water=50:50(v/v)
Solvent (mobile phase) is pumped into the first chromatographic column 103.First chromatographic column 103 is eluted, and record-keeping system is for spectrogram (such as Fig. 5 a).
Now the first triple valve 112 opens first interface and second interface, closes the 3rd interface, the first chromatographic column 103 with
First collection port 109 communicates.Preceding miscellaneous component is taken in the first collection port 109.
4) when finding target components on preparing spectrogram, start to receive target components.
When the first detector 104 detects the first flex point (see shown in Fig. 5 a), i.e., when target components occur, to the first threeway
Valve 112 carries out switch switching, closes its second interface, opens the 3rd interface, and open the second triple valve 113 first interface and
3rd interface, the second interface of the second triple valve 113 is closed, the first chromatographic column 103 communicates with the second chromatographic column 107, target group
Divide and be transported to the second chromatographic column 107, record-keeping system is for two-dimentional spectrogram (such as Fig. 5 b).
5) when the first detector 104 detects target components Second Inflexion Point (see shown in Fig. 5 a), i.e., target components terminate, after
When miscellaneous component occurs, mobile phase is injected into the second chromatographic column 107 from the second colvent inlet 105 by the second chromatography pump 106, to mesh
Mark component and carry out two-dimentional purifying.
A two-port valve can be connected on the path of second chromatography pump 106 to the second chromatographic column 107, opens the two-port valve, liquid
Body is pumped into the second chromatographic column 107.
Meanwhile the 3rd interface of the second triple valve 113 is closed, first, second interface of the second triple valve 113 is opened, is made
First chromatographic column 103 is communicated with the second collection port 110, and rear miscellaneous component is inputted into the second collection port 110.
6) the first chromatographic column of cleaning and regeneration 103.And product is detected by the second detector 108, will after product is detected
Product is received into the 3rd collection port 111.
7) the second chromatographic column 107 is cleaned after product finishes receiving.
Detected through high performance liquid chromatography (High Performance Liquid Chromatography, HPLC), such as
Shown in Fig. 5 c, the purity of target component product is up to 99.93%.
Chromatogram purification piece-rate system described in the embodiment of the present invention and the method isolated and purified, improve the production of more difficult separation
The separation purity of product or the higher product of quality requirement, the system integrated artistic is simple and easy to control, while cost is relatively low.
Although the present invention and its advantage is described in detail it should be appreciated that without departing from by appended claim
Various changes, replacement and conversion can be carried out in the case of the spirit and scope of the present invention limited.Moreover, the model of the application
Enclose the process described by specification of being not limited only to, equipment, means, the specific embodiment of method and steps.In the art is common
Technical staff will readily appreciate that from the disclosure, can be used and performed and corresponding reality described herein according to the present invention
Apply the essentially identical function of example or obtain process essentially identical with it result, existing and that future is to be developed, equipment,
Means, method or step.Therefore, appended claim includes such process, equipment, hand in the range of being directed at them
Section, method or step.
Claims (8)
- A kind of 1. chromatogram purification piece-rate system, it is characterised in that including：First colvent inlet, the first chromatography pump, the first chromatographic column, the first detector, the second colvent inlet, the second chromatography pump, the Two chromatographic columns, the second detector, the first collection port, the second collection port, the 3rd collection port, the first triple valve, the second triple valve；First colvent inlet connects the entrance of first chromatographic column by the described first chromatography pump；The outlet of first chromatographic column connects the first interface of first triple valve by first detector；The second interface of first triple valve connects first collection port, the 3rd orifice institute of first triple valve State the first interface of the second triple valve；The second interface of second triple valve connects second collection port, the 3rd orifice institute of second triple valve State the entrance of the second chromatographic column；Second colvent inlet connects the entrance of second chromatographic column by the described second chromatography pump；The outlet of second chromatographic column connects the 3rd collection port by second detector；The system also includes flowmeter, and the flowmeter is connected to the first of first detector and first triple valve Between interface；First chromatographic column and second chromatographic column include post sieve plate, distributor, pressing plate and column jecket, the post sieve respectively Plate, the distributor and the pressing plate are bonded successively to be arranged in the column jecket.
