A dual robotic arm automated solid phase extraction system and methods of use thereof

Abstract

The application discloses a double-robot-arm type automatic solid-phase extraction system and a use method thereof, and comprises two groups of injection pump assemblies, two groups of solution buffer tube assemblies, two groups of ten-way valve assemblies, two groups of extraction column assemblies, two groups of mechanical arms, a transmission belt, two groups of sample feeding mechanical arm assemblies, two groups of sample feeding needles, two groups of solution collecting mechanical arms, two groups of solution collecting needles, two groups of elution reagent groups, two groups of waste liquid collecting bottles, two groups of sample tube racks, a solution collecting tube rack, two groups of waste liquid tanks and a control system. The application can realize the application of chemical element separation and enrichment under multiple scenes, replace manual liquid adding operation, realize adjustable extraction flow rate through the cooperation of a closed extraction column and an injection pump, and improves experimental efficiency. The control system independently controls each component, and can simultaneously complete the operation of two different sample pretreatment processes. Through the control of one group of sample feeding mechanical arms on the sampling of the collected solution in the solution collecting tube group rack, the use of a string column can be completed.

Description

Technical Field

[0001] This invention relates to the field of solid phase extraction experimental apparatus, and in particular to a dual-robotic arm automated solid phase extraction system and its usage method. Background Technology

[0002] Multi-receiver inductively coupled plasma mass spectrometry (MC-ICP-MS) offers advantages such as high analytical precision, small sample volume, and fast testing speed in the analysis of radiogenic isotopes and stable metal isotopes. However, samples from environmental, geological, and biological fields often have complex matrices. When isotopes are directly analyzed using MC-ICP-MS on digested solutions of various samples, interference from matrix elements can affect the accurate determination of isotopic composition. Therefore, obtaining pure analyte components through chemical pretreatment before sample analysis is crucial. Currently, solid-phase extraction (SPE) is commonly used to separate and purify analyte elements from interfering elements in samples, reducing interference during MC-ICP-MS analysis and obtaining high-precision isotopic data.

[0003] Traditional manual solid-phase extraction (SPE) methods require manual addition of sample solution and eluent to each SPE column, a cumbersome and time-consuming process with uncontrollable extraction time. Automated SPE technology primarily utilizes mechanical devices and pumps to replace manual operation, automating liquid collection and addition during the extraction process. However, existing automated SPE devices typically only allow one sample pretreatment method per extraction cycle, and each extraction path is equipped with only one extraction column. This can lead to situations where a single SPE column or a single extraction cycle cannot achieve the chemical separation and enrichment of the target element. Furthermore, the number of solution collection tubes generally corresponds to the number of sample tubes, making it impossible to collect fractions from a single sample multiple times to monitor changes in elemental composition.

[0004] Therefore, to solve the above problems, this invention provides a dual-robotic-arm automated solid-phase extraction system and its usage method. It features a 3×16-digit solution collection rack, capable of collecting the extract fraction of a single sample in 16 segments, monitoring changes in elemental composition within the fraction, and applying this system to optimize isotope sample pretreatment processes. The control system independently controls each component, simultaneously enabling the operation of two different sample pretreatment processes. Furthermore, it can control one set of sample injection robotic arms to sample the already collected solution from the solution collection rack for further solid-phase extraction, replacing the traditional column extraction mode. This solves the problem that a single solid-phase extraction column or a single solid-phase extraction cannot achieve the chemical separation and enrichment of the target element. Summary of the Invention

[0005] This invention provides a dual-robotic-arm automated solid-phase extraction system and its usage method, enabling a single extraction system to simultaneously perform different chemical pretreatment processes, thereby improving experimental efficiency.

[0006] To achieve the above objectives, the present invention provides the following solution:

[0007] A dual-robotic-arm automated solid-phase extraction system includes two sets of injection pump assemblies (1, 16), two sets of solution buffer tubes (2, 17), two sets of ten-way valve assemblies (3, 18), two sets of extraction columns (4, 19), two sets of robotic arms (5, 20), a drive belt (6), two sets of sample injection robotic arm assemblies (7, 21), two sets of injection needles (8, 22), two sets of solution collection robotic arms (9, 23), two sets of solution collection needles (10, 24), two sets of elution reagent sets (11, 25), two sets of waste liquid collection bottles (12, 26), two sets of sample tube racks (13, 27), a solution collection tube rack (14), two sets of waste liquid tanks (15, 28), and a control system (29). The system connects the two sets of injection needles (8, 22) and solution collection needles (10, 24) to the system. The system is combined with robotic arms (5, 20), injection robotic arms (7, 21), and solution collection robotic arms (9, 23) to form a dual-robotic-arm automatic injection and solution collection module. Each side of the dual robotic arms is equipped with an independent solid-phase extraction component, which is connected to the injection pump assembly (1, 16), injection needle (8, 22), solution collection needle (10, 24), elution reagent group (11, 25), and waste liquid collection bottle (12, 26) by a ten-way valve assembly (3, 18). The ten-way valve assembly (3, 18) includes a ten-way valve. A solution buffer tube assembly (2, 17) is provided between the J port of the ten-way valve and the injection pump (1, 16). An extraction column assembly is provided between the ten-way valve assembly (3, 18) and the solution collection needle (10, 24).

