CN106290592B - High performance liquid chromatography device and working method thereof - Google Patents
High performance liquid chromatography device and working method thereof Download PDFInfo
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- CN106290592B CN106290592B CN201510252372.8A CN201510252372A CN106290592B CN 106290592 B CN106290592 B CN 106290592B CN 201510252372 A CN201510252372 A CN 201510252372A CN 106290592 B CN106290592 B CN 106290592B
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- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000002347 injection Methods 0.000 claims abstract description 77
- 239000007924 injection Substances 0.000 claims abstract description 77
- 238000012423 maintenance Methods 0.000 claims abstract description 54
- 239000012459 cleaning agent Substances 0.000 claims abstract description 48
- 238000004458 analytical method Methods 0.000 claims abstract description 39
- 238000005259 measurement Methods 0.000 claims abstract description 31
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 40
- 238000004140 cleaning Methods 0.000 claims description 39
- 239000003153 chemical reaction reagent Substances 0.000 claims description 35
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims 4
- 238000010619 multiway switching Methods 0.000 claims 2
- 239000012530 fluid Substances 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 description 19
- 239000002699 waste material Substances 0.000 description 19
- 239000000306 component Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 6
- 239000006226 wash reagent Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000000872 buffer Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000013375 chromatographic separation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 102000017011 Glycated Hemoglobin A Human genes 0.000 description 1
- 108010014663 Glycated Hemoglobin A Proteins 0.000 description 1
- 206010018910 Haemolysis Diseases 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 210000000601 blood cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000008588 hemolysis Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention provides a high performance liquid chromatography device, which has a measurement mode and a maintenance mode. The high performance liquid chromatography device comprises a sample injection system, an analysis system and a control system. The sample injection system is used for providing a sample to be tested and a mobile phase to the analysis system. The analysis system includes a chromatography column and a detector. The control system is used for controlling the sample injection system and the analysis system. The analysis system also includes a filter and a diverter disposed between the filter and the chromatographic column. The diverter places the filter in different fluid paths in the measurement mode and the maintenance mode. In the measurement mode, the sample to be measured enters the chromatographic column for chromatography through a filter and a reverser. In the maintenance mode, the first cleaning agent is discharged through the filter and the diverter, and the first cleaning agent cleans the filter while passing through the filter. The invention also provides a working method of the high performance liquid chromatography.
Description
Technical Field
The invention relates to a high performance liquid chromatography device and a working method thereof.
Background
The chromatographic column is a core component for determining the analytical performance of the high performance liquid chromatography device. Sample component analysis, such as glycosylated hemoglobin analysis, is performed based on a High Performance Liquid Chromatography (HPLC) device, and typically, a blood sample after hemolysis is separated by a chromatographic column. The hemolyzed sample contains a large amount of cell membrane fragments, and impurities such as clots in blood. Along with the increase of the analysis times of the chromatographic column, the impurities can be retained in the chromatographic column, so that the flow resistance of the chromatographic column is increased, the column pressure is increased, the column efficiency is seriously reduced, the accuracy of sample analysis is affected, and finally the chromatographic column has to be replaced. At present, the current time of the process, the chromatographic column is usually protected pre-column by a filtration device.
However, the filter device is also blocked by impurities in the sample to be analyzed along with the increase of the test times, the pressure drop is increased, and after the pressure drop is increased to the upper pressure limit of the system, the filter or the pre-column is required to be replaced, so that inconvenience is brought to a user, and the use cost is increased.
Disclosure of Invention
In view of the foregoing, it is desirable to provide a high performance liquid chromatography device free of filter replacement and a method of operating the same.
A high performance liquid chromatography device has a measurement mode and a maintenance mode. The high performance liquid chromatography device comprises a sample injection system, an analysis system and a control system. The sample injection system is used for providing a sample to be tested and a mobile phase to the analysis system. The analysis system comprises a chromatographic column and a detector, wherein the mobile phase forms continuous liquid flow under the pushing of the sample injection system, the chromatographic column separates the components to be detected in the sample to be detected under the action of the liquid flow, and the detector detects the signals of the components to be detected. The control system is used for controlling the sample injection system and the analysis system. The analysis system also includes a filter and a diverter disposed between the filter and the chromatographic column. The diverter places the filter in different fluid paths in the measurement mode and the maintenance mode. In the measurement mode, the sample to be measured enters the chromatographic column for chromatography through a filter and a reverser. In the maintenance mode, the first cleaning agent is discharged through the filter and the diverter, and the first cleaning agent cleans the filter while passing through the filter.
