A one-way / two-way circulation fluorescence detection device and a control method and system thereof

Abstract

The application discloses a one-way / two-way circulation fluorescence detection device and a control method and system thereof, comprising a mobile phase bottle, a plurality of multi-way valves, a current-carrying unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit, different pipes of the plurality of multi-way valves are connected, different detection flow paths are formed between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle, and the detection flow path comprises any one of a one-way fluorescence detection flow path, a one-way circulation fluorescence detection flow path, a two-way circulation fluorescence first detection flow path or a two-way circulation fluorescence second detection flow path; the current-carrying unit is used for controlling the liquid flow rate of the detection flow path; and the fluorescence detection unit is used for detecting the liquid spectrum in the fluorescence detection cell. The embodiment of the application can improve the detection accuracy, reduce the cost and is simple to operate, and can be widely applied to the field of fluorescence detection technology.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of fluorescence detection technology, and in particular to a one-way / two-way circulation fluorescence detection device and a control method and system thereof. BACKGROUND

[0002] Fluorescence detection is widely used in many fields such as environmental analysis, food and drug detection, or clinical chemistry. Traditional methods of fluorescence detection (such as standard titration, chromatography and spectral analysis) usually require a large amount of manual operation, which is time-consuming and prone to errors. These methods usually consume a large amount of reagents and samples, which is not conducive to cost control. SUMMARY

[0003] Therefore, in order to solve one of the above problems, the purpose of the embodiments of the present application is to provide a one-way / two-way circulation fluorescence detection device and a control method and system thereof, which can improve detection accuracy, reduce cost and be simple to operate.

[0004] In one aspect, the embodiments of the present application provide a one-way / two-way circulation fluorescence detection device, comprising a mobile phase bottle, a plurality of multi-way valves, a liquid carrying unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit, different pipes of the plurality of multi-way valves are connected, different detection flow paths are formed between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle, and the detection flow path comprises any one of a one-way fluorescence detection flow path, a one-way circulation fluorescence detection flow path, a two-way circulation fluorescence first detection flow path or a two-way circulation fluorescence second detection flow path; wherein,

[0005] The liquid carrying unit is configured to control the liquid flow rate of the detection flow path.

[0006] The fluorescence detection unit is configured to detect the spectrum of the liquid in the fluorescence detection cell.

[0007] Optionally, the multi-way valve comprises an extension coil pipe, the extension coil pipe is arranged between two valves, and the length of the extension coil pipe is 50cm-500cm.

[0008] Optionally, the liquid carrying unit comprises any one or more of a peristaltic pump, a plunger pump or a syringe pump.

[0009] Optionally, the fluorescence detection unit comprises a light source and a fiber optic spectrometer, the light emitted by the light source passes through the fluorescence detection cell to the fiber optic spectrometer, and the wavelength range of the light source includes 300nm-600nm.

[0010] The embodiment of the present application has the following advantages: the embodiment includes a mobile phase bottle, a plurality of multi-way valves, a carrier solution unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit, different pipes of the plurality of multi-way valves are connected, different detection flow paths are formed between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle, the detection flow path includes any one of a one-way fluorescence detection flow path, a one-way circulating fluorescence detection flow path, a two-way circulating fluorescence first detection flow path or a two-way circulating fluorescence second detection flow path, the sample is injected into the carrier solution in continuous circulation, the mixing and reaction are more uniform, more complex sample processing and analysis can be achieved, the detection accuracy is improved, in addition, the circulation can save materials and reduce costs.

[0011] In another aspect, the embodiment of the present application provides a control method of a one-way / two-way circulating fluorescence detection device, which applies the one-way / two-way circulating fluorescence detection device described above, and includes the following steps:

[0012] obtaining a control instruction of a detection flow path;

[0013] controlling the pipe connection of the plurality of multi-way valves according to the control instruction to obtain a detection flow path corresponding to the control instruction.

[0014] Optionally, the one-way / two-way circulating fluorescence detection device includes a plurality of six-way valves, and the step of controlling the pipe connection of the plurality of multi-way valves according to the control instruction includes the following steps:

[0015] if the detection flow path corresponding to the control instruction is a one-way fluorescence detection flow path, controlling the liquid of the mobile phase bottle to flow through the first valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the second valve of the third six-way valve, the sample injection valve, the fluorescence detection cell, the first valve and the second valve of the fourth six-way valve, the third valve and the fourth valve of the second six-way valve, the third valve and the fourth valve of the first six-way valve and enter the waste liquid bottle.

[0016] Optionally, the one-way / two-way circulating fluorescence detection device includes a plurality of six-way valves, and the step of controlling the pipe connection of the plurality of multi-way valves according to the control instruction includes the following steps:

[0017] if the detection flow path corresponding to the control instruction is a one-way circulating fluorescence detection flow path, controlling the liquid of the flow pipe to flow between the third valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the second valve of the third six-way valve, the sample injection valve, the fluorescence detection cell, the first valve and the second valve of the fourth six-way valve and the third valve and the fourth valve of the second six-way valve.