[0008] Preferably, the injection pump assembly includes at least three injection pumps connected to one end of the solution buffer tube assembly, and the other end of the solution buffer tube assembly is connected to the ten-way valve.

[0009] Preferably, the rinsing reagent group includes six rinsing reagent tubes, which are respectively connected to ports D to I on the ten-way valve assembly.

[0010] Preferably, the B port of the ten-way valve is connected to the 3×16-digit solution collection tube.

[0011] Preferably, the C port of the ten-way valve is connected to the waste liquid collection bottle.

[0012] Preferably, the A port of the ten-way valve is connected to the sample tube.

[0013] Preferably, the ten-way valve assembly includes at least three ten-way valves.

[0014] A method of using a dual-robotic-arm automated solid-phase extraction device includes the following steps:

[0015] Under the command of the control system, the robotic arm (5, 20) and its components on the left and right sides (component ①, component ②) can independently complete the following steps asynchronously:

[0016] Sample loading: The digested sample solution is transferred to a centrifuge tube and placed on the sample tube rack (13, 27). The injection robotic arm (7, 21) drives the injection needle (8, 22) to the designated sample tube rack (13, 27). The solution is quantitatively drawn up through the injection pump assembly (1, 16) and the flow rate of the solution in the pipeline is controlled. The solution enters the solution buffer tube assembly (2, 17) through the A and J ports of the ten-way valve assembly (3, 18). The ten-way valve assembly is switched to port B. The injection pump assembly pumps the solution out of the buffer tube assembly and through the J and B ports of the ten-way valve assembly into the extraction column (4, 19).

[0017] Eluting and Sample Collection: The ten-way valve (3, 18) is switched to any of the ports from D to I. Under the action of the syringe pump (1, 16), different elution reagents (11, 25) are quantitatively extracted and sequentially passed through the extraction column (4, 19). The extracted solution is then piped to the solution collection injection needle (10, 24). The robotic arm (5, 20) controls the solution injection needle to collect the solution at a designated position on the 3*16-position solution collection rack (14). During the extraction of a single sample, 16 sets of solution fractions can be collected. Solutions that do not need to be collected are moved by the solution collection needle (10, 24) to the waste liquid tank (15, 28) for discharge.

[0018] Extraction column and tubing cleaning: After the rinsing process is completed, under the action of the syringe pump (1, 16) and the ten-way valve (3, 18), different rinsing reagents (11, 25) are quantitatively extracted and passed through the extraction column (4, 19) in sequence to clean and balance the extraction column. Then, the ten-way valve (3, 18) is switched to interface A, and the injection needle (8, 22) is moved to a specific position on the sample tube rack (13, 27) to obtain the cleaning solution. The syringe pump (1, 16) is started to draw up the cleaning solution. Then, the ten-way valve (3, 18) is switched to interface C, and the syringe pump (1, 16) injects the cleaning waste liquid into the waste liquid collection bottle (12, 26). After completion, the ten-way valve (3, 18) is switched again. Under the instruction of the control system (29), the robotic arm (5, 20) moves the injection needle (8, 22) to the designated position to start the next sample loading.

[0019] The present invention achieves the following technical effects compared to the prior art:

[0020] 1. This invention replaces manual liquid addition, sets up multiple extraction pathways, effectively reduces the risk of cross-contamination between samples, reduces pipeline memory effect, and achieves adjustable extraction flow rate through the combination of closed solid phase extraction column and plunger pump.

[0021] 2. This invention features a 3×16-digit solution collection rack, which can collect the extract fraction of a single sample in 16 segments, monitor the changes in elemental composition in the fraction, and be applied to the optimization of isotope sample pretreatment processes.