The high performance liquid chromatography device also comprises a pressure sensor, when the pressure of the flow path system, at least including the filter, measured by the pressure sensor exceeds a preset value, information is sent to the control system, and the control system outputs alarm information and/or starts the maintenance mode.
The sample injection system comprises an injector, a sample injection valve, a quantitative ring and a constant flow pump for providing the mobile phase, wherein in the measurement mode, the injector injects a sample to be measured into the quantitative ring through the sample injection valve, and the mobile phase drives the sample to be measured collected in the quantitative ring to flow to the chromatographic column; in the maintenance mode, the injector injects the first cleaning reagent into the dosing ring through the sample injection valve, and the mobile phase drives the first cleaning reagent collected in the dosing ring to flow to the filter.
The high performance liquid chromatography device also comprises an additional liquid path module, the additional fluid circuit module has a power source that provides a first cleaning agent into the filter.
The additional liquid path module is directly connected with the filter, and the first cleaning reagent firstly cleans the filter and then is discharged through the reverser.
The additional liquid path module is directly connected with the reverser, and the first cleaning reagent enters the filter through the reverser, cleans the filter and is discharged through the reverser.
A high performance liquid chromatography working method comprises the following steps:
the control system sends a maintenance starting instruction, and the commutator is converted to disconnect the filter from the chromatographic column;
delivering a first cleaning reagent to the filter and cleaning the filter;
delivering a mobile phase to the filter and cleaning the filter of residual cleaning agent;
the control system receives the maintenance completion instruction and determines a measurement starting instruction, and converts the commutator to connect the filter with the chromatographic column;
the sample to be measured is conveyed to the filter and enters the chromatographic column for chromatography through the reverser.
The high performance liquid chromatography working method further comprises the step of monitoring the pre-column pressure of the chromatography column by a pressure sensor, and outputting alarm information and/or starting a maintenance mode when the pre-column pressure exceeds a preset value.
The first cleaning reagent and the sample to be tested share a sample injection pipeline.
The first cleaning reagent enters the filter through the additional liquid path module.
Compared with the prior art, the high performance liquid chromatography device is provided with the reverser between the filter and the chromatographic column. When the high performance liquid chromatography device is in a maintenance mode, the first cleaning reagent passes through the filter and cleans the filter to remove impurities blocked on the filter. The commutator controls the first cleaning reagent discharged from the filter to be discharged through the commutator, so that the problem that the chromatographic separation effect of the chromatographic column is affected due to the fact that the pressure drop of the filter is increased due to the blockage of impurities is solved, and the situation that a user frequently opens the device shell to replace the filter when using is avoided, so that the use cost is reduced. The high performance liquid chromatography working method of the invention comprises the step of cleaning the filter, so that the chromatographic separation effect of the chromatographic column is better.
Drawings
Fig. 1 is a system configuration diagram of sample loading to be tested according to a first preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 2 is a system configuration diagram of sample injection of a sample to be tested according to a first preferred embodiment of the present invention.
FIG. 3 is a block diagram showing a system for loading a cleaning agent in accordance with a first preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 4 is a system configuration diagram of a cleaning reagent sample injection of a first preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 5 is a system configuration diagram of a measurement mode of a second preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 6 is a system configuration diagram of a maintenance mode of a second preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 7 is a system configuration diagram of a measurement mode of a third preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Fig. 8 is a system configuration diagram of a maintenance mode of a third preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
FIG. 9 is a fourth embodiment of a high performance liquid chromatography device according to the invention system configuration diagram of measurement mode of preferred embodiment.
Fig. 10 is a system configuration diagram of a maintenance mode of a fourth preferred embodiment of the high performance liquid chromatography apparatus of the present invention.
Description of the main reference signs
| High performance liquid chromatography device | 100，200，300，400 |
| Sample injection system | 10 |
| Injection syringe | 11 |
| Sample injection valve | 12 |
| Joint | 12a，12b，12c，12d， 12e，12f，23a，23b，23c，23d，23e，23f，33a，33b，33c， 33d，43a，43b，43c，43d，43e，43f，53a，53b，53c，53d，53e，53f |
| Quantitative ring | 13 |
| Sample bottle | 14 |
| Sample injection pipeline | 15 |
| Reagent bottle | 16 |
| Buffer solution bottle | 17 |
| Constant flow pump | 18 |
| Analysis system | 20 |
| Pressure sensor | 21 |
| Filter device | 22 |
| Commutator device | 23，33，43，53 |
| Chromatographic column | 24 |
| Detector for detecting a target object | 25 |
| Recording device | 26 |
| Back pressure regulating device | 27 |
| Waste liquid an outlet | 28 |
| Waste liquid channel | 29 |
| Control system | 30 |
| Additional liquid circuit module | 44，54 |
The invention will be further described in the following detailed description in conjunction with the above-described figures.
