WO2021227546A1

WO2021227546A1 - Multifunctional sample extraction flow path and method

Info

Publication number: WO2021227546A1
Application number: PCT/CN2021/071354
Authority: WO
Inventors: 林春生; 戴相辉; 陈克彦; 郭宝辉; 林志杰
Original assignee: 睿科集团(厦门)股份有限公司
Priority date: 2020-05-12
Filing date: 2021-01-13
Publication date: 2021-11-18

Abstract

A multifunctional sample extraction flow path, comprising a multi-channel solenoid valve (10), a rotary valve (20), an injector (30), a collection tube (40), an SPE column (50), a waste discharge tank (60), and a sample bottle (70). The multi-channel solenoid valve (10) is provided with a plurality of solvent channels controlled by the solenoid valve; the rotary valve (20) comprises positions 0, positions 1, positions 2, positions 3, and positions 4; the positions 1, positions 2, positions 3, and positions 4 are distributed on the edge of the rotary valve (20), and the positions 0 are arranged in the middle of the rotary valve (20); the injector (30) is connected to a position 0; the collection tube (40) is connected to a position 1; the outlet of the multi-channel solenoid valve (10) is connected to a position 2; the inlet of the SPE column (50) is connected to a position 3; the outlet of the SPE column (50) can selectively guide to the collection tube (40) or the waste discharge tank (60); the sample bottle (70) is connected to a position 4; the rotary valve (20) is provided with radial channels, and the positions 0 are communicated with the other positions by means of the radial channels. According to the extraction flow path, continuous and automatic extraction operation of small-volume or large-volume samples can be implemented, and the extraction efficiency and convenience are improved.

Description

Multifunctional sample extraction flow path and method

This case has two priority rights (priority number 202010395244.X, priority date 2020-5-12, priority number 202020772149.2, priority date 2020-5-12)

Technical field

The invention relates to the technical field of experimental extraction, in particular to a multifunctional sample extraction flow path and method.

Background technique

The existing extraction technology is to achieve extraction through a special extraction column (SPE column), and the instrument to achieve this method is relatively simple. Extraction cartridges, for large-volume samples, this process takes a long time and is not convenient to use. There are still many areas for improvement. Although extraction is a well-known process technology, for most laboratories and factories, there is still a long-term demand for more comprehensive extraction technology.

Summary of the invention

The purpose of the present invention is to provide a multifunctional sample extraction flow path and method, which can realize the continuity and automatic extraction operation of small-volume or large-volume samples, and improve the extraction efficiency and convenience.

To achieve the above objective, the solution of the present invention is: a multi-channel sample extraction flow path, including a multi-channel solenoid valve, a rotary valve, a syringe, a collection tube, an SPE column, a waste tank, a sample bottle, and the multi-channel solenoid valve The valve is provided with a variety of solvent channels controlled by solenoid valves. The rotary valve includes No. 0 position, No. 1 position, No. 2 position, No. 3 position and No. 4 position. Position and position 4 are distributed on the outer edge of the rotary valve, the position 0 is set in the middle of the rotary valve, the syringe is connected to position 0, the collection tube is connected to position 1, and the outlet of the multi-channel solenoid valve is connected to 2. No. 3, the inlet of the SPE column is connected to No. 3, the outlet of the SPE column can choose to flow to a collection tube or a waste discharge tank, and the sample bottle is connected to No. 4; the rotary valve is provided with a radial channel, The number 0 position and each number position are communicated with each other through the radial channel.

Preferably, the rotary valve is further provided with an edge channel, the edge channel is arranged on the side of the outer end of the radial channel, and the edge channel is used to connect two adjacent numbers on the edge of the rotary valve.

Preferably, the rotary valve adopts a three-turn twelve-way valve, the three-turn twelve-way valve includes three sets of indexing positions, and each set of indexing positions includes a 0 position, a 1 position, a second position, A No. 3 position, a No. 4 position, a radial channel and an edge channel, a total of twelve positions, three radial channels and three edge channels, the three sets of indexing rings are evenly distributed on the rotary valve .

Preferably, it further includes a three-way solenoid valve, the multi-channel solenoid valve is also provided with a nitrogen channel controlled by the solenoid valve, the nitrogen channel is connected to the sample bottle, and the three-way solenoid valve is arranged between the nitrogen channel and the sample bottle .

