Full-automatic chromatographic distillate collecting device

Abstract

The invention discloses a full-automatic chromatographic distillate collecting device which comprises a fixing support, a flow path control component and a fraction collecting component, the fraction collecting component comprises a plurality of collecting containers, and a fraction collecting control multi-way valve, a spraying control multi-way valve and a two-position three-way valve are arranged in the flow path control component; the common end of the fraction collection control multi-way valve is connected with the common end of the two-position three-way valve, one of the rest two ports of the two-position three-way valve is connected with a distillate inlet pipeline, and the other port of the two-position three-way valve is connected with a distillate outlet pipeline; a plurality of outlets of the fraction collection control multi-way valve are respectively connected with different collection containers through different distillate branches; the common end of the spraying control multi-way valve is connected with a cleaning liquid inflow pipeline, and a plurality of outlets of the spraying control multi-way valve are connected with different collecting containers through different cleaning liquid branches respectively. The device can complete automatic collection of chromatographic distillate, merge the whole process, and automatically clean the collection container, so that the automation degree of chromatographic fraction collection work is greatly improved.

Description

Technical Field

[0001] The present invention relates to a fully automatic chromatographic eluate collection device for the automatic collection, merging of target compounds after chromatographic separation, and automatic cleaning of collection containers. Background Art

[0002] A fraction collector is an auxiliary device of a liquid chromatograph, mainly used for preparing and enriching pure components. To obtain a pure product of a target compound, the fraction collector needs to complete two steps: collecting the required components at the outlet of the separation column and merging the target fractions and introducing them into a subsequent device to remove the mobile phase in the fractions. To achieve a continuous and fully automatic chromatographic fraction collection process, the fraction collector is also required to have functions of automatic cleaning and resetting.

[0003] Currently, fraction collectors are generally divided into two categories. The first category is that collection containers are arranged in a general rectangular array, and the fraction distribution head is arranged in a two-dimensional plane or in three-dimensional dimensions, so as to selectively distribute liquid to each collection container to achieve the collection of different fractions. The first type of collector is collectively referred to as an "X-Y collector". The second category is that collection containers are installed on a circular turntable, and the fraction collector generally operates through the combination of a rotating turntable and an arm with a distribution head installed rotatably to achieve the collection of fractions. The second type of collector is collectively referred to as a "turntable collector".

[0004] The above two types of fraction collectors usually can only complete the function of automatic switching of collection containers, while the merging and concentration of target fractions and the cleaning and resetting of collection containers still need to be manually completed. These two time-consuming and laborious tasks limit the convenience and efficiency of using automatic fraction collectors, and make the existing devices unable to continuously and automatically process a large number of samples for a long time. Therefore, a fully automatic chromatographic fraction collection device that can complete the whole process of chromatographic fraction collection and can automatically clean and reset is needed. Summary of the Invention

[0005] To overcome the deficiencies of the above prior art, the present invention provides a device that can complete the full process of automatic collection and merging of chromatographic eluates and can automatically clean and reset the fraction collection containers, thereby further improving the automation degree of chromatographic fraction collection work.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A fully automatic chromatographic distillate collection device includes a fixed bracket and a flow path control component and a fraction collection component mounted on the fixed bracket. Among them, the fraction collection component includes a plurality of collection containers, and these collection containers are respectively connected to the flow path control component through different branches. It is characterized in that at least one fraction collection control multi-way valve, one spray control multi-way valve and one two-position three-way valve are arranged in the flow path control component. The common end of the fraction collection control multi-way valve is connected to the common end of the two-position three-way valve. The remaining two ports of the two-position three-way valve, one is connected to the distillate inlet pipe, and the other is connected to the distillate outlet pipe. The multiple outlets of the fraction collection control multi-way valve are respectively connected to different collection containers through different distillate branches. The common end of the spray control multi-way valve is connected to the cleaning liquid inlet pipe, and its multiple outlets are respectively connected to different collection containers through different cleaning liquid branches.

[0008] The distillate of the liquid chromatograph enters this fully automatic chromatographic distillate collection device through the distillate inlet pipe, and the fraction is collected by the collection container. The cleaning liquid enters this fully automatic chromatographic distillate collection device through the cleaning liquid inlet pipe to clean the collection container.