Detailed Description
As shown in fig. 1, 2, 3 and 4, a first preferred embodiment of the hplc apparatus 100 of the present invention includes a sample injection system 10, an analysis system 20 and a control system 30, wherein the control system 30 is used for controlling the sample injection system 10 and the analysis system 20. The high performance liquid chromatography device 100 has a measurement mode and a maintenance mode.
In the measurement mode, the sample injection system 10 includes a syringe 11, a sample injection valve 12, a dosing ring 13, a sample bottle 14, a sample injection line 15, a buffer bottle 17, and a constant flow pump 18. The sample injection pipeline 15 is connected among the injector 11, the sample injection valve 12, the quantitative ring 13, the reagent bottle 14, the buffer solution bottle 17 and the constant flow pump 18.
Those skilled in the art will appreciate that the sample injection system 10 may also be a direct means for transferring trace amounts of liquid to load the liquid into the analysis system 20, i.e., the sample injection system 10 may not include the sample injection valve 12 and the metering ring 13.
It will be appreciated that in maintenance mode, the sample vial 14 is replaced by a reagent vial 16 storing a first wash reagent, i.e. the first wash reagent shares a sample line 15 with the sample to be tested.
The syringe 11 is used to aspirate a first wash reagent of a sample or reagent bottle 16 to be measured stored in the sample bottle 14 into the dosing ring 13. Those skilled in the art will appreciate that the present invention is not limited to syringes and that other devices that can effect transfer of a trace amount of liquid may be used with the present invention.
The injection valve 12 is, for example, an n-way switching valve (n > 2) or a combination of n-way switching valves. Further, the sample injection valve 12 is, for example, a three-way switching valve, a four-way switching valve, a six-way switching valve, or a combination thereof. The commutator 23 is in the measuring mode and the different liquid paths are formed in the maintenance mode.
In this embodiment, the sample injection valve 12 is a six-way switching valve, and the sample injection valve 12 is provided with a plurality of connectors 12a,12b,12c,12d, 12e,12f, and each connector is connected with an adjacent conversion port in a switching manner through a driving motor (not shown).
It will be appreciated that the dosing ring 13 is capable of performing a quantitative manipulation of the sample flow.
The constant flow pump 18 is used to provide a mobile phase with a constant flow rate. The buffer bottle 17 is used for storing the mobile phase. The mobile phase provided by the constant flow pump 18 is capable of loading the sample to be tested into the analysis system 20.
The analysis system 20 comprises a pressure sensor 21, a filter 22, a commutator 23, a chromatographic column 24, a detector 25, a recording device 26, a back pressure regulating device 27 and a waste liquid outlet 28.
In this embodiment, the joint 23b of the commutator 23 is connected to a waste liquid channel 29.
Those skilled in the art will appreciate that the connector 23c of the commutator 23 may also be connected to other fluid circuit modules (not shown).
The pressure sensor 21 is used to monitor the flow path system pressure including the filter 22. The pressure sensor 21 may be disposed in the flow path before the chromatographic column 24, between the filter 22 and the commutator 23, between the commutator 23 and the chromatographic column 24, before the metering gasket 13 and the filter 22, or between the constant flow pump 18 and the sample injection valve 12. When the column pressure in front of the chromatographic column 24 exceeds a preset value, a message is sent to the control system 30, the control system 30 issues an alarm message to prompt the user for maintenance work.
The filter 22 is, for example, a mesh or a filter cartridge. The chromatographic column 24 is used to separate the component to be tested into individual components. The detector 25 is used to measure the response signal generated within the detector 25 for each individual component. The recording device 26 is used for recording the electrical signal data measured by the detector 25. The back pressure regulating device 27 may be a back pressure regulating valve. The waste outlet 28 discharges waste. The waste liquid channel 29 is used for discharging the first cleaning agent and impurities passing through the filter 22.
The commutator 23 is, for example, an n-way switching valve (n > 2) or a combination of a plurality of n-way switching valves. Further, the commutator 23 is, for example, a three-way switching valve, a four-way switching valve, a six-way switching valve, or a combination thereof. The commutator 23 forms different liquid paths in the measurement mode and the maintenance mode.