[0018] Optionally, the one-way / two-way circulating fluorescence detection device includes a plurality of six-way valves, and the step of controlling the pipe connection of the plurality of multi-way valves according to the control instruction includes the following steps:

[0019] If the control instruction corresponds to a bidirectional circulation fluorescence first detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve, the fourth valve, the extension coil pipe path, the second valve, the third valve, the fourth valve of the third six-way valve, the sample valve, the fluorescence detection cell, the first valve, the fourth valve, the extension coil pipe path, the third valve, the second valve of the fourth six-way valve, the third valve and the fourth valve of the second six-way valve, the third valve and the fourth valve of the first six-way valve, and enters the waste liquid bottle.

[0020] Optionally, the unidirectional / bidirectional circulation fluorescence detection device comprises a plurality of six-way valves, and the pipeline connection of the plurality of six-way valves is controlled according to the control instruction, comprising:

[0021] If the control instruction corresponds to a bidirectional circulation fluorescence second detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve and the second valve of the first six-way valve, the first valve and the third valve of the second six-way valve, the second valve, the third valve, the extension coil pipe path, the fourth valve and the first valve of the fourth six-way valve, the fluorescence detection cell, the sample valve, the second valve, the third valve, the extension coil pipe path, the fourth valve and the first valve of the third six-way valve, the second valve and the fifth valve of the second six-way valve, and enters the waste liquid bottle.

[0022] In another aspect, an embodiment of the present application provides a control system of a unidirectional / bidirectional circulation fluorescence detection device, comprising an industrial personal computer and the unidirectional / bidirectional circulation fluorescence detection device described above, wherein,

[0023] The industrial personal computer is configured to execute the control method described above.

[0024] The embodiment of the present application has the following beneficial effects: in the control process, the control instruction of the detection flow path is obtained, and the pipeline connection of the plurality of six-way valves is automatically controlled according to the control instruction to obtain the detection flow path corresponding to the control instruction. Only the control instruction of the detection flow path needs to be obtained, and the operation is simple. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 FIG. 1 is a structural schematic diagram of a unidirectional / bidirectional circulation fluorescence detection device provided by an embodiment of the present application;

[0026] Figure 2 FIG. 2 is a step flowchart of a control method of a unidirectional / bidirectional circulation fluorescence detection device provided by an embodiment of the present application;

[0027] Figure 3 FIG. 3 is a schematic diagram of a unidirectional fluorescence detection flow path provided by an embodiment of the present application;

[0028] Figure 4is a schematic diagram of a one-way circulating fluorescence detection flow path provided by an embodiment of the present application;

[0029] Figure 5 is a schematic diagram of a two-way circulating fluorescence first detection flow path provided by an embodiment of the present application;

[0030] Figure 6 is a schematic diagram of a two-way circulating fluorescence second detection flow path provided by an embodiment of the present application;

[0031] Figure 7 is a schematic diagram of a one-way / two-way circulating fluorescence detection result provided by an embodiment of the present application;

[0032] Figure 8 is a schematic diagram of another one-way / two-way circulating fluorescence detection result provided by an embodiment of the present application;

[0033] Figure 9 is a schematic diagram of another one-way / two-way circulating fluorescence detection result provided by an embodiment of the present application;

[0034] Figure 10 is a schematic diagram of another one-way / two-way circulating fluorescence detection result provided by an embodiment of the present application. DETAILED DESCRIPTION

[0035] The present application will be further described below in conjunction with the accompanying drawings and specific embodiments. For the step numbers in the following embodiments, they are only set for the convenience of description and explanation, and the order between the steps is not limited in any way, and the execution order of each step in the embodiments can be adaptively adjusted according to the understanding of those skilled in the art.

[0036] As shown in Figure 1 , the present application provides a one-way / two-way circulating fluorescence detection device, comprising a mobile phase bottle, a plurality of multi-way valves, a current-carrying unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit, different pipes of the plurality of multi-way valves are connected, different detection flow paths are formed between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle, and the detection flow path comprises any one of a one-way fluorescence detection flow path, a one-way circulating fluorescence detection flow path, a two-way circulating fluorescence first detection flow path or a two-way circulating fluorescence second detection flow path; wherein,

[0037] The current-carrying unit is used to control the liquid flow rate of the detection flow path;

[0038] The fluorescence detection unit is used to detect the spectrum of the liquid in the fluorescence detection cell.

[0039] The mobile phase bottle is used for loading the carrier solution, the detection sample is injected through the sample injection unit, the carrier solution and the detection sample flow in the detection flow path of the unidirectional / bidirectional circulation fluorescence detection device, and after the detection is completed, the waste liquid is collected in the waste liquid bottle.

[0040] The sample injection unit further comprises a sample injection needle connected with the sample inlet, and the sample in the sample injection needle is the detection sample. The sample injection unit further comprises a burette with a capacity of 5-200 μL.

[0041] It should be noted that the number of multi-way valves and the number of valves are determined according to actual application, and the embodiment is not specifically limited; for example, 1-6 valves. The fluorescence detection cell can be obtained by 3D printing.

[0042] The detection sample can be a polymer dye, a small molecule organic dye, a quantum dot, a fluorescent probe, a luminescent material, etc. having a fluorescence signal sample, such as Rhodamine B, Lissamine Rhodamine B, Qdot565 probe, green fluorescent protein or red fluorescent protein, etc.

[0043] Optionally, the multi-way valve comprises an extension coil pipeline, which is arranged between two valves, and the length of the extension coil pipeline is 50 cm-500 cm.