[0009] Further, the flow path control component further includes a housing and a connector. The fraction collection control multi-way valve and the spray control multi-way valve are electric valves, and the two-position three-way valve is a solenoid valve, and all are electrically connected to an external control system through the connector. The external control system provides power and control signals for this fully automatic chromatographic distillate collection device to achieve automatic control. Preferably, the housing is a waterproof housing.

[0010] In some embodiments of the present invention, the main bodies of the fraction collection control multi-way valve and the spray control multi-way valve are located inside the housing. The outlet of the fraction collection control multi-way valve is located on the bottom surface of the housing, and the outlet of the spray control multi-way valve is located on the top surface of the housing. The two-position three-way valve is arranged on one side surface of the housing, close to the fraction collection control multi-way valve.

[0011] Preferably, the top end of the collection container is connected to the outlet of the spray control multi-way valve through the cleaning liquid branch, and the bottom end is connected to the outlet of the fraction collection control multi-way valve through the distillate branch.

[0012] In some embodiments of the present invention, the collection container includes a screw - mouth test tube, a spray connection assembly, and a fraction collection connection assembly. Among them, the spray connection assembly is connected to the top of the screw - mouth test tube by a thread and includes a spray head, a first washer, a first adapter, a first end cap, and a first joint connected and assembled in sequence. The first joint is connected to an outlet of the spray control multi - way valve through a cleaning liquid branch; the fraction collection connection assembly is connected to the bottom of the screw - mouth test tube by a thread and includes a second washer, a second adapter, a second end cap, and a second joint connected and assembled in sequence. The second joint is connected to an outlet of the fraction collection control multi - way valve through a distillate branch.

[0013] In some embodiments of the present invention, the fraction collection component includes a plurality of collection containers and a fixed base. The collection containers are fixed on the fixed base through the mounting holes and spring positioning pins on the fixed base.

[0014] In some embodiments of the present invention, the fraction collection control multi - way valve and the spray control multi - way valve can be a six - way valve, an eight - way valve, a ten - way valve, a twelve - way valve, etc. Correspondingly, the fraction collection component includes 6, 8, 10, or 12 collection containers, and these collection containers are divided into two rows and are arranged on both sides of the flow path control component.

[0015] Using the above - mentioned fully automatic chromatographic distillate collection device, automatic fraction collection, automatic fraction merging, and automatic cleaning of the collection container of the liquid chromatographic distillate can be carried out.

[0016] When performing fraction collection, control the common end of the two - way three - way valve to communicate with the distillate inlet pipe. The liquid chromatograph injects the distillate into the distillate inlet pipe, flows out from the common end of the two - way three - way valve, and flows into the common end of the fraction collection control multi - way valve. The program controls the fraction collection control multi - way valve to sequentially connect its common end with its multiple outlets, and the distillate enters multiple collection containers in sequence.

[0017] When performing automatic fraction merging, select the collection container where the target product is located, control the common end of the two - way three - way valve to communicate with the distillate outlet pipe. The fraction collection control multi - way valve is sequentially switched to the distillate branch connecting the selected collection container. The distillate in the selected collection container flows into the corresponding distillate branch, then flows out from the common end of the fraction collection control multi - way valve, and flows into the common end of the two - way three - way valve, and finally flows out from the distillate outlet pipe.

[0018] When cleaning the collection container, the program controls the common end of the spray control multi-way valve to be connected to its outlet in sequence. The cleaning liquid enters the common end of the spray control multi-way valve through the cleaning liquid inflow pipeline, then flows through each cleaning liquid branch and enters the collection container to clean the collection container. The cleaned solution sequentially passes through the distillate branch, the fraction collection control multi-way valve, and the two-way three-way valve, and flows out from the distillate outflow pipeline.

[0019] Preferably, a spray head is provided at the top of the collection container, and the cleaning liquid is sprayed out from the spray head to wash the inner wall of the collection container and enter the collection container to clean the distillate remaining in the collection container.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] 1. The present invention can realize the automatic collection and merging of chromatographic distillates, which is convenient for introducing into subsequent devices to remove the mobile phase in the fractions and obtain pure target compounds. The present invention switches the connection states of the distillate inlet pipeline, the outlet pipeline, and the specific fraction collection container through the two-way three-way solenoid valve and the fraction collection control multi-way valve, and can realize the full process of automatic collection and merging of distillates in cooperation with subsequent devices.