- 2. chromatogram purification piece-rate system according to claim 1, it is characterised in that first colvent inlet is 2 to 5 tunnels Entrance, second colvent inlet are 2 to 5 road entrances.
- 3. chromatogram purification piece-rate system according to claim 1, it is characterised in that first colvent inlet and described the Flow valve is provided between one chromatography pump.
- 4. chromatogram purification piece-rate system according to claim 1, it is characterised in that second colvent inlet and described the Flow valve is provided between two chromatography pumps.
- 5. chromatogram purification piece-rate system according to claim 1, it is characterised in that the first chromatography pump and described second It is respectively plunger pump or membrane pump to chromatograph pump.
- 6. chromatogram purification piece-rate system according to claim 1, it is characterised in that the post sieve plate includes sieve plate seat, if Dry deck unit；The sieve plate seat is identical provided with some shapes and the through hole of equidistantly distributed, several described deck units lead to described Hole is engaged, and is placed in the through hole.
- 7. the method isolated and purified using the chromatogram purification piece-rate system described in claim 1-6 any one, its feature It is, comprises the following steps：1) the first chromatographic column is first injected a sample into；2) elution mobile phase is pumped into the first chromatographic column by the first chromatography pump through the first colvent inlet again, proceeds by elution, And record-keeping system is for one-dimensional spectrogram；3) the first triple valve opens first interface and second interface, closes the 3rd interface, and preceding miscellaneous Fraction collection enters first and collected Mouthful；4) when there are target components during record-keeping system is for spectrogram, the first triple valve is subjected to switch switching, second interface is closed, opens The 3rd interface is opened, and opens the first interface and the 3rd interface of the second triple valve, the second interface of the second triple valve of closing, first Chromatographic column connects with the second chromatographic column, and target components are transported to the second chromatographic column, and record-keeping system is for the second spectrogram；5) terminate when the first detector detects target components, when rear miscellaneous component occurs, close the 3rd interface of the second triple valve, The connection between the first chromatographic column and the second chromatographic column is disconnected, and opens first, second interface of the second triple valve, by latter miscellaneous group Divide input the second collection port；6) while by elution mobile phase by the second chromatography infusion enter the second chromatographic column, carry out two dimensional separation purifying, will after purification Target components receive into the 3rd collection port.
- 8. isolation and purification method according to claim 7, it is characterised in that before being isolated and purified and isolate and purify Afterwards, to the first chromatographic column and the second chromatographic column is cleaned respectively and Balance Treatment.
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| CN109917035B (en) * | 2019-03-22 | 2022-02-18 | 肖传绪 | Elution device with pressure drop measurement function and application thereof |
| WO2020258706A1 (en) * | 2019-06-28 | 2020-12-30 | 信达生物制药(苏州)有限公司 | Combined chromatography apparatus, seamless connection chromatography method, and biological agent purification method |
| CN115015458A (en) * | 2022-07-01 | 2022-09-06 | 江苏汉邦科技股份有限公司 | Split-flow chromatography system and method for preparing ethyl eicosapentaenoate by using split-flow chromatography system |
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| US5071547A (en) * | 1990-03-23 | 1991-12-10 | Separations Technology, Inc. | Column chromatographic column apparatus with switching capability |
| CN203108263U (en) * | 2013-03-19 | 2013-08-07 | 利穗科技(苏州)有限公司 | Double column circulating chromatographic system |
| CN204073503U (en) * | 2014-09-18 | 2015-01-07 | 北京佰纯润宇生物科技有限公司 | The multicolumn shunt layer analysis system of bypass and positive reflux is realized based on cross valve and twin columns valve |
| CN204405612U (en) * | 2015-02-11 | 2015-06-17 | 王峰 | A kind of liquid chromatograph |
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