[0044] It should be noted that the length of the extension coil pipeline is determined according to actual application, and the embodiment is not specifically limited.

[0045] Optionally, the carrier liquid unit comprises any one or more of a peristaltic pump, a plunger pump or a syringe pump.

[0046] The carrier liquid unit comprises but is not limited to a peristaltic pump, a plunger pump or a syringe pump, etc., and the flow rate ranges from 10 μL / min-5 mL / min. The pipeline of the carrier liquid device can be polyether ether ketone resin, polytetrafluoroethylene or stainless steel, etc., and the length is 20-200 cm.

[0047] Optionally, the fluorescence detection unit comprises a light source and a fiber spectrometer, the light emitted by the light source passes through the fluorescence detection cell to the fiber spectrometer, and the wavelength range of the light source includes 300 nm-600 nm.

[0048] It should be noted that the wavelength of the light source is determined according to actual application, and the embodiment is not specifically limited. The light source comprises but is not limited to a laser and an LED. The light source is connected perpendicularly with the fluorescence detection cell, and the fiber spectrometer is connected with the fluorescence detection cell through an optical fiber and an optical fiber collimator.

[0049] The embodiment of the present application has the following advantages: the embodiment includes a mobile phase bottle, a plurality of multi-way valves, a carrier solution unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit, different pipes of the plurality of multi-way valves are connected to form different detection flow paths between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle, the detection flow paths include any one of a one-way fluorescence detection flow path, a one-way circulating fluorescence detection flow path, a two-way circulating fluorescence first detection flow path or a two-way circulating fluorescence second detection flow path, the sample is injected into the carrier solution in continuous circulation, the mixing and reaction are more uniform, more complex sample processing and analysis can be realized, the detection accuracy is improved, in addition, the circulation flow can save materials and reduce costs.

[0050] Referring to Figure 2 The embodiment of the present application provides a control method of a one-way / two-way circulating fluorescence detection device, and the one-way / two-way circulating fluorescence detection device is used, and the control method comprises the following steps:

[0051] S100, a control instruction of a detection flow path is acquired.

[0052] S200, according to the control instruction, pipe connections of a plurality of multi-way valves are controlled to obtain a detection flow path corresponding to the control instruction.

[0053] The detection flow path includes but is not limited to a one-way fluorescence detection flow path, a one-way circulating fluorescence detection flow path, a two-way circulating fluorescence first detection flow path or a two-way circulating fluorescence second detection flow path, each detection flow path corresponds to a control instruction. The control instruction of the detection flow path can be acquired in an interactive mode, such as an interactive interface or a case. The pipe connections of the plurality of multi-way valves include connections between different multi-way valves and connections between internal multi-way valves.

[0054] Optionally, the one-way / two-way circulating fluorescence detection device includes a plurality of six-way valves, and according to the control instruction, the pipe connections of the plurality of multi-way valves are controlled, which comprises the following steps:

[0055] If the detection flow path corresponding to the control instruction is a one-way fluorescence detection flow path, the liquid of the mobile phase bottle is controlled to pass through a first valve and a second valve of a first six-way valve, a first valve and a second valve of a second six-way valve, a first valve and a second valve of a third six-way valve, a sample injection valve, a fluorescence detection cell, a first valve and a second valve of a fourth six-way valve, a third valve and a fourth valve of the second six-way valve, a third valve and a fourth valve of the first six-way valve and enter a waste liquid bottle in sequence.

[0056] Referring to Figure 3When the pipeline is in a one-way fluorescence detection flow path state, the mobile phase bottle (6) is connected to the first valve (a1) of the first six-way valve (1), the second valve (b1) of the first six-way valve (1) is connected to the first valve (f2) of the second six-way valve, and under the power action of the peristaltic pump (7), the liquid of the mobile phase bottle sequentially passes through the first valve (f2) and the second valve (a2) of the second six-way valve (2), the first valve (f3) and the second valve (a3) of the third six-way valve (3), d4-e4 of the sample valve (4), the fluorescence detection cell (10), the first valve (c5) and the second valve (b5) of the fourth six-way valve (5), the third valve (e2) and the fourth valve (d2) of the second six-way valve (2), the third valve (c1) and the fourth valve (d1) of the first six-way valve (1), and enters the waste liquid bottle or the carrier liquid recovery system (13). Among them, Figure 3 The fluorescence detection unit (11) performs fluorescence detection on the liquid of the fluorescence detection cell (10).

[0057] Optionally, the one-way / two-way circulation fluorescence detection device includes a plurality of six-way valves, and the pipeline connection of the plurality of multi-way valves is controlled according to a control instruction, including:

[0058] If the control instruction corresponds to a one-way circulation fluorescence detection flow path, the liquid in the flow pipeline flows between the third valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the second valve of the third six-way valve, the sample valve, the fluorescence detection cell, the first valve and the second valve of the fourth six-way valve, and the third valve and the fourth valve of the second six-way valve.

[0059] Referring to Figure 3 and Figure 4 The first six-way valve (1) has an on-off mode, and after the first six-way valve (1) is switched from on to off mode, the first six-way valve (1) is switched from a1-b1, c1-d1 communication to b1-c1 communication, and the one-way fluorescence detection flow path is converted into a one-way circulation fluorescence detection flow path.

