CN214150580U - Liquid chromatographic column maintenance device - Google Patents
Liquid chromatographic column maintenance device Download PDFInfo
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- CN214150580U CN214150580U CN202023291458.7U CN202023291458U CN214150580U CN 214150580 U CN214150580 U CN 214150580U CN 202023291458 U CN202023291458 U CN 202023291458U CN 214150580 U CN214150580 U CN 214150580U
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Abstract
The invention relates to a liquid chromatographic column maintenance device which comprises a solvent selection valve, a peristaltic pump, a two-way electromagnetic valve, a three-way electromagnetic valve, a controller, a buffer container, a magnetic stirrer, a magnetic stirring device, an ultrasonic module, a filter element, a liquid discharge valve, a high-pressure pump, a chromatographic column selection valve, a column incubator, a waste liquid receiving barrel, a liquid level sensor (buffer container) and a liquid level sensor (waste liquid receiving barrel). The liquid chromatographic column maintenance device can automatically wash a plurality of liquid chromatographic columns by using a stock solvent without connecting a liquid chromatograph, saves chromatograph resources, can remotely control to close the washing of the chromatographic columns and remotely control to open the balance of the chromatographic columns, and improves the working efficiency.
Description
Technical Field
The invention relates to a chromatographic column maintenance device, belongs to the fields of medicines, foods and chemistry, and particularly relates to a liquid chromatographic column maintenance device.
Background
A High Performance Liquid Chromatograph (HPLC) is an instrument and equipment which applies the principle of high performance liquid chromatography and is mainly used for analyzing organic compounds with high boiling points, difficult volatilization, unstable heating and large molecular weight. It is composed of liquid storage, pump, mixer, sample injector, chromatographic column, detector and recorder. The mobile phase in the liquid storage device is pumped into the system by a high-pressure pump through a mixer, the sample solution enters the mobile phase through a sample injector and is loaded into a chromatographic column (stationary phase) by the mobile phase, and because each component in the sample solution has different distribution coefficients in two phases, when the two phases do relative motion, through repeated adsorption-desorption distribution processes, each component generates a large difference in moving speed, is separated into single components and sequentially flows out of the column, when the sample passes through a detector, the concentration of the sample is converted into an electric signal and is transmitted to a recorder, and data is printed in a graph form. HPLC is widely used in life sciences, food sciences, pharmaceutical research, and environmental research.
The chromatographic column is used as a core component for liquid chromatography, and is expensive, so that the correct use and maintenance of the chromatographic column are very important, and the column efficiency is reduced, the service life is shortened and even the chromatographic column is damaged.
The particle size range of the filler particles of the chromatographic column widely used at present is 3-10 mu m, the pore size is 6-10 nm, a large amount of mobile phase can pass through the chromatographic column in the using process, if the mobile phase or a sample contains trace insoluble impurity particles, the particles can be easily intercepted at the column head part, the mechanical blockage of the chromatographic column can be caused as time passes, and the column pressure is increased. When the aqueous solution is used as a mobile phase or contains a certain concentration of phosphate buffer solution in the mobile phase, some bacteria or molds can grow in the aqueous solution or the phosphate solution, so that the gaps among the stationary phase particles of the chromatographic column are blocked. Furthermore, the sample may contain various components or impurities other than the component to be analyzed (particularly for traditional Chinese medicine analysis), and these components or impurities may cause irreversible adsorption in the column, thereby, the active sites of the stationary phase are covered, and the retention characteristics of the chromatographic column are changed.