A multifunctional sample extraction method, including the following steps:

1. Activate the SPE column, put the sample into the sample bottle, seal the sample bottle, and then turn it upside down. Next, rotate the rotary valve. The rotary valve connects position 0 and position 2 through the radial channel. Open the solenoid valve to select the activator, and suck liquid, turn the valve again, turn the valve to switch to position 0 and connect to position 3. The syringe pushes the liquid, and the solvent pushes the activator through the SPE column to the waste tank through the No. 3 port. Repeat to complete the activation of the activated SPE column;

2. Load the sample, switch the rotary valve to position 0 to connect to position 4, the syringe draws the sample from the sample bottle, rotate the rotary valve again, the rotary valve switches to position 0 to connect to position 3, the syringe pushes the liquid, and the sample passes through the SPE column Go to the waste discharge tank and complete the sample loading;

3. Rinse, rotate the rotary valve, the rotary valve is switched to position 0 to connect to position 2, the syringe selects the eluent from the multi-port solenoid valve through the No. 2 port, and sucks the liquid, rotates the rotary valve again, and the rotary valve switches to 0 The number position is connected to the No. 3 position, the syringe pushes the liquid, and the eluent is pushed through the SPE column to the waste discharge tank through the No. 3 port, and repeats so as to complete the leaching;

4. To elute, rotate the valve to switch to position 0 and connect to position 2. The syringe selects a different eluent again from the multi-port solenoid valve through the No. 2 port, and sucks the liquid, and then rotates the valve again to turn the valve. Switch to No. 0 and connect to No. 3, the syringe pushes the liquid, and the target extract is pushed through the SPE column to the collection tube through the No. 3 port to complete the elution.

Preferably, the concentration step can be performed after the elution step, and the collection tube is externally provided with a nitrogen pipeline controlled by a two-way solenoid valve. After the SPE column is eluted, the two-way solenoid valve is opened, and the nitrogen gas can pass through the two-way solenoid valve. The solenoid valve is blown directly onto the liquid surface of the collection tube to concentrate until the concentration reaches the specified volume.

Preferably, the dissolution step can be performed after the elution step. After the target extract is collected in the collection tube, the rotary valve is rotated, and the rotary valve is switched to position 0 to communicate with position 2. The valve selects the required solvent and aspirates the liquid, then rotates the rotary valve again, and the rotary valve switches to position 0 to communicate with position 1. The syringe pushes the liquid, and the required solvent is directly dropped into the collection tube through the No. 1 port to complete the transfer.

After adopting the above scheme, the beneficial effect of the present invention is: the multi-channel solenoid valve of the extraction flow path can be loaded with a variety of solvents required for extraction, which is convenient for uniformly replenishing various solvents. The solvents include activators, eluents, eluents, etc. Wait. The radial channel on the rotary valve in this case is a channel extending from the middle to the edge, so the switching rotary valve can control the central position 0 and the edge positions (position 1, position 2, position 3, and position 4). Connected, by flexibly changing the operating sequence of the communication channels, continuous extraction operations for both small-volume samples and large-volume samples can be realized. The degree of automation is more obvious, which improves the inconvenience of the existing solid phase extraction instrument and improves Extraction efficiency.

Description of the drawings

FIG. 1 is a schematic diagram of the structure of the first state of an embodiment of the present invention.

Fig. 2 is a schematic structural diagram of a second state of an embodiment of the present invention.

Fig. 3 is a schematic structural diagram of the third state of an embodiment of the present invention.

Fig. 4 is a schematic structural diagram of a fourth state of an embodiment of the present invention.

Fig. 5 is a schematic structural diagram of a fifth state of an embodiment of the present invention.

Label description:

Multi-channel solenoid valve 10, solvent channel 101, nitrogen channel 102, air channel 103, rotary valve 20, radial channel 201, edge channel 202, syringe 30, collection tube 40, SPE column 50, waste tank 60, sample bottle 70 , Three-way solenoid valve 80, two-way solenoid valve 90, nitrogen pipeline 901.

Detailed ways

The present invention will be described in detail below with reference to the drawings and specific embodiments.

The present invention provides a multifunctional sample extraction flow path, as shown in Figure 1, comprising a multi-channel solenoid valve 10, a rotary valve 20, a syringe 30, a collection tube 40, an SPE column 50, a waste tank 60, a sample bottle 70, three Two-way solenoid valve 80 and a two-way solenoid valve 90. The multi-channel solenoid valve 10 is provided with multiple solvent channels 101 controlled by the solenoid valve. The rotary valve 20 includes No. 0 position, No. 1 position, No. 2 position, 3 No. and No. 4 positions, the No. 1, No. 2, No. 3 positions, and No. 4 positions are distributed on the outer edge of the rotary valve 20, the No. 0 position is arranged in the middle of the rotary valve 20, and the syringe 30 is connected to 0 No. 1, the collection tube 40 is connected to the No. 1, the outlet of the multi-channel solenoid valve 10 is connected to the No. 2, the inlet of the SPE column 50 is connected to the No. 3, and the outlet of the SPE column 50 can select the flow direction to collect The tube 40 or the waste tank 60, the sample bottle 70 is connected to the 4th position.