[0060] Referring to Figure 4 Under the one-way circulation fluorescence detection flow path, the liquid in the flow pipeline flows between the third valve (c1) and the second valve (b1) of the first six-way valve (1), the first valve (f2) and the second valve (a2) of the second six-way valve (2), the first valve (f3) and the second valve (a3) of the third six-way valve (3), d4-e4 of the sample valve (4), the fluorescence detection cell (10), the first valve (c5) and the second valve (b5) of the fourth six-way valve (5), and the third valve (e2) and the fourth valve (d2) of the second six-way valve (2).

[0061] Optionally, the one-way / two-way circulation fluorescence detection device includes a plurality of six-way valves, and the pipeline connection of the plurality of multi-way valves is controlled according to a control instruction, including:

[0062] If the detection flow path corresponding to the control instruction is the first bidirectional circulation fluorescence detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve, the second valve of the first six-way valve, the first valve, the second valve of the second six-way valve, the first valve, the fourth valve of the third six-way valve, the extension coil pipe, the third valve, the second valve, the sampling valve, the fluorescence detection cell, the first valve, the fourth valve of the fourth six-way valve, the extension coil pipe, the third valve, the second valve, the third valve, the fourth valve of the second six-way valve, the third valve, the fourth valve of the first six-way valve, and then enter the waste liquid bottle.

[0063] The first detection flow path refers to the clockwise detection flow path. The flow path direction switching is controlled by the second six-way valve (2). The second six-way valve (2) has an on-off mode. The on-off mode of the six-way valve (2) is switched periodically by the industrial computer setting step, so that the liquid in the flow path reciprocates multiple times through the detection cell to generate a series of signals.

[0064] Referring to Figure 5 If the detection flow path corresponding to the control instruction is the first bidirectional circulation fluorescence detection flow path, that is, the clockwise detection flow path, the first six-way valve (1) is connected with the mobile phase bottle (6). Under the action of the peristaltic pump (7), the liquid passes through the first valve (f2), the second valve (a2) of the second six-way valve (2), the first valve (f3), the fourth valve (e3) of the third six-way valve (3), the extension coil pipe (8), the third valve (b3), the second valve (a3) of the third six-way valve (3), d4-e4 of the sampling valve (4), the fluorescence detection cell (10), the first valve (c5), the fourth valve (d5) of the fourth six-way valve (5), the extension coil pipe (12), the third valve (a5), the second valve (b5) of the fourth six-way valve (5), the third valve (e2), the fourth valve (d2) of the second six-way valve (2), the third valve (c1), the fourth valve (d1) of the first six-way valve (1), and then enters the waste liquid bottle or the carrier liquid recovery system (13).

[0065] Optionally, the unidirectional / bidirectional circulation fluorescence detection device includes a plurality of six-way valves. The pipe connections of the plurality of six-way valves are controlled according to the control instruction, including:

[0066] If the detection flow path corresponding to the control instruction is the second bidirectional circulation fluorescence detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve, the second valve of the first six-way valve, the first valve, the third valve of the second six-way valve, the second valve, the third valve, the extension coil pipe, the fourth valve, the first valve of the fourth six-way valve, the fluorescence detection cell, the sampling valve, the second valve, the third valve, the extension coil pipe, the fourth valve, the first valve of the third six-way valve, the second valve, the fifth valve of the second six-way valve, and then enter the waste liquid bottle.

[0067] The second six-way valve (2) of the bidirectional circulation fluorescence detection flow path has an on-off mode, and after the second six-way valve (2) is switched from on to off mode, the unidirectional flow path six-way valve (2) is switched from f2-a2, e2-d2 to a2-b2, f2-e2, and the bidirectional circulation fluorescence detection flow path is switched from clockwise flow path to counterclockwise flow path.

[0068] Referring to Figure 6 If the control instruction corresponds to the bidirectional circulation fluorescence second detection flow path, that is, the counterclockwise direction detection flow path, the first six-way valve (1) is connected to the mobile phase bottle (6), under the power of the peristaltic pump (7), the mobile phase passes through the first valve (f2) and the third valve (e2) of the second six-way valve (2), the second valve (b5) and the third valve (a5) of the fourth six-way valve (5), the extension coil pipe (12), the fourth valve (d5) and the first valve (c5) of the fourth six-way valve (5), the fluorescence detection cell (10), e4-d4 of the sample valve (4), the second valve (a3) and the third valve (b3) of the third six-way valve (3), the extension coil pipe (8), the fourth valve (e3) and the first valve (f3) of the third six-way valve (3), the second valve (a2) and the fifth valve (b2) of the second six-way valve (2), and enters the waste liquid bottle or the carrier liquid recovery system (13).

[0069] The embodiment of the present application also provides a control system of the unidirectional / bidirectional circulation fluorescence detection device, which comprises:

[0070] The first module is used for acquiring a control instruction of a detection flow path.

[0071] The second module is used for controlling pipeline connection of a plurality of multi-way valves according to the control instruction, so as to obtain the detection flow path corresponding to the control instruction.

[0072] It can be seen that the contents in the above method embodiments are all applicable to the system embodiment, the system embodiment specifically realizes the same functions as the above method embodiments, and achieves the same beneficial effects as the above method embodiments.

[0073] The embodiment of the present application also provides a control device of the unidirectional / bidirectional circulation fluorescence detection device, which comprises:

[0074] At least one processor;

[0075] At least one memory is used for storing at least one program.