In this embodiment, the commutator 23 is a six-way switching valve, and the commutator 23 is provided with a plurality of connectors 23a,23b,23c,23d,23e,23f, each of which is switchably connected to its adjacent switching port by a driving motor (not shown).
Referring to fig. 1 and fig. 2 together, when the hplc apparatus 100 performs measurement of a sample to be measured, the sample injection system 10 loads the sample to be measured. The syringe 11 is connected with the joint 12b through a pipeline; the joint 12a of the sample injection valve 12 is connected with the joint 12b, the joint 12c is connected with the joint 12d, and the joint 12e is connected with the joint 12 f; two ends of the quantitative ring 13 are respectively connected with a joint 12a and a joint 12 d; the sample vial 14 is connected to the connector 12 c. The syringe 11 sucks the sample to be measured stored in the sample bottle 14 to the dosing ring 13, thereby completing the loading of the sample to be measured.
Next, by switching the sample valve 12, the connection joint 12a is connected to the joint 12f, the joint 12e is connected to the joint 12d, and the joint 12b is connected to the joint 12c, so that the dosing ring 13 is directly connected to the filter 22.
Further, by switching the commutator 23, the connection joint 23a is connected with the joint 23f, the joint 23e is connected with the joint 23d, and the joint 23b is connected with the joint 23c, so that the filter 22 is directly connected with the chromatographic column 24.
It will be appreciated that the switch of the diverter 23 may be accomplished prior to loading of the sample to be tested, or may be accomplished simultaneously with the sample valve 12 during loading of the sample to be tested.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Then, the mobile phase with constant flow rate provided by the constant flow pump 18 enters the quantitative loop 13 through the joint 12a and the joint 12f, and the sample to be measured collected by the quantitative loop 13 is eluted and then sent out, enters the filter 22 through the joint 12d and the joint 12e for filtration, and then enters the chromatographic column 24 through the joint 23a and the joint 23 f. The sample to be measured is separated in the chromatographic column 24, and then enters the detector 25 through the connector 23e and the connector 23d, and each component is sequentially detected by the detector 25.
It will be appreciated that the components to be measured are separated into individual components after passing through the column 24 and flow to the detector 25. The concentration of the sample components in the detector 25 is converted into an electrical signal which is transmitted to the recording device 26, printed in the form of a map or subjected to subsequent data processing. The waste liquid from the measurement process is discharged to the waste liquid outlet 28.
Referring to fig. 3 and 4, when the hplc apparatus 100 performs maintenance, the sample injection system 10 loads the first cleaning agent. The syringe 11 is connected to the connector 12 b; the joint 12a of the sample injection valve 12 is connected with the joint 12b, the joint 12c is connected with the joint 12d, and the joint 12e is connected with the joint 12 f; two ends of the quantitative ring 13 are respectively connected with a joint 12a and a joint 12 d; the reagent bottle 16 is connected to the connector 12 c. The syringe 11 sucks the first washing reagent stored in the reagent bottle 16 to the dosing ring 13, thereby completing the loading of the first washing reagent.
Next, by switching the sample valve 12, the connection joint 12a is connected to the joint 12f, the joint 12e is connected to the joint 12d, and the joint 12b is connected to the joint 12c, so that the dosing ring 13 is directly connected to the filter 23.
Further, by switching the commutator 23, the connection joint 23a is connected to the joint 23b, the joint 23c is connected to the joint 23d, and the joint 23e is connected to the joint 23f, so that the filter 23 is disconnected from the column 24.
Those skilled in the art will appreciate that the connector 23c of the commutator 23 may also be connected to other fluid circuit modules (not shown).
It will be appreciated that the switch of the diverter 23 may be accomplished prior to the loading of the wash reagent or simultaneously with the sample valve 12 during the loading of the wash reagent.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Then, the mobile phase provided by the constant flow pump 18 enters the quantitative loop 13 through the joint 12a and the joint 12f, and the first cleaning agent collected by the quantitative loop 13 is eluted and then sent out, enters the filter 23 through the joint 12d and the joint 12e, and cleans the filter 23, and the first cleaning agent and other impurities discharged from the filter are discharged to the waste liquid channel 29 through the joint 23a and the joint 23 b.
It will be appreciated that the first cleaning reagent may be repeatedly loaded and injected a number of times to clean impurities that have clogged the filter. After the cleaning by the loaded cleaning agent, the first cleaning agent remaining in the filter 23 may be removed by the second cleaning agent. The second wash reagent is, for example, a mobile phase or other buffer reagent stored in the buffer bottle 17.