Therefore, the chromatographic column needs to be properly and timely washed and maintained after being used, and a plurality of washing media are frequently required to be replaced during washing, for example, when a mobile phase containing buffer salt is used in the use process of the chromatographic column, a solution which has the same composition as the mobile phase for analysis and does not contain the buffer salt needs to be firstly used for washing, and then the washing is gradually transited to pure methanol or pure acetonitrile. Isopropanol is the only reagent miscible with various solvents, has good solubility for many substances and also has a certain solubility for inorganic salts, so that sometimes it is often necessary to wash the column with isopropanol at a low flow rate to restore the column performance. The mixed solution of tetrahydrofuran and acetonitrile or methanol can remove lipids. Protein contamination was removed by rinsing with acetonitrile, acetone and trifluoroacetic acid (0.1%). It is also sometimes often necessary to wash the column with a strong solvent to remove impurities remaining in the column and regenerate the column. The silica gel column is washed by n-hexane, dichloromethane and methanol in sequence, and then washed by the reverse sequence, the methanol can wash away residual strong polar impurities, and the n-hexane can reactivate the surface of the silica gel. The reverse phase column was washed with water, methanol, acetonitrile, and methyl chloride (or chloroform) in this order, and then washed in the reverse order. The cation exchange column can be washed by dilute acid buffer solution, the anion exchange column can be washed by dilute alkali buffer solution to remove salts with strong exchange performance, and then water, methanol, dichloromethane (to remove organic matters adsorbed on the surface of the stationary phase), methanol and water are sequentially washed.
In summary, the maintenance of the chromatographic column is a complicated process, and often requires the replacement of various solvents, while the liquid chromatograph is usually equipped with at most 4 pumps and can select at most 4 mobile phases, so that the solvent in the mobile phase bottle often needs to be replaced manually during washing, the operation is cumbersome, and unattended operation cannot be achieved, for example, the mobile phases before and after replacement are not dissolved, and precipitation and blockage of the apparatus can be caused. In addition, the washing process often needs 1-2 hours, if a high performance liquid chromatograph is used for washing, expensive liquid chromatograph resources need to be occupied, and the chromatographic column can be replaced to analyze the next batch of samples after the washing is finished, so that the working efficiency is low.
Patent application No. 201410608204.3 provides an intelligence automatic switch-over multichannel liquid chromatography column connecting device, but it still needs to connect and occupies liquid chromatograph, does not solve the problem that needs a plurality of solvents to wash simultaneously.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a liquid chromatography column maintenance apparatus, which can flush a plurality of chromatography columns in a set sequence according to a set flushing program, is frequently provided with a plurality of commonly used flushing solvents, and can liberate resources of a plurality of high performance liquid spectrometers without replacing the solvents during flushing, so that a next batch of samples can be analyzed without waiting for completion of flushing, and meanwhile, unattended flushing can be performed by remote control, the chromatography columns can be automatically flushed and maintained and remotely closed after work is completed every day, and mobile phase balance can be remotely performed before work is started every day, thereby greatly saving time required for balancing the chromatography columns and flushing the chromatography columns every day, and improving work efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a liquid chromatographic column maintenance device comprises a solvent selection valve, a peristaltic pump, a buffer container, a high-pressure pump and a chromatographic column selection valve, wherein the solvent selection valve selects one branch of a plurality of solvent branches, the peristaltic pump extracts a certain volume of solvent from the selected solvent branch, a single solvent or a mixed solvent of a plurality of solvents is formed in the buffer container and is used as a flushing solvent, the chromatographic column selection valve selects the chromatographic column branch needing to be flushed, and the high-pressure pump pumps the flushing solvent into the selected chromatographic column branch to flush a chromatographic column; further comprising: a controller for washing the chromatography column according to a user set washing program.
Preferably, the liquid chromatography column maintenance device further comprises a three-way electromagnetic valve, the three-way electromagnetic valve is arranged between the peristaltic pump and the buffer container, when the solvent is replaced, the pipeline can be rinsed, and the rinsing is directly discharged into the waste liquid.
Preferably, the liquid chromatography column maintenance device further comprises a two-way electromagnetic valve, the two-way electromagnetic valve is arranged on a branch between the peristaltic pump and the three-way electromagnetic valve, and the liquid chromatography column maintenance device can be used together, so that each liquid chromatography column maintenance device can extract the solvent of other liquid chromatography column maintenance devices for washing, and the solvent can be selected to be many by expanding the way.