[0076] When the at least one program is executed by the at least one processor, the at least one processor realizes the control method steps of the unidirectional / bidirectional circulation fluorescence detection device described in the above method embodiments.

[0077] The memory, as a non-transitory computer readable storage medium, can be used to store non-transitory software programs and non-transitory computer executable programs. The memory can include a high-speed random access memory, and can also include a non-transitory memory, such as at least one magnetic disk storage device, a flash memory device, or other non-transitory solid-state memory device. In some embodiments, the memory can optionally include remote memory that is remotely located relative to the processor, and the remote memory can be connected to the processor through a network. Examples of the network include, but are not limited to, the Internet, an intranet, a local area network, a mobile communication network, and a combination thereof.

[0078] It can be seen that the contents in the method embodiments are applicable to the device embodiments, the device embodiments specifically implement the same functions as the method embodiments, and achieve the same beneficial effects as the method embodiments.

[0079] In addition, the embodiments of the present application further disclose a computer program product or a computer program, which is stored in a computer readable storage medium. The processor of the computer device can read the computer program from the computer readable storage medium, and the processor executes the computer program, so that the computer device executes the above-mentioned method.

[0080] The embodiments of the present application further provide a computer readable storage medium, which stores a program executable by a processor, and the program executable by the processor is used to implement the above-mentioned method when executed by the processor. Similarly, the contents in the method embodiments are applicable to the storage medium embodiments, the storage medium embodiments specifically implement the same functions as the method embodiments, and achieve the same beneficial effects as the method embodiments.

[0081] It is to be understood that all or some of the steps, systems, etc. in the methods disclosed above can be implemented in software, firmware, hardware, and any suitable combination thereof. Some or all of the physical components can be implemented as software executed by a processor, such as a central processing unit, a digital signal processor, or a microprocessor, as hardware, or as an integrated circuit, such as an application- specific integrated circuit. Such software can be distributed on computer readable media, which can comprise computer storage media (or non-transitory media) and communication media (or transitory media). As is well known to those of ordinary skill in the art, computer storage media includes volatile and non-volatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions, data structures, program modules or other data. Computer storage media includes, but is not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, digital versatile disks (DVD) or other optical disk storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can be accessed by a computer. Further, as is well known to those of ordinary skill in the art, communication media typically embodies computer readable instructions, data structures, program modules or other data in a modulated data signal such as a carrier wave or other transport mechanism and includes any information delivery media.

[0082] The embodiment of the present application provides a control system of a one-way / two-way circulating fluorescence detection device, which comprises an industrial control all-in-one machine and the one-way / two-way circulating fluorescence detection device.

[0083] The industrial control all-in-one machine is used for executing the control method.

[0084] Specifically, for the industrial control all-in-one machine, the terminal includes but is not limited to a desktop computer, a laptop computer, a smart processing device, etc. The industrial control all-in-one machine is also used for controlling the flow rate and steering of the peristaltic pump, the on-off of the electromagnetic valve, the communication control of the multi-channel injection pump, the light source on-off control, and the data transmission of the fiber-optic spectrometer, etc.

[0085] The embodiments of the present application are described below in combination with the drawings.

[0086] Case 1

[0087] (1) Online different injection stability test

[0088] When the instrument is stably running, in order to test its reproducibility, a lissamine rhodamine B solution sample (0.3 μg mL -1 ) is injected into the flowing carrier liquid, and then a fluorescence light path system is used for collection, and the parameter setting is as follows: LED 550 nm, the emission wave band of the spectrometer is 585 nm, and the integration time is 300 ms.

[0089] Fixed lissamine rhodamine B concentration is 0.3 μg mL -1 Under the condition, the peak intensity of 9 times of repeated injection under different flow rates was tested, refer to Figure 7 (A) in the figure, with the increase of flow rate, the peak intensity has no obvious change (the peak intensity is 7143.9 ± 418.7 a.u., RSD is 5.8%), which shows that the instrument has good stability.

[0090] (2) One-way circulation fluorescence detection stability test

[0091] When the instrument is stably running, in order to test the one-way circulation fluorescence detection stability, lissamine rhodamine B solution sample (0.3 μg mL -1 ) is injected into the flowing carrier liquid, and then the fluorescence light path system is used for collection, the parameter setting is: LED 550 nm, the emission band of the spectrometer is 585 nm, and the integration time is 300 ms. Through nine times of one-way circulation process under the same flow rate, the one-way circulation periodic damping curve is recorded, the peak height corresponding to each circulation period is calculated, each peak height is extracted, the RSD is calculated, and the stability of the instrument is tested.

[0092] From Figure 7 (B) in the figure, it can be seen that the diffusion speed of lissamine rhodamine B increases with the increase of flow rate, which is consistent with the theoretical result. From Figure 7 (C) in the figure, under the condition that the dye concentration is fixed, with the increase of circulation times, the circulation peak intensity of the sample under different flow rates at the same one-way circulation fluorescence detection moving distance is basically close, the flow rate has no obvious effect on the peak intensity, which shows that the stability of the instrument in the one-way circulation fluorescence detection process.