It will be appreciated that the first cleaning agent effectively eliminates the pressure drop across the filter 23 by breaking down impurities, such as blood cell membrane debris, blood clots, etc., that clog the filter 23 into smaller substances by chemical principles that pass through the pore size of the filter 23.
It will be appreciated that the addition of a diverter in front of the column 24 allows the first cleaning agent to flow to the waste channel 33 without flowing through the column 24 during cleaning of the filter 23, thereby avoiding the effect of cleaning agent on the column.
In this embodiment, the sample injection system 10 is loaded with a predetermined volume of the sample to be measured in the measurement mode of the hplc apparatus 100, the sample to be tested is pushed by the mobile phase and enters the chromatographic column 24 for chromatography through the filter 22 and the reverser 23. During the measurement process of the sample to be measured, the pressure sensor 21 monitors the pre-column pressure of the chromatographic column 24 in real time, and when the measured pre-column pressure of the chromatographic column 24 exceeds a preset value, information is sent to the control system 30, and the control system 30 controls the start of the maintenance mode. In maintenance mode, the sample injection system 10 injects the first cleaning agent into the mobile phase, then loads the first cleaning agent into the filter 22, cleans the filter 22, and discharges the first cleaning agent and impurities discharged through the filter 22 to the waste channel 29 through the diverter 23. After cleaning, the filter is cleaned of residual cleaning agent with a second cleaning agent to complete maintenance.
It will be appreciated that in other embodiments, the hplc apparatus may also be operated in a manual start-up maintenance mode as desired. For example, when the pressure sensor 21 detects that the pressure exceeds a preset value, information is sent to the control system 30, and the control system 30 sends alarm information to prompt the user to perform maintenance operation through a man-machine interaction interface. After the user inputs the maintenance instruction through the man-machine interaction interface, the control system 30 obtains maintenance instructions and initiates maintenance mode operation.
The high performance liquid chromatography device is provided with the pressure sensor so as to monitor the pressure of a flow path system at least comprising the filter in real time. When the measured pressure exceeds a preset value, the high performance liquid chromatography device automatically starts a maintenance mode to work. In the maintenance mode, the filter-plugged impurities are repeatedly cleaned by the first cleaning agent until the pressure drops below a preset value, thereby realizing that the user does not replace the filter or pre-column.
Referring to fig. 5 and 6, a system structure diagram of a second preferred embodiment of the hplc apparatus 200 of the present invention is shown.
The sample injection system 10, the analysis system 20 and the control system 30 are substantially identical to those of the first preferred embodiment. The commutator 33 is a four-way switching valve. The commutator 33 is provided with several joints 33a, 33b, 33c, 33d. The first cleaning agent is carried into the filter 22 via the mobile phase provided by the constant flow pump 18 and cleans the filter 22, and the diverter 33 controls the flow of the first cleaning agent discharged from the filter 22 to the waste outlet 28.
In this embodiment, the first cleaning reagent is the same as the sample line 15 of the sample to be tested.
Referring to fig. 5, when the hplc apparatus 200 performs measurement of a sample to be measured, the sample injection system 10 loads the sample to be measured, similar to fig. 1 and 2.
Further, by switching the commutator 33, the connection joint 33a and the joint 33b, and the joint 33c and the joint 33d are connected so that the filter 22 is directly connected to the column 24.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Subsequently, a constant flow of the mobile phase supplied from the constant flow pump 18 of the analysis system 20 enters the quantitative loop 13 through the connector 12a and the connector 12f, and the sample to be measured collected by the quantitative loop 13 is eluted and then sent out, enters the filter 22 through the connector 12d and the connector 12e for filtration, and then enters the chromatographic column 24 through the connector 33b and the connector 33 a. The sample to be measured is separated in the column 24, and then enters the detector 25 through the connector 33d and the connector 33c, and each component is sequentially detected by the detector 25.
Referring to fig. 6, when the hplc apparatus 200 performs maintenance, the sample injection system 10 loads the first cleaning agent, similar to fig. 3 and 4.
Further, by switching the commutator 33, the connection joint 33a and the joint 33d, and the joint 33b and the joint 33c are connected, so that the filter 22 is disconnected from the column 24.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Then, the constant flow rate of the mobile phase supplied from the constant flow pump 18 of the analysis system 20 enters the dosing ring 13 through the connectors 12a and 12f, and the first cleaning agent collected by the dosing ring 13 is eluted and then sent out, enters the filter 22 through the connectors 12d and 12e, and cleans the filter 22, and then the first cleaning agent and other impurities discharged from the filter 22 are discharged to the waste liquid outlet 28 through the connectors 33b and 33 c.