Preferably, the liquid chromatography column maintenance device further comprises a magnetic stirrer and a magnetic stirring device, which are arranged on the buffer container and can uniformly mix the solvent in the buffer container.
Preferably, the liquid chromatography column maintenance device further comprises an ultrasonic module, which is arranged on the buffer container and can perform ultrasonic degassing on the solvent in the buffer container.
Preferably, the liquid chromatography column maintenance device further comprises a drain valve disposed on the buffer container and capable of draining the solvent in the buffer container.
Preferably, the liquid chromatography column maintenance device further comprises a heat preservation module arranged on the chromatography column, and the heat preservation module can preserve heat of the chromatography column so as to improve the washing effect when needed.
Preferably, the liquid chromatography column maintenance device further comprises a liquid level sensor arranged on the buffer container, when the liquid level sensor feeds back that the liquid in the buffer container is too little to the controller, the controller stops pumping the high-pressure pump to avoid pumping air, protect the chromatography column, and simultaneously give out early warning of insufficient solvent to a user.
Preferably, liquid chromatography column maintenance device still includes another level sensor, sets up on the waste liquid receiving bucket, and the waste liquid is close when full when receiving in the bucket to the waste liquid and makes the early warning to avoid the waste liquid to spill over and cause the pollution.
Preferably, for performing a single solvent wash, the liquid chromatography column maintenance device performs the wash according to the following wash procedure: the controller controls the solvent selection valve to select a selected solvent branch, controls the three-way electromagnetic valve to be communicated with the waste liquid receiving barrel, starts the peristaltic pump to perform rinsing, stops the peristaltic pump, controls the three-way electromagnetic valve to be communicated with the buffer container, starts the peristaltic pump to pump a certain volume of the selected solvent, starts the magnetic stirring device to perform stirring rinsing, stops stirring, opens the liquid discharge valve to discharge rinsing liquid into the waste liquid receiving barrel, closes the liquid discharge valve, pumps the solvent with a set volume, starts ultrasonic degassing for a set time, closes the ultrasonic module, selects a chromatographic column branch needing rinsing through the chromatographic column selection valve, starts the high-pressure pump to perform rinsing according to a set flow rate, and closes the high-pressure pump after rinsing is completed.
Preferably, for performing a mixed solvent wash of a plurality of solvent compositions, the liquid chromatography column maintenance device performs the wash according to the following wash procedure: the controller controls the solvent selection valve to select one of the selected solvent branches, controls the three-way electromagnetic valve to be communicated with the waste liquid receiving barrel, starts the peristaltic pump to perform rinsing, stops the peristaltic pump, controls the three-way electromagnetic valve to be communicated with the buffer container, starts the peristaltic pump to pump a certain volume of the selected solvent, starts the magnetic stirring device to perform stirring rinsing, stops stirring, opens the liquid discharge valve to discharge rinsing liquid into the waste liquid receiving barrel, closes the liquid discharge valve, pumps the set volume of the solvent, controls the solvent selection valve to select another one of the selected solvent branches, controls the three-way electromagnetic valve to be communicated with the waste liquid receiving barrel, starts the peristaltic pump to perform rinsing, stops the peristaltic pump, controls the three-way electromagnetic valve to be communicated with the buffer container, starts the peristaltic pump to pump a certain volume of the selected solvent, and repeatedly pumps all the selected solvents with the required volume, and starts the magnetic stirring device to perform stirring and mixing, stopping stirring, starting ultrasonic degassing for a set time, closing the ultrasonic module, selecting a chromatographic column branch needing to be washed by a chromatographic column selection valve, starting a high-pressure pump to wash at a set flow rate, and closing the high-pressure pump after washing is finished.
Has the advantages that:
(1) the invention can automatically wash a plurality of chromatographic columns by selecting a plurality of solvents according to a user setting program, can prepare a plurality of commonly used solvents for washing, does not need to replace the solvents manually during washing, and avoids the damage of the chromatographic columns and even the chromatograph caused by possible incompatibility during solvent replacement.