[0093] (3) Kinetic process calculation (simple diffusion controlled by concentration gradient conforms to first-order kinetic process) to calculate k

[0094] The dye diffusion is used to obtain the periodic damping oscillation curve as an important index of the stability of the one-way circulation fluorescence detection flow path, such as Figure 6 The ultrapure water is pumped into the one-way circulation pipe, after the ultrapure water fills the whole one-way pipe system, the valve 1 is switched to “1b, 1c”, forming a one-way circulation fluorescence detection closed system, at this time, the pure water solution repeatedly flows through the detection cell, and the detector reads the blank baseline. The injection valve 4 is switched to “injecting state”, the lissamine rhodamine B dye is introduced into the quantitative ring in the injection valve, after switching to “injecting state”, the spectrum collection program is started, the periodic signal of one-way circulation is recorded, and the peak height, half-peak width and time of each circulation period are extracted as important parameter indexes through data processing analysis. The time of one determination is about 10 minutes. Each flow rate (3.5 mL·min-1 , 4.64 mL·min -1 , 5.8 mL·min -1 , 6.96 mL·min -1 , 8.12 mL·min -1 ) was repeated 20 times, i.e. the pump rotation speed scale button was switched from 30 rpm to 80 rpm, and the conversion formula of flow rate and pump rotation speed was: Q = λ * n * d^2, n represented rotation speed, d represented the inner diameter of the hose (1.0 mm), and λ represented the flow rate coefficient 0.116.

[0095] a. Calculate the rate constant k of the dilution process. Considering that the carrier liquid is excessive relative to the dye, and that the process follows first-order kinetics:

[0096] v = k [dye] (1)

[0097] log(F t -F eq ) = log(F0-F eq ) - kt / 2.303 (2)

[0098] The concentration of lissamine rhodamine B was fixed at 0.01 mg·mL -1 Under the condition, by adjusting the recording of one-way circulation periodic damping curves at different flow rates, by extracting the peak value information of each periodic damping curve, the change rule of one-way circulation at each cycle time t and relative peak height (Ft-Feq) (a.u.) can be obtained. As shown in (D) and (E) in Figure 7 , log(F t -F eq ) has a clear linear relationship with cycle t, which conforms to the first-order kinetics equation. The absolute value of the slope k is the rate constant, and the rate constant gradually increases with the increase of the flow rate. When the rotation speed is 9.3 mL·min -1 , the rate constant k is 0.54 / min.

[0099] b. Lissamine rhodamine B diffusion coefficient test

[0100] D = (F 0 ) / (F p ) (3)

[0101] Wherein, F 0 is the initial fluorescence peak height of the non-diffusion sample in the detection cell, and F p is the peak height of each cycle.

[0102] The substance coefficient D defines the ratio of the dispersion before and after the dye. Since within a certain range, the concentration and fluorescence intensity have a clear linear relationship, i.e. using the equation D = (F 0 ) / (Fp The diffusion coefficient of lissamine rhodamine B was calculated, as shown in Table 1. Lr is the moving distance of the sample in the one-way circulation channel. The device was measured to have a path of about 40 cm per one-way cycle. Therefore, the diffusion coefficient of the material under different flow rates and different cycle numbers was calculated according to the peak intensity ratio of the initial non-diffusion concentration and each cycle. Under the same flow rate, the diffusion coefficient of lissamine rhodamine B increased with the increase of the cycle number. From (E) in Table 1, it can be seen that under the same cycle number, the diffusion coefficient decreases with the increase of the flow rate, which is consistent with the theoretical result. From (G) in Table 1, it can be seen that under the condition of constant dye concentration, the half-peak width ts of the cycle peak gradually increases with the increase of the cycle number, which indicates that with the increase of the diffusion cycle, the peak width gradually expands to both sides, resulting in the gradual increase of the half-peak width. Further, by setting different concentrations of dye molecules, it is found that the half-peak width has no obvious difference in the same cycle period, which is greatly related to the cycle number and the flow rate. Therefore, by adjusting different flow rates, the relationship between Lr and ts of the dye molecules was determined, and from (H) in Table 1, it can be seen that with the gradual increase of the cycle moving distance, the half-peak width also gradually increases, and under the condition of constant flow rate, the cycle moving distance Lr and the half-peak width ts have a clear linear relationship. With the decrease of the flow rate, the intercept of the equation increases, indicating that the lower the flow rate, the greater the diffusion width of each cycle. Figure 7 Figure 7 Figure 7

[0103] Table 1

[0104]

[0105] Case 2

[0106] This case provides a kinetic test in a two-way mode without diffusion mode, and the specific steps are as follows:

[0107] (1) Open the circulation channel system, fill the entire pipeline with electronic fluorinated liquid FC-3283 through the peristaltic pump, and when the liquid waste position is discharged, it can be judged that the pipeline is full of liquid. The pump speed of the peristaltic pump is set to different speeds.

[0108] (2) Turn on the LED light source, preheat for about 15 minutes, then turn on the fluorescence data acquisition operation system, and write the time control program of the electromagnetic valve;

[0109] (3) The analyte is lissamine rhodamine B, the concentration is 100 nmol·L -1 , and the sample amount is 20 μL. The sample is transferred to the quantitative ring through the injection valve and the sample needle.

[0110] ​​​(4) Start the spectrum collection program, open the electromagnetic control valve switching program, and switch the injection valve at the same time to transfer the sample into the circulating flow path system.