The multi-channel solenoid valve 10 in this case can be loaded with a variety of solvents required for extraction, which is convenient for uniformly replenishing various solvents. The solvents include activators, eluents, eluents, and so on.

The rotary valve 20 is provided with a radial channel 201 and an edge channel 202, and the diameter is passed between the 0 position and the other positions (position 1, position 2, position 3, and position 4). It is connected to the channel 201, and the edge channel 202 is arranged on the side of the outer end of the radial channel 201. The edge channel 202 is used to connect the two adjacent positions of the edge of the rotary valve 20 (position 1, position 2, and position 2). And position 3, position 3 and position 4).

The rotary valve 20 adopts a three-turn twelve-way valve. The three-turn twelve-way valve includes three sets of indexing positions. Number position, a number position, a radial channel 201 and an edge channel 202, a total of twelve number positions, three radial channels 201 and three edge channels 202, the three sets of indexing rings are evenly distributed in the rotation The valve 20 is on.

The number position mentioned in this case means the gear position. For example, position 1 is the first gear position, and position 2 is the second gear position...., it is hereby explained that the position 0 is set at the rotary valve 20 Therefore, in the fan-shaped active area of each group of indexing, the 0 position is basically kept in the middle. When the rotary valve 20 is rotated, the outer end of the radial channel 201 continuously changes to communicate with other positions, and the radial channel 201 The inner end is connected to position 0, so as to realize the communication combination of the syringe 30 and the instrument, and obtain the combined effect of different flow paths.

The present invention also provides a multifunctional sample extraction method, including the following steps:

1. The SPE column 50 is activated, the sample is loaded into the sample bottle 70, the sample bottle 70 is capped, and then turned upside down. Next, the rotary valve 20 is rotated. With reference to Figs. 2 and 3, the rotary valve 20 communicates with No. 0 through the radial channel 201 Position and position 2 (state 2), the syringe 30 selects the activator from the multi-channel solenoid valve 10 through the No. 2 port, and sucks the liquid, then rotates the rotary valve 20 again, and the rotary valve 20 switches to the position 0 to connect to the position 3 (state (3) The syringe 30 pushes the liquid, and the solvent pushes the activator through the SPE column 50 to the waste tank 60 through the No. 3 port, and repeats this process to complete the activation of the activated SPE column 50.

2. Load the sample, combined with Figures 4 and 3, switch the rotary valve 20 to position 0 and connect to position 4 (state 4), the syringe 30 draws the sample from the sample bottle 70, and rotates the rotary valve 20 again, and the rotary valve 20 switches to The position 0 is connected to the position 3 (state 3), the syringe 30 pushes the liquid, and the sample passes through the SPE column 50 to the waste tank 60 to complete the sample loading.

The multi-channel solenoid valve 10 is also provided with a nitrogen channel 102 and an air channel 103 controlled by a solenoid valve, the nitrogen channel 102 is connected to the sample bottle 70, and the three-way solenoid valve 80 is arranged between the nitrogen channel 102 and the sample bottle 70 between. The existing solid phase extraction instrument cannot pass the column quickly and continuously. Compared with the ordinary sample loading speed, the present invention can realize the positive pressure auxiliary syringe 30 sample loading and the positive pressure rapid sample loading to achieve the purpose of accelerating the sample loading speed. The sample loading process of the positive pressure auxiliary syringe 30 is specifically as follows: first rotate the rotary valve 20. With reference to Figs. 4 and 3, the rotary valve 20 communicates with position 0 and position 4 (state 4) through a radial channel 201. At the same time, three The solenoid valve 80 opens the NC COM port, and nitrogen can flow from the nitrogen channel 102 to the sample bottle 70. Positive pressure is generated in the sample bottle 70 to accelerate the suction speed of the syringe 30, and then switch the rotary valve to position 0 and connect to position 3. (State 3), the syringe 30 pushes the liquid, and the sample can pass through the SPE column 50 to the waste tank 60 for sample loading. The positive pressure auxiliary syringe 30 is suitable for sample loading with high density or low boiling point, which cannot be loaded quickly and needs to be loaded stably.