(2) The invention can execute the flushing program without a liquid chromatograph, thereby saving chromatograph resources.
(3) The invention can carry out unattended operation chromatographic column washing after use, remotely control and close, remotely control and open unattended operation chromatographic column balance before use, and save working time.
(4) The invention can be used in combination of multiple units, and each unit can use the stock solvents of other units after combination, thereby greatly expanding the variety of the stock solvents.
Drawings
FIG. 1 is a schematic view of a liquid chromatography column maintenance apparatus according to an embodiment of the present invention.
In the figure: 1. solvent bottle 1, 2, solvent bottle n, 3, solvent selection valve, 4, peristaltic pump, 5, two-way solenoid valve, 6, to another liquid chromatography column maintenance device, 7, three-way solenoid valve, 8, controller, 9, buffer container, 10, magnetic stirrer, 11, magnetic stirring device, 12, ultrasonic module, 13, filter element, 14, liquid level sensor (buffer container), 15, liquid discharge valve, 16, high pressure pump, 17, chromatography column selection valve, 18, chromatography column 1, 19, chromatography column n, 20, column incubator 1, 21, column incubator n, 22, waste liquid receiving barrel, 23, liquid level sensor (waste liquid receiving barrel).
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The first embodiment is as follows:
as shown in fig. 1, a liquid chromatography column maintenance device comprises a solvent bottle, a solvent selection valve, a peristaltic pump, a two-way solenoid valve, a three-way solenoid valve, a controller, a buffer container, a magnetic stirrer, a magnetic stirring device, an ultrasonic module, a filter element, a drain valve, a high-pressure pump, a chromatography column selection valve, a column incubator, a waste liquid receiving tank, a liquid level sensor (buffer container), and a liquid level sensor (waste liquid receiving tank).
The solvent bottle deposits various solvents for washing, one branch road in a plurality of solvent branch roads is selected to the solvent selector valve, the peristaltic pump provides the power of pumping solvent, the two-way solenoid valve is used for being connected to another chromatographic column maintenance device to ally oneself with, three-way solenoid valve one end is connected to the waste liquid and receives the bucket for rinse the pipeline, and one end is connected to buffer container for pump into buffer container with solution, buffer container is used for depositing the washing solvent, magnetic stirrers and magnetic stirring device are used for carrying out the mixing to the solvent in the buffer container, the supersound module is used for the ultrasonic degassing of buffer container internal solvent, the filter core is used for filtering the washing solvent, the flowing back valve is used for emptying the surplus solution in the buffer container, the high-pressure pump provides the power of pumping the chromatographic column with washing solvent, chromatographic column selector valve selects a branch road in a plurality of chromatographic column branches of waiting to wash, the column incubator is used for preserving heat of the chromatographic column, and the waste liquid receiving barrel is used for receiving the washed waste liquid and the rinsed waste liquid.
In order to control the processing flow of the liquid chromatographic column maintenance device, the liquid chromatographic column maintenance device is provided with a controller which can be a PLC or a single chip microcomputer and is used for storing and executing a washing program set by a user, such as the volume of a washing solvent pipeline, the type of a washing solvent, the volume, the stirring speed, the stirring time, the ultrasonic time, the washing speed, the column temperature and the like, and can be communicated with the controller of another liquid chromatographic column maintenance device so as to realize the linkage of a plurality of liquid chromatographic column maintenance devices.
The controller may store sequences of washing programs, each sequence executing a set washing program for one chromatography column, and in the washing process, a user may insert a sequence after the sequence is currently run and before the sequence is not run, or delete a certain sequence which is not run, so that washing is executed according to the sequence set by the user.
The controller stops the pump when the liquid level sensor (buffer container) detects that the flushing solvent in the buffer container is too little, so that air pumping is avoided, the chromatographic column is protected, and a solvent quantity shortage alarm is given to a user.