Referring to fig. 7 and 8 together, a third preferred embodiment of the hplc apparatus 300 of the present invention is similar to fig. 3 and 4 in that the hplc apparatus 300 includes a sample injection system 10, an analysis system 20 and a control system 30.
The sample injection system 10, the analysis system 20 and the control system 30 are substantially identical to those of the first preferred embodiment. Instead, the additional fluid circuit module 44 is directly connected to the filter 22. The additional fluid circuit module 44 has a power source that provides a first cleaning agent into the filter 22. The additional fluid circuit module 44 may be other high pressure or low pressure fluid circuit modules of the hplc that provide power and piping to deliver the first and second cleaning fluids to the filter when the filter requires maintenance. The cleaning agent can be a constant flow pump and a pipeline similar to a sample injection system, or a common low pressure pump, a peristaltic pump and the like and a corresponding pipeline, so long as the cleaning agent can be transported.
It will be appreciated that the commutator 43 is, for example, a six-way switching valve. The commutator 43 is provided with several joints 43a,43b,43c,43d,43e,43f, each connector is connected with the adjacent conversion port in a switching way through a driving motor (not shown).
Referring to fig. 7, when the hplc apparatus 300 performs measurement of a sample to be measured, the sample injection system 10 loads the sample to be measured, similar to fig. 1 and 2.
Further, by switching the commutator 43, the connection joint 43a is connected with the joint 43f, the joint 43e is connected with the joint 43d, and the joint 43b is connected with the joint 43c, so that the filter 22 is directly connected with the column 24.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Further, a constant flow rate of the mobile phase supplied from the constant flow pump 18 of the analysis system 20 enters the quantitative loop 13 through the connector 12a and the connector 12f, and the sample to be measured collected by the quantitative loop 13 is eluted and then sent out, enters the filter 22 through the connector 12d and the connector 12e for filtration, and then enters the chromatographic column 24 through the connector 43a and the connector 43 f. The sample to be measured is separated in the column 24, and then enters the detector 25 through the connector 43e and the connector 43d, and each component is sequentially detected by the detector 25.
Referring to fig. 8, when the hplc apparatus 300 performs maintenance, the additional liquid path module 44 loads the first cleaning agent. By switching the commutator 43, the connection joint 43a is connected with the joint 43b, the joint 43c is connected with the joint 43d, and the joint 43e is connected with the joint 43f, so that the filter 22 is disconnected from the column 24.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Further, the first cleaning agent supplied through the additional liquid path module 44 is injected into the filter 22 and cleans the filter 22, and then the first cleaning agent and other impurities discharged from the filter 22 are discharged to the waste liquid channel 29 through the connectors 43a and 43 b.
It will be appreciated that the first cleaning agent and other impurities discharged from the filter 22 can also be discharged to the waste outlet 28 via the connectors 43a and 43 b.
Referring to fig. 9 and 10, a system structure diagram of a fourth preferred embodiment of the hplc apparatus 400 of the present invention is shown. Similar to fig. 3 and 4, the high performance liquid chromatography apparatus 400 includes a sample injection system 10, an analysis system 20, and a control system 30.
It is understood that the sample injection system 10, the analysis system 20 and the control system 30 are identical to those of the first preferred embodiment.
In contrast, the diverter 53 is directly connected to the additional fluid path module 54, and the diverter 53 controls the first cleaning agent to flow through the filter 22 and then to be discharged to the waste fluid channel 29.
It will be appreciated that the additional fluid circuit module 54 has a power source that provides the first cleaning agent into the filter 22.
In this embodiment, the reverse cleaning of the filter 22 is achieved, and the cleaning effect is better.
Referring to fig. 9, when the hplc apparatus 300 performs measurement of a sample to be measured, the sample injection system 10 loads the sample to be measured.
Further, by switching the commutator 53, the connection terminal 53a is connected to the terminal 53b, the terminal 53c is connected to the terminal 53d, and the terminal 53e is connected to the terminal 53f, so that the filter 22 is directly connected to the column 24.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Then, the constant flow rate of the mobile phase supplied from the constant flow pump 18 of the analysis system 20 enters the quantitative loop 13 through the connector 12a and the connector 12f, and the sample to be measured collected by the quantitative loop 13 is eluted and then sent out, enters the filter 22 through the connector 12d and the connector 12e for filtration, and then enters the chromatographic column 24 through the connector 53f and the connector 53 e. The sample to be measured is separated in the chromatographic column 24 and then enters the detector 25, and each component is sequentially detected by the detector 25.