[0111] When the injected analyte and the carrier fluid are completely insoluble, the system presents a similar periodic rectangular pulse curve, as shown in Figure 8 As the pump speed gradually increases from 40 rpm to 90 rpm, the rectangular pulse width decreases, i.e., the time for the flow path to determine the lissamine rhodamine B per cycle decreases. The average rectangular pulse width at low speed (40 rpm) is 8 s, the average repetitive cycle is 40 s, and the average pulse amplitude is 4213 (a.u.). As the pump speed gradually increases to 90 rpm, the average matrix width gradually decreases to 3 s, the average repetitive cycle is 20 s, and the average pulse amplitude is 3762 (a.u.). Under the condition of 50 rpm, the RSD of the pulse width is 6.5%, the RSD of the average repetitive cycle is 2.4%, and the RSD of the average pulse amplitude is 2.1%. Whether from the stability of signal collection intensity or the stability of periodic change, good results have been achieved.

[0112] Case 3

[0113] This case provides a bidirectional mode sample injection flux test, and the specific steps are as follows:

[0114] (1) Open the circulating flow path system, fill the entire pipeline with pure electronic fluorinated liquid FC-3283 solution through the peristaltic pump, and when the liquid waste position is discharged, it can be judged that the pipeline is filled with liquid. The pump speed of the peristaltic pump is set to 30 rpm;

[0115] (2) Turn on the LED light source, preheat for about 15 min, and then turn on the fluorescence data collection operating system. Write a time control program for the electromagnetic valve.

[0116] (3) The analyte is lissamine rhodamine B with a concentration of 100 nmol·L -1 , and the sample injection amount is 20 μL. The sample is transferred to the quantitative ring through the injection valve and the sample injection needle.

[0117] (4) Start the spectrum collection program, and switch the injection valve at the same time to transfer the sample into the circulating flow path system. Sample injection every 10 s.

[0118] (5) After all the samples are injected and the signals are collected through the detection cell, manually open the electromagnetic control valve switching to detect the array signal collection unit after the flow path switching. Refer to Figure 9, the RSD of the fluorescence intensity signal collected at 585 nm emission wavelength after 15 cycles of single detection is 3.3%, which has good stability. The maximum sample throughput of the system is 20, which is adapted by the programmed control of the electromagnetic valve and peristaltic pump. It is not difficult to find that the maximum test throughput of 10 samples can be maintained under the condition of 30 rpm, and the RSDs are 3.3% and 4.4%, respectively. The time interval of two sample injections in the forward direction of the reciprocating cycle is about 12 s.

[0119] Case 4

[0120] This case provides a cyclic dye test and condition optimization in a bidirectional cycle mode, and the specific steps are as follows:

[0121] (1) Open the circulation flow path system, fill the entire pipeline with pure water solution by peristaltic pump, and discharge the liquid waste position to determine that the pipeline is full of liquid. The pump speed of the peristaltic pump is set to 50 rpm.

[0122] (2) Turn on the LED light source, preheat for about 15 min, then turn on the fluorescence data acquisition operating system, and write the time control program of the electromagnetic valve;

[0123] (3) The analyte is lysamine rhodamine B with a concentration of 100 nmol·L -1 and a sample size of 20 μL; the sample is transferred to the quantitative ring by the injection valve and the sample needle;

[0124] (4) Start the spectrum acquisition program, and at the same time, open the switching program of the electromagnetic control valve and switch the injection valve to transfer the sample to the circulation flow path system.

[0125] (5) Under the condition of peristaltic pump speed of 50 rpm, the time control program of electromagnetic valve switching setting is optimized to ensure that the peak information is complete in each reciprocating cycle. See Figure 10, I-VI represent different electromagnetic valve time control programs, T1 is the time of sample passing through the injection valve and completely flowing through the detection cell, T1 is in the range of 8-10s, which can ensure that the first peak is complete, T2-T7 in I-IV is set to equal time interval size (10s, 12s and 15s), at this time, the incomplete peak information under the cycle period can be obviously observed, which indicates that the sample has not completely flowed out of the detection cell, and the sample is repeatedly introduced into the detection cell due to the switching of the electromagnetic valve, and the single sample introduction information cannot be completely collected. V-VI sets a time gradient (T1-T7 is raised at equal gradient, respectively 0s-14s and 0s-18s) in the time sequence, and the peak information under each cycle period is complete. The setting of this gradient time sequence is suitable for the diffusion conditions between the carrier liquid and the substance in the reciprocating cycle system, which is caused by the gradually increasing half-peak width of the sample under different cycle periods and the liquid pulse under the driving of the peristaltic pump.

[0126] It can be seen that the contents in the method embodiments are applicable to the system embodiments, the system embodiments specifically realize the same functions as the method embodiments, and achieve the same beneficial effects as the method embodiments.

[0127] The above is a specific description of the preferred implementation of the present application, but the present application is not limited to the above embodiments, and those skilled in the art can make various equivalent modifications or replacements without departing from the spirit of the present application, and these equivalent modifications or replacements are all included in the scope defined by the claims of the present application.