[0022] 2. The present invention can realize the automatic cleaning of the device itself. After the cleaning is completed, the next fraction collection work can be carried out, thereby realizing the fraction collection work of continuously and automatically processing a large number of samples for a long time. After the target compounds are merged, the two-way three-way solenoid valve is connected to the distillate outflow pipeline, and the fraction collection container is sequentially cleaned through the spray head to realize the automatic cleaning of the device itself.

[0023] 3. The present invention has no moving parts, does not require lubrication, and will not cause loss of chromatographic distillates. The multi-way valve and the three-way valve are used to control the liquid flow direction. Compared with the traditional fraction collector, it has no moving parts and is reliable and easy to use. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic structural diagram of a full-automatic chromatographic distillate collection device according to an example of the present invention;

[0025] Figure 2 It is a schematic structural diagram of a flow path control component according to an example of the present invention;

[0026] Figure 3 It is an exploded view of a fraction collection component according to an example of the present invention;

[0027] Figure 4 It is a schematic structural diagram and an exploded view of a unit of a fraction collection component according to an example of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0028] In order to make the content of the present invention easier to be clearly understood, the present invention will be further described below according to specific embodiments in conjunction with the accompanying drawings.

[0029] As Figure 1 shown, a full-automatic chromatographic distillate collection device includes: a fixed bracket 1, a flow path control component 2 for controlling the flow direction of the chromatographic distillate, and a fraction collection component 3 for collecting the chromatographic distillate; the flow path control component 2 and the fraction collection component 3 are both installed on the fixed bracket 1; a distillate inlet pipe 4, a distillate outlet pipe 5, and a cleaning liquid inlet pipe 6 are provided on the flow path control component 2. Figure 1 In the full-automatic chromatographic distillate collection device shown, the structure of the flow path control component 2 is as Figure 2 shown, including a housing 2-1, a spray control multi-way valve 2-2 is provided at the top of the housing 2-1, a fraction collection control multi-way valve 2-3 is provided at the bottom, a two-way three-way valve 2-4 is provided on one side surface, and a circular connector 2-5 is provided on the other side surface. Among them, the housing 2-1 is a waterproof housing; in this embodiment, the spray control multi-way valve 2-2 is a ten-way valve, the main body is located in the housing 2-1, has a common end and 10 cleaning liquid outlets, its common end is connected to the cleaning liquid inlet pipe 6, and the 10 cleaning liquid outlets are respectively connected to 10 branches of the fraction collection component 3. The spray control multi-way valve 2-2 is used to select the connection between the cleaning liquid inlet pipe 6 and a branch of the fraction collection component 3; the fraction collection control multi-way valve 2-3 is also a ten-way valve, the main body is located in the housing 2-1, has a common end and 10 distillate outlets, its common end is connected to the common end of the two-way three-way valve 2-4, and the 10 distillate outlets are respectively connected to 10 branches of the fraction collection component 3. The fraction collection control multi-way valve 2-3 is used to select the connection between the common end of the two-way three-way valve 2-4 and a branch of the fraction collection component 3; the two-way three-way valve 2-4 is fixed on the housing 2-1, its common end is connected to the common end of the fraction collection control multi-way valve 2-3, one port is connected to the distillate inlet pipe 4, and the other port is connected to the distillate outlet pipe 5. The two-way three-way valve 2-4 is used to select the connection between the distillate inlet pipe 4 or the distillate outlet pipe 5 and the common end. The spray control multi-way valve 2-2, the fraction collection control multi-way valve 2-3, and the two-way three-way valve 2-4 are all connected to the circular connector 2-5, and the circular connector 2-5 is connected to the control system to provide power and control signals for the device. <l

[0030] The composition of the fraction collection component 3 is as Figure 3As shown in the figure, it includes a fixed base 3-1 and several collection containers 3-3. The collection containers 3-3 are fixed on the fixed base 3-1 through the mounting holes on the fixed base 3-1 and the spring positioning pins 3-2. The fixed base 3-1 is installed on the fixed bracket 1. In this embodiment, two rows of 10 collection containers 3-3 are provided, which are arranged on both sides of the flow path control component 2.