Referring to fig. 10, when the hplc apparatus 400 performs maintenance work, the connection terminal 53a is connected to the terminal 53b, the connection terminal 53c is connected to the terminal 53d, and the connection terminal 53e is connected to the terminal 53f, so that the filter 22 is disconnected from the chromatographic column 24, and the additional liquid path module 54 is connected to the filter 22. The additional fluid circuit module 54 may be other high pressure or low pressure fluid circuit modules of the hplc, and may provide power and piping to deliver the first and second cleaning fluids to the filter when the filter requires maintenance. The cleaning agent can be a constant flow pump and a pipeline similar to a sample injection system, or a common low pressure pump, a peristaltic pump and the like and a corresponding pipeline, so long as the cleaning agent can be transported.
It will be appreciated that in this embodiment, the injection valve 12 and the commutator 23 are switched in position by a driving motor (not shown).
Further, the additional liquid path module 54 allows the first cleaning agent to enter the filter 22 through the connectors 53c and 53 and cleans the filter 22, and then the first cleaning agent and other impurities discharged from the filter 22 are discharged to the waste liquid channel 29 through the connectors 53a and 53 b. The additional fluid circuit module 54 provides the mobile phase through other lines to clean the remaining cleaning agent in the filter 22.
It will be appreciated that in the above four embodiments, by providing a pressure sensor, the hplc device automatically starts the maintenance mode when the pressure measured by the pressure sensor exceeds a predetermined value. In addition, the high performance liquid chromatography device can also be started to work in a maintenance mode manually according to the requirement. The specific operation is as described above.
It will be appreciated that the filter is cleaned by the first cleaning agent so that impurities clogged in the filter are broken down into small substances and pass through the aperture of the filter, and the cleaned first cleaning agent and impurities are simultaneously flowed to the waste liquid channel, thereby preventing the first cleaning agent from entering the chromatographic column and avoiding the chromatographic column from being damaged.
The high performance liquid chromatography device is provided with the pressure sensor so as to monitor the pressure of a flow path system at least comprising the filter in real time. When the measured pressure exceeds a preset value, the high performance liquid chromatography device automatically starts a maintenance mode to work. In the maintenance mode, the filter clogged impurities are repeatedly cleaned by the first cleaning agent until the pressure drops below a preset value. The cleaning and maintenance of the filter solve the problem that the chromatographic separation effect of the chromatographic column is affected by the rising of pressure drop of the filter caused by the blockage of impurities, and avoid the frequent opening of the device shell for the replacement of the filter when the filter is used, thereby reducing the use cost.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above examples, which are only for explaining the claims. The scope of the invention is not limited by the description. Any changes or substitutions that would be readily apparent to one skilled in the art within the scope of the present disclosure are intended to be included within the scope of the present invention.
Claims (7)
1. The high performance liquid chromatography device comprises a measurement mode and a maintenance mode, and comprises a sample injection system, an analysis system and a control system, wherein the sample injection system is used for providing a sample to be tested and a mobile phase to the analysis system, and comprises a syringe, a sample injection valve, a quantitative ring and a constant flow pump used for providing the mobile phase; the analysis system comprises a chromatographic column and a detector, wherein the mobile phase forms continuous liquid flow under the pushing of the constant flow pump, the chromatographic column separates components to be detected in a sample to be detected under the action of the liquid flow, and the detector detects signals of the components to be detected; the control system is used for controlling the sample injection system and the analysis system; the analysis system also comprises a filter and a reverser arranged between the filter and the chromatographic column, wherein the number of the filters is one, the reverser enables the filter to be in different liquid paths in the measurement mode and the maintenance mode, in the measurement mode, the sample to be detected enters the chromatographic column to be chromatographed through the filter and the reverser in sequence, the injector injects the sample to be detected into the quantitative ring through the sample injection valve, and the mobile phase provided by the constant flow pump drives the sample to be detected collected in the quantitative ring to flow to the chromatographic column; in a maintenance mode, the first cleaning reagent is discharged through the filter and the reverser, the filter is cleaned when the first cleaning reagent passes through the filter, the injector injects the first cleaning reagent into the quantitative ring through the sample injection valve, and the mobile phase provided by the constant flow pump drives the first cleaning reagent collected in the quantitative ring to flow to the filter;
the sample injection valve is a multi-way switching valve and is provided with a plurality of connectors; the joint communication state of the sample injection valve when the constant flow pump drives the sample to be detected collected in the quantitative ring to flow to the chromatographic column in the measurement mode is the same as the joint communication state of the sample injection valve when the constant flow pump drives the first cleaning reagent collected in the quantitative ring to flow to the filter in the maintenance mode; the constant flow pump drives a pipeline between the constant flow pump and the filter when the sample to be measured, which is collected in the quantitative ring, flows to the chromatographic column in the measurement mode, and the constant flow pump drives a pipeline between the constant flow pump and the filter when the first cleaning reagent, which is collected in the quantitative ring, flows to the filter in the maintenance mode.