The operation process of the positive pressure rapid sample loading is specifically as follows: first rotate the three-turn twelve-way valve, as shown in FIG. When the three-way solenoid valve 80 opens the NC port COM, nitrogen can flow from the nitrogen channel 102 to the sample bottle 70, generate positive pressure in the sample bottle 70, and then directly positive pressure to the SPE column 50 (membrane), and finally to the waste tank 60. Compared with the positive pressure auxiliary syringe 30 for sample loading, the positive pressure rapid sample loading does not need to pass through the syringe 30, and is suitable for samples that require very fast loading, such as membrane extraction.

3. Rinse, rotate the rotary valve 20, combined with Fig. 2 and Fig. 3, the rotary valve 20 is switched to the 0 position to connect to the 2 position (state 2), the syringe 30 selects the eluent from the multi-channel solenoid valve 10 through the No. 2 port , And aspirate liquid, turn the rotary valve 20 again, the rotary valve 20 is switched to position 0 to connect to position 3 (state 3), the syringe 30 pushes the liquid, and the eluent is pushed through the SPE column 50 through the No. 3 port to the waste discharge tank 60. Repeat this process to complete the rinse;

4. Elution, rotate the rotary valve 20, combined with Fig. 2 and Fig. 3, the rotary valve 20 is switched to position 0 and connected to position 2 (state 2), and the syringe 30 selects a different wash from the multi-channel solenoid valve 10 through the No. 2 port. Remove the agent and aspirate the liquid, then turn the rotary valve 20 again, the rotary valve 20 switches to position 0 and connects to position 3 (state 3), the syringe 30 pushes the liquid, and the target extract is pushed through the SPE column 50 through the No. 3 port. Collect tube 40 to complete the elution.

In one embodiment, between the rinsing step and the elution step, there is also a drying step of the SPE column 50. The process of this step is to rotate the rotary valve 20. As shown in FIG. 4, the rotary valve 20 passes through the edge channel 202. Connect No. 2 and No. 3 positions (state 4). At this time, open the nitrogen channel 102 of the multi-channel solenoid valve, and the nitrogen can pass through the 2nd-3rd-SPE column 50 for nitrogen blowing to dry the SPE Column 50 packing effect.

As a further improvement, a concentration step can be performed after the elution step. The collection tube 40 is externally provided with a nitrogen pipeline 901 controlled by a two-way solenoid valve 90. After the SPE column 50 is eluted, the two-way solenoid valve is turned on. Valve 90, the nitrogen can be blown directly onto the liquid surface of the collection pipe 40 through the two-way solenoid valve 90 for concentration until the concentration reaches the specified capacity.

As a further improvement, the dissolution step can be performed after the elution step. After the target extract is collected in the collection tube 40, the rotary valve 20 is rotated. With reference to Figures 2 and 1, the rotary valve 20 is switched to position 0 to communicate No. 2 position (state 2), the syringe 30 selects the required solvent from the multi-channel solenoid valve 10 through the No. 2 port, and sucks the liquid, and then rotates the rotary valve 20 again, and the rotary valve 20 switches to the 0th position and connects to the 1st position (state 1) The syringe 30 pushes the liquid, and drops the required solvent directly into the collection tube 40 through the No. 1 port to complete the transfer.

The extraction flow path can realize the extraction action of SPE column activation-multi-function loading-rinsing-SPE column drying-elution-dissolution or concentration at one time. In this case, the radial channel 201 on the rotary valve 20 is from the middle to the The edge extension channel, the edge channel 202 is a channel with two adjacent positions on the edge. Therefore, the switching rotary valve 20 can control the central position 0 and the edge positions (position 1, position 2, position 3, and position 4). It can also connect to position 1 and position 2 (state 3), position 2 and position 3 (state 4), position 3 and position 4 (state 5), and then flexibly change the communication channel The sequence of operations can realize continuous extraction operations for small-volume samples or large-volume samples. The degree of automation is more obvious, which improves the inconvenience of the existing solid phase extraction instrument and improves the extraction efficiency.

The above descriptions are only preferred embodiments of the present invention, and are not a limitation to the design of this case. All equivalent changes made in accordance with the key design of this case fall within the scope of protection of this case.