[0031] The structure of a single collection container 3-3 is as Figure 4 shown, and it includes a screw-mouth test tube 3-3-1, a spray connection assembly, and a fraction collection connection assembly; the spray connection assembly is connected to the top end of the screw-mouth test tube 3-3-1 through a thread, and includes a spray head 3-3-2, a first washer 3-3-3, a first adapter 3-3-4, a first end cap 3-3-5, and a first joint 3-3-6 that are sequentially connected and assembled together; the fraction collection connection assembly is connected to the bottom end of the screw-mouth test tube 3-3-1 through a thread, and includes a second washer 3-3-7, a second adapter 3-3-8, a second end cap 3-3-9, and a second joint 3-3-10 that are sequentially connected and assembled together. The first joint 3-3-6 is connected to a cleaning liquid outlet of the spray control multi-way valve 2-2 through a pipeline, and the spray head 3-3-2 can spray the cleaning liquid to clean the inner wall of the screw-mouth test tube 3-3-1. The second joint 3-3-10 is connected to a distillate outlet of the fraction collection control multi-way valve 2-3 through a pipeline.

[0032] The full-automatic chromatographic distillate collection device further includes a control system for realizing the automatic control of the collection device.

[0033] Generally speaking, the above full-automatic chromatographic distillate collection device can be automatically operated through the following steps:

[0034] When fraction collection is required, control the common end of the two-way three-way valve 2-4 to communicate with the distillate inlet pipeline 4. The liquid chromatograph injects the distillate into the distillate inlet pipeline 4, flows out from its common end through the two-way three-way valve 2-4, and flows into the common end of the fraction collection control multi-way valve 2-3. The program controls the fraction collection control multi-way valve 2-3 to sequentially connect its common end with its 10 distillate outlets, and the distillate sequentially enters the 10 collection containers 3-3;

[0035] When automatic fraction merging is required, select the number of the collection container 3-3 where the target product is located in the control system, control the common end of the two-way three-way valve 2-4 to communicate with the distillate outlet pipeline 5, and the fraction collection control multi-way valve 2-3 is sequentially switched to the collection container 3-3 corresponding to this number. The distillate in this collection container 3-3 flows into the corresponding branch of the fraction collection control multi-way valve, flows out from the common end of the fraction collection control multi-way valve 2-3 and into the common end of the two-way three-way valve 2-4, and finally flows out from the distillate outlet pipeline 5;

[0036] When the fraction collection container 3-3 needs to be cleaned, the program controls the common end of the spray control multi-way valve 2-2 to communicate with a cleaning liquid outlet. The cleaning liquid enters the common end of the spray control multi-way valve 2-2 through the cleaning liquid inlet pipe 6, flows through the branch of the spray control multi-way valve 2-2 connecting the collection container 3-3, and finally sprays out from the spray head 3-3-2. The cleaning liquid sprayed out from the spray head 3-3-2 can impact the inner wall of the screw mouth test tube 3-3-1 and enter the collection container 3-3 to clean the distillate remaining in the collection container 3-3.

[0037] Generally speaking, a working cycle includes three steps: automatic fraction collection, automatic fraction merging, and automatic cleaning.

[0038] First, perform automatic fraction collection to collect the chromatographic distillate according to the set conditions.

[0039] After the chromatographic work is completed, perform automatic fraction merging as needed to merge the distillates containing the target compound, which is convenient for subsequent operations such as evaporation to remove the solvent. When performing automatic fraction merging, the cleaning is usually intermittently turned on to increase the yield of the target product.

[0040] After automatic fraction merging, the remaining waste liquid is sucked out from the distillate outlet pipe 5, and automatic cleaning is performed. Finally, the cleaning liquid is also sucked out from the distillate outlet pipe 5.

[0041] Thus, a cycle is completed.

[0042] It should be emphasized that the purpose of publishing the embodiments is to further help understand the connotation and extension of the present invention. However, those skilled in the art can understand that various substitutions and modifications are possible without departing from the present invention and the appended claims. Therefore, the present invention should not be limited to the content disclosed in the embodiments, and the scope of protection claimed by the present invention is subject to the scope defined by the claims.

Claims

1. An automatic chromatographic distillate collection device, comprising a fixed bracket and a flow path control component and a fraction collection component mounted on the fixed bracket, wherein, The fraction collection component includes a plurality of collection containers, and these collection containers are respectively connected to the flow path control component through different branch paths; characterized in that at least one fraction collection control multi-way valve, one spray control multi-way valve and one two-way three-way valve are arranged in the flow path control component, the common end of the fraction collection control multi-way valve is connected to the common end of the two-way three-way valve, and the remaining two ports of the two-way three-way valve are respectively connected to a distillate inlet pipe and a distillate outlet pipe; the multiple outlets of the fraction collection control multi-way valve are respectively connected to different collection containers through different distillate branch paths; the common end of the spray control multi-way valve is connected to a cleaning liquid inlet pipe, and its multiple outlets are respectively connected to different collection containers through different cleaning liquid branch paths.