Claims

1. A control method of a unidirectional / bidirectional circulation fluorescence detection device, characterized by, The detection device comprises a mobile phase bottle, a plurality of multi-way valves, a carrier liquid unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit. Different pipes of the plurality of multi-way valves are connected to form different detection flow paths between the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle. The detection flow paths comprise a one-way fluorescence detection flow path, a one-way circulation fluorescence detection flow path, a bidirectional circulation fluorescence first detection flow path and a bidirectional circulation fluorescence second detection flow path. The carrier liquid unit is used to control the liquid flow rate of the detection flow path. The fluorescence detection unit is used to detect the liquid spectrum in the fluorescence detection cell. The control method comprises: obtaining a control instruction of a detection flow path; controlling the pipe connection of the plurality of multi-way valves according to the control instruction to obtain a detection flow path corresponding to the control instruction; the one-way / bidirectional circulation fluorescence detection device comprises a plurality of six-way valves, and the control of the pipe connection of the plurality of multi-way valves according to the control instruction comprises: if the detection flow path corresponding to the control instruction is a one-way fluorescence detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the second valve of the third six-way valve, the sample injection valve, the fluorescence detection cell, the first valve and the second valve of the fourth six-way valve, the third valve and the fourth valve of the second six-way valve, the third valve and the fourth valve of the first six-way valve, and enter the waste liquid bottle.

2. The control method according to claim 1, characterized by, the one-way / bidirectional circulation fluorescence detection device comprises a plurality of six-way valves, and the control of the pipe connection of the plurality of multi-way valves according to the control instruction comprises: if the detection flow path corresponding to the control instruction is a one-way circulation fluorescence detection flow path, the liquid of the flow path is controlled to flow between the third valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the second valve of the third six-way valve, the sample injection valve, the fluorescence detection cell, the first valve and the second valve of the fourth six-way valve, and the third valve and the fourth valve of the second six-way valve.

3. The control method according to claim 1, characterized by, the one-way / bidirectional circulation fluorescence detection device comprises a plurality of six-way valves, and the control of the pipe connection of the plurality of multi-way valves according to the control instruction comprises: if the detection flow path corresponding to the control instruction is a bidirectional circulation fluorescence first detection flow path, the liquid of the mobile phase bottle is controlled to pass through the first valve and the second valve of the first six-way valve, the first valve and the second valve of the second six-way valve, the first valve and the fourth valve of the third six-way valve, the extension coil pipe, the third valve and the second valve, the sample injection valve, the fluorescence detection cell, the first valve and the fourth valve of the fourth six-way valve, the extension coil pipe, the third valve and the second valve, the third valve and the fourth valve of the second six-way valve, the third valve and the fourth valve of the first six-way valve, and enter the waste liquid bottle.

4. The control method according to claim 1, characterized by, the one-way / bidirectional circulation fluorescence detection device comprises a plurality of six-way valves, and the control of the pipe connection of the plurality of multi-way valves according to the control instruction comprises: If the control instruction corresponds to a two-way circulating fluorescence second detection flow path, the liquid of the mobile phase bottle is controlled to pass through a first valve, a second valve of a first six-way valve, a first valve, a third valve of a second six-way valve, a second valve, a third valve, an extension coil pipe line, a fourth valve, a first valve of a fourth six-way valve, a fluorescence detection cell, a sample injection valve, a second valve, a third valve, an extension coil pipe line, a fourth valve, a first valve of a third six-way valve, a second valve, a fifth valve of the second six-way valve, and enters the waste liquid bottle.

5. A control system for a unidirectional / bidirectional circulation fluorescence detection apparatus, characterized by, The application relates to a control method of a single-way / two-way circulating fluorescence detection device, and a single-way / two-way circulating fluorescence detection device. The single-way / two-way circulating fluorescence detection device comprises a mobile phase bottle, a plurality of multi-way valves, a liquid carrying unit, a sample injection unit, a fluorescence detection cell, a waste liquid bottle and a fluorescence detection unit. Different pipelines of the plurality of multi-way valves are connected to form different detection flow paths among the mobile phase bottle, the plurality of multi-way valves, the sample injection unit, the fluorescence detection cell and the waste liquid bottle. The detection flow paths comprise a single-way fluorescence detection flow path, a single-way circulating fluorescence detection flow path, a two-way circulating fluorescence first detection flow path and a two-way circulating fluorescence second detection flow path. The liquid flow rate of the detection flow paths is controlled by the liquid carrying unit. The fluorescence detection cell is detected by the fluorescence detection unit. The single-way / two-way circulating fluorescence detection device comprises a plurality of six-way valves, wherein, The industrial control computer is used for executing the control method in any one of claims 1-4.

6. The control system of claim 5, wherein, The multi-way valve comprises an extension coil pipe line, the extension coil pipe line is arranged between two valves, and the length of the extension coil pipe line is 50cm-500cm.

7. The control system of claim 5, wherein, The liquid carrying unit comprises any one or more of a peristaltic pump, a plunger pump or a syringe pump.

8. The control system of claim 5, wherein, The fluorescence detection unit comprises a light source and a fiber spectrometer. The light emitted by the light source reaches the fiber spectrometer through the fluorescence detection cell. The wavelength range of the light source comprises 300nm-600nm. The liquid carrying unit comprises any one or more of a peristaltic pump, a plunger pump or a syringe pump. The fluorescence detection unit comprises a light source and a fiber spectrometer. The light emitted by the light source reaches the fiber spectrometer through the fluorescence detection cell. The wavelength range of the light source comprises 300nm-600nm.

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