Claims

A multi-functional sample extraction flow path, which is characterized in that it comprises a multi-channel solenoid valve, a rotary valve, a syringe, a collection tube, an SPE column, a waste tank, and a sample bottle. The multi-channel solenoid valve is provided with a solenoid valve controlled Multiple solvent channels, the rotary valve includes position 0, position 1, position 2, position 3, and position 4. The position 1, position 2, position 3, and position 4 are distributed in the rotation On the outer edge of the valve, the 0 position is set in the middle of the rotary valve, the syringe is connected to the 0 position, the collection tube is connected to the 1 position, the outlet of the multi-channel solenoid valve is connected to the 2 position, and the SPE column The inlet is connected to position 3, the outlet of the SPE column can choose to flow to the collection tube or the waste tank, the sample bottle is connected to position 4; the rotary valve is provided with a radial channel, and the 0 position and each number The positions are communicated with each other through the radial channel.
The multifunctional sample extraction flow path according to claim 1, wherein the rotary valve is further provided with an edge channel, the edge channel is arranged on the side of the outer end of the radial channel, and the edge channel is used to communicate with the rotation Two positions adjacent to the edge of the valve.
The multifunctional sample extraction flow path according to claim 2, wherein the rotary valve adopts a three-turn twelve-way valve, and the three-turn twelve-way valve includes three sets of indexing, and each set of indexing Including a No. 0 position, a No. 1 position, a No. 2 position, a No. 3 position, a No. 4 position, a radial channel and an edge channel, a total of twelve positions, three radial channels and three In the edge channel, the three groups of indexing rings are evenly distributed on the rotary valve.
The multi-functional sample extraction flow path of claim 1, further comprising a three-way solenoid valve, the multi-channel solenoid valve is also provided with a nitrogen channel controlled by the solenoid valve, and the nitrogen channel is connected to the sample bottle , The three-way solenoid valve is arranged between the nitrogen channel and the sample bottle.
A multifunctional sample extraction method relates to the above-mentioned multifunctional sample extraction flow path. The method includes the following steps:

1. Activate the SPE column, put the sample into the sample bottle, seal the sample bottle, and then turn it upside down. Next, rotate the rotary valve. The rotary valve connects position 0 and position 2 through the radial channel. Open the solenoid valve to select the activator, and suck liquid, turn the valve again, turn the valve to switch to position 0 and connect to position 3. The syringe pushes the liquid, and the solvent pushes the activator through the SPE column to the waste tank through the No. 3 port. Repeat to complete the activation of the activated SPE column;

2. Load the sample, switch the rotary valve to position 0 to connect to position 4, the syringe draws the sample from the sample bottle, rotate the rotary valve again, the rotary valve switches to position 0 to connect to position 3, the syringe pushes the liquid, and the sample passes through the SPE column Go to the waste discharge tank and complete the sample loading;

3. Rinse, rotate the rotary valve, the rotary valve is switched to position 0 to connect to position 2, the syringe selects the eluent from the multi-port solenoid valve through the No. 2 port, and sucks the liquid, rotates the rotary valve again, and the rotary valve switches to 0 The number position is connected to the No. 3 position, the syringe pushes the liquid, and the eluent is pushed through the SPE column to the waste discharge tank through the No. 3 port, and repeats so as to complete the leaching;

4. To elute, rotate the valve to switch to position 0 and connect to position 2. The syringe selects a different eluent again from the multi-port solenoid valve through the No. 2 port, and sucks the liquid, and then rotates the valve again to turn the valve. Switch to No. 0 and connect to No. 3, the syringe pushes the liquid, and the target extract is pushed through the SPE column to the collection tube through the No. 3 port to complete the elution.
A multifunctional sample extraction method according to claim 5, characterized in that: after the elution step, a concentration step can be performed, and the collection tube is externally provided with a nitrogen pipeline controlled by a two-way solenoid valve, and the SPE column After elution, open the two-way solenoid valve, and the nitrogen can be blown directly onto the liquid surface of the collection tube through the two-way solenoid valve for concentration until it is concentrated to the specified volume.
A multifunctional sample extraction method according to claim 5, characterized in that: after the elution step, a dissolution step can be performed, and when the target extract is collected in the collection tube, the rotary valve is rotated, and the rotary valve is switched to No. 0 Position is connected to No. 2, the syringe selects the required solvent from the multi-way solenoid valve through the No. 2 port, and sucks the liquid, and then rotates the rotary valve again, and the valve is switched to No. 0 to connect to the No. 1 position. The syringe pushes the liquid and passes through No. 1. Drop the required solvent directly into the collection tube to complete the transfer.