2. The high performance liquid chromatography device of claim 1, wherein: the high performance liquid chromatography device also comprises a pressure sensor, when the pressure measured by the pressure sensor exceeds a preset value, the pressure sensor sends information to the control system, and the control system outputs alarm information and/or starts the maintenance mode.
3. A high performance liquid chromatography device having a measurement mode and a maintenance mode, comprising a sample injection system, an analysis system and a control system, wherein the sample injection system is used for providing a sample to be tested and a mobile phase to the analysis system; the sample injection system comprises a syringe, a sample injection valve, a quantitative ring and a constant flow pump for providing the mobile phase; the analysis system comprises a chromatographic column and a detector, wherein the mobile phase forms continuous liquid flow under the pushing of the sample injection system, the chromatographic column separates components to be detected in a sample to be detected under the action of the liquid flow, and the detector detects signals of the components to be detected; the control system is used for controlling the a sample injection system and the analysis system; the analysis system also comprises a filter and a reverser, wherein the number of the filters is one, the reverser enables the filters to be in different liquid paths in the measurement mode and the maintenance mode, in the measurement mode, the sample to be detected enters the chromatographic column for chromatography through the filters and the reverser, and the sample to be detected flows to the chromatographic column through the sample injection system; in the maintenance mode, the first cleaning reagent is discharged through the filter and the reverser, and the first cleaning reagent cleans the filter when passing through the filter; the high performance liquid chromatography device also comprises an additional liquid path module, wherein the additional liquid path module is provided with a power source for providing a first cleaning reagent to enter the filter, and the first cleaning reagent flows to the filter through the additional liquid path module;
the sample injection valve is a multi-way switching valve and is provided with a plurality of connectors; the joint communication state of the sample injection valve when the constant flow pump drives the sample to be tested to flow to the chromatographic column in the measurement mode is the same as the joint communication state of the sample injection valve when the additional liquid path module drives the first cleaning reagent to flow to the filter in the maintenance mode.
4. A high performance liquid chromatography apparatus according to claim 3, wherein: the additional liquid path module is directly connected with the filter, the first cleaning reagent firstly cleans the filter and then is discharged through the reverser, and under the measuring mode, the sample to be measured enters the chromatographic column for chromatography through the filter and the reverser in sequence.
5. A high performance liquid chromatography apparatus according to claim 3, wherein: the additional liquid path module is directly connected with the reverser, and the first cleaning reagent enters the filter through the reverser, cleans the filter and is discharged through the reverser.
6. A method of high performance liquid chromatography operation of the high performance liquid chromatography device of any one of claims 1 to 5, comprising the steps of:
the control system sends a maintenance starting instruction, and the commutator is converted to disconnect the filter from the chromatographic column;
delivering a first cleaning reagent to the filter and cleaning the filter;
delivering a second cleaning agent to the filter and cleaning the filter of residual cleaning agent;
the control system receives the maintenance completion instruction and determines a measurement starting instruction, and converts the commutator to connect the filter with the chromatographic column;
the sample to be measured is conveyed to the filter and enters the chromatographic column for chromatography through the reverser.
7. The method of high performance liquid chromatography according to claim 5, wherein: the high performance liquid chromatography working method also comprises the steps of monitoring the pressure of a flow path system at least comprising a filter, and outputting alarm information and/or starting a maintenance mode when the pressure exceeds a preset value.
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| CN204203174U (en) * | 2014-11-27 | 2015-03-11 | 王峰 | A kind of liquid chromatograph |
| CN204203173U (en) * | 2014-11-27 | 2015-03-11 | 王峰 | A kind of liquid chromatograph |
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| JP2012145513A (en) * | 2011-01-14 | 2012-08-02 | Hitachi High-Technologies Corp | Analyzer |
| CN204203174U (en) * | 2014-11-27 | 2015-03-11 | 王峰 | A kind of liquid chromatograph |
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