2. The fully automatic chromatographic eluate collection device according to claim 1, wherein The flow path control component further includes a housing and a connector, the fraction collection control multi-way valve and the spray control multi-way valve are electric valves, and the two-way three-way valve is a solenoid valve, and all are electrically connected to an external control system through the connector.

3. The fully automatic chromatographic distillate collection device according to claim 2, characterized in that, The main bodies of the fraction collection control multi-way valve and the spray control multi-way valve are located inside the housing, the outlet of the fraction collection control multi-way valve is located on the bottom surface of the housing, and the outlet of the spray control multi-way valve is located on the top surface of the housing; the two-way three-way valve is arranged on one side surface of the housing, close to the fraction collection control multi-way valve.

4. The fully automatic chromatographic eluate collection device according to claim 1, wherein The top end of the collection container is connected to the outlet of the spray control multi-way valve through a cleaning liquid branch path, and the bottom end is connected to the outlet of the fraction collection control multi-way valve through a distillate branch path.

5. The fully automatic chromatographic eluate collection device according to claim 4, wherein, The collection container includes a screw-mouth test tube, a spray connection assembly and a fraction collection connection assembly. Among them, the spray connection assembly is connected to the top end of the screw-mouth test tube through a thread, and includes a spray head, a first gasket, a first adapter, a first end cap and a first joint connected and assembled in sequence, and the first joint is connected to an outlet of the spray control multi-way valve through a cleaning liquid branch path; the fraction collection connection assembly is connected to the bottom end of the screw-mouth test tube through a thread, and includes a second gasket, a second adapter, a second end cap and a second joint connected and assembled in sequence, and the second joint is connected to an outlet of the fraction collection control multi-way valve through a distillate branch path.

6. The fully automatic chromatographic eluate collection device according to claim 1, wherein The fraction collection component includes a plurality of collection containers and a fixed base, and the collection containers are fixed on the fixed base through the mounting holes and spring positioning pins on the fixed base.

7. The fully automatic chromatographic eluate collection device according to claim 1, wherein, The fraction collection control multi-way valve and the spray control multi-way valve are six-way valves, eight-way valves, ten-way valves or twelve-way valves. Correspondingly, the fraction collection component includes 6, 8, 10 or 12 collection containers, and these collection containers are divided into two rows and are arranged on both sides of the flow path control component.

8. The operation method of the fully automatic chromatographic distillate collection device according to any one of claims 1 to 7, includes: When performing fraction collection, the common end of the two-way three-way valve is controlled to connect the distillate into the pipeline. The liquid chromatograph pumps the distillate into the distillate inlet pipeline, flows out from its common end through the two-way three-way valve, and flows into the common end of the multi-way valve for fraction collection control. The program controls the multi-way valve for fraction collection control to sequentially connect its common end with its multiple outlets, and the distillate sequentially enters multiple collection containers; When performing automatic fraction merging, the collection container where the target product is located is selected, and the common end of the two-way three-way valve is controlled to connect the distillate outlet pipeline. The multi-way valve for fraction collection control is sequentially switched to the distillate branch connecting the selected collection container. The distillate in the selected collection container flows into the corresponding distillate branch, then flows out from the common end of the multi-way valve for fraction collection control, and flows into the common end of the two-way three-way valve, and finally flows out from the distillate outlet pipeline; When performing cleaning of the collection container, the program controls the common end of the multi-way valve for spray control to be sequentially connected with its outlets. The cleaning liquid enters the common end of the multi-way valve for spray control through the cleaning liquid inlet pipeline, then flows through each cleaning liquid branch into the collection container to clean the collection container; the cleaned solution sequentially passes through the distillate branch, the multi-way valve for fraction collection control and the two-way three-way valve, and flows out from the distillate outlet pipeline.

9. The operating method according to claim 8, characterized in that, A spray head is provided at the top of the collection container, and the cleaning liquid is sprayed out from the spray head to wash the inner wall of the collection container and enter the collection container to clean the distillate remaining in the collection container.

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