The controller gives an early warning to a user when the liquid level sensor (the waste liquid receiving barrel) detects that liquid in the waste liquid receiving barrel is close to full, prompts the user to timely treat the liquid in the waste liquid receiving barrel, and avoids overflowing.
Claims (10)
1. A liquid chromatographic column maintenance device comprises a solvent selection valve, a peristaltic pump, a buffer container, a high-pressure pump and a chromatographic column selection valve, wherein a port of the solvent selection valve is connected with a plurality of solvent branches, one branch of the solvent branches is selected, the peristaltic pump is connected with the solvent selection valve and provides power for pumping a solvent, the buffer container is connected with the peristaltic pump and is used for storing a flushing solvent, the high-pressure pump is connected with the buffer container and pumps the solvent from the buffer container and provides power for pumping the flushing solvent into a chromatographic column, and the chromatographic column selection valve is connected with the high-pressure pump and selects one branch of the solvent branches; the method is characterized in that: this liquid chromatography column maintenance device still includes: a controller for controlling the rinsing process.
2. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a three-way electromagnetic valve arranged between the peristaltic pump and the buffer container, one branch of the three-way electromagnetic valve is connected with the waste liquid outlet, the other branch of the three-way electromagnetic valve is connected to the buffer container, the controller is connected with the three-way electromagnetic valve, the controller executes rinsing according to a user set program and discharges rinsing liquid into waste liquid, and the controller pumps a solvent with a set volume into the buffer container according to the user set program.
3. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device also comprises a two-way electromagnetic valve arranged on a branch between the peristaltic pump and the three-way electromagnetic valve, and the controller controls the two-way electromagnetic valve to be opened and communicated to another liquid chromatographic column maintenance device according to a program set by a user to execute multi-machine combination.
4. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a magnetic stirrer and a magnetic stirring device which are arranged on the buffer container, the controller is connected with the magnetic stirring device, and the controller uniformly mixes the solvent in the buffer container according to a user setting method.
5. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises an ultrasonic module arranged on the buffer container, the controller is connected with the ultrasonic module, and the controller carries out ultrasonic degassing on the solvent in the buffer container according to a user setting method.
6. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a liquid discharge valve arranged on the buffer container, the controller is connected with the liquid discharge valve, and the controller can be used for discharging the solvent in the buffer container.
7. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a liquid level sensor arranged on the buffer container, the controller is connected with the liquid level sensor, when the flushing solvent in the buffer container fed back by the liquid level sensor is too little, the pump is controlled to be stopped in time, air is prevented from being pumped into the buffer container, and a chromatographic column is protected.
8. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a column temperature box arranged on the chromatographic column, the controller is connected with the column temperature box, and the controller is used for preserving heat of the chromatographic column according to a user setting method.
9. The liquid chromatography column maintenance device of claim 1, wherein: the liquid chromatographic column maintenance device further comprises a liquid level sensor arranged on the waste liquid receiving barrel, the controller is connected with the liquid level sensor, and the controller prompts the liquid amount of the waste liquid receiving barrel of a user according to the feedback of the liquid level sensor and gives an overflow early warning.
10. A liquid chromatography column maintenance device according to any one of claims 1 to 9, wherein: the liquid chromatography column maintenance device can carry out the thing networking, and the user can look over the washing state and remote control starts or stops washing procedure.
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| CN202023291458.7U CN214150580U (en) | 2020-12-31 | 2020-12-31 | Liquid chromatographic column maintenance device |
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| CN202023291458.7U CN214150580U (en) | 2020-12-31 | 2020-12-31 | Liquid chromatographic column maintenance device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115097048A (en) * | 2022-07-15 | 2022-09-23 | 浙江康恩贝制药股份有限公司 | Regeneration and activation method for normal phase silica gel column in high performance liquid chromatograph |
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2020
- 2020-12-31 CN CN202023291458.7U patent/CN214150580U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115097048A (en) * | 2022-07-15 | 2022-09-23 | 浙江康恩贝制药股份有限公司 | Regeneration and activation method for normal phase silica gel column in high performance liquid chromatograph |
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