[0022] 3. This invention employs a dual-robotic arm automated sample introduction and solution collection operation, which can simultaneously complete two different sample pretreatment processes; it can also control one set of sample introduction robotic arms to sample the solution already collected in the solution collection tube rack and perform solid-phase extraction again, replacing the serial column extraction mode, thus solving the dilemma that a single solid-phase extraction column or a single solid-phase extraction cannot complete the chemical separation and enrichment of the target element. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Appendix Figure 1 This is a schematic diagram of the structure of the present invention;

[0025] 1. Injection pump assembly ①; 2. Solution buffer tube ①; 3. 10-way valve assembly ①; 4. Extraction column ①; 5. Robotic arm ①; 6. Drive belt; 7. Robotic arm assembly ①; 8. Injection needle ①; 9. Solution collection robotic arm ①; 10. Solution collection needle ①; 11. Eluent ①; 12. Waste collection bottle ①; 13. Sample tube rack ①; 14. 3×16-digit solution collection tube rack; 15. Waste ① Liquid tank; 16. Injection pump assembly ②; 17. Solution buffer tube ②; 18. Ten-way valve assembly ②; 19. Extraction column ②; 20. Robotic arm ②; 21. Injection robotic arm assembly ②; 22. Injection needle ②; 23. Solution collection robotic arm ②; 24. Solution collection needle ②; 25. Eluent assembly ②; 26. Waste collection bottle ②; 27. Sample tube rack ②; 28. Waste tank ②; 29. ​​Control system. Detailed Implementation

[0026] The purpose of this invention is to provide a dual-robotic-arm automated solid-phase extraction system and its usage method, so as to achieve the simultaneous operation of two different sample pretreatment processes.

[0027] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0028] refer to Figure 1 A dual-robotic-arm automated solid-phase extraction system includes two sets of injection pump assemblies, two sets of solution buffer tube assemblies, two sets of ten-way valve assemblies, two sets of extraction column assemblies, two sets of robotic arms, a drive belt, two sets of sample injection robotic arm assemblies, two sets of sample injection needles, two sets of solution collection robotic arms, two sets of solution collection needles, two sets of elution reagent sets, two sets of waste liquid collection bottles, two sets of sample tube racks, solution collection tube racks, two sets of waste liquid tanks, and a control system. Components 1-15 constitute one extraction system, and components 16-28 constitute another extraction system. The two systems are independently controlled by the control system 29. The injection needles 7 and 21 can not only draw sample solutions from sample tube racks 13 and 27 respectively for extraction, but also simultaneously run two different sample pretreatment processes. The solution collection tube rack 14 is located between the robotic arm 5 and the robotic arm 20. It can also be moved to a designated position on the solution collection tube rack 14 by the robotic arm 5 and the robotic arm 20 respectively to aspirate the solution collected after extraction and inject it again, thus completing two consecutive solid phase extractions of a single sample. This replaces the column extraction mode and solves the dilemma that a single solid phase extraction column or a single solid phase extraction cannot complete the chemical separation and enrichment of the target element.

[0029] refer to Figure 1 The injection pump assembly includes at least three injection pumps connected to one end of the solution buffer tube assembly, and the other end of the solution buffer tube assembly is connected to the ten-way valve.

[0030] refer to Figure 1 The rinsing reagent assembly includes six rinsing reagent tubes, which are respectively connected to ports D to I on the ten-way valve assembly.

[0031] refer to Figure 1 The B port of the ten-way valve is connected to the extraction column assembly.

[0032] refer to Figure 1 The C port of the ten-way valve is connected to the waste liquid collection bottle.

[0033] refer to Figure 1 The A port of the ten-way valve is connected to the solution collection pipe.

[0034] refer to Figure 1 The ten-way valve assembly includes at least three of the ten-way valves.

[0035] Example 1:

[0036] Step 1, activate the extraction column: switch the 10-way valve assembly 3 and 18 to any of the ports from D to I. Under the action of the injection pump assembly 1 and 16, extract different elution reagents 11 and 25 quantitatively through the extraction column 4 and 19 to complete the activation.

[0037] The second step is sample loading: The digested sample solution is transferred to centrifuge tubes and placed on sample tube racks 13 and 27 respectively. The robotic arms 5 and 20 drive the injection needles 7 and 21 to the designated positions on the sample tube racks 13 and 27 respectively. The solution is quantitatively drawn up by the syringe pump assembly 1 and 16 and the flow rate of the solution in the pipeline is controlled. The solution enters the solution buffer tube assembly 2 and 17 through the A and J ports of the ten-way valve assembly. The ten-way valve assembly is switched to port B. The syringe pump assembly pumps the solution out of the solution buffer tube assembly and through the J and B ports of the ten-way valve assembly into the extraction column 4 and 19.

[0038] The third step, rinsing and sample collection: the ten-way valves 3 and 18 are switched to any of the ports from D to I. Under the action of the syringe pumps 1 and 16, different rinsing reagents 11 and 25 are quantitatively extracted and passed sequentially through the extraction columns 4 and 19. The extracted solution reaches the solution collection injection needles 10 and 24 through the pipeline. The robotic arms 5 and 20 control the solution injection needles to collect the solution at the designated position on the solution collection tube rack 14. The solution that does not need to be collected is moved by the solution collection needles 10 and 24 to the waste liquid tanks 15 and 28 for discharge.

[0039] Step 4, Cleaning of Extraction Column and Tubing: After the rinsing process is completed, under the action of syringe pumps 1 and 16 and ten-way valves 3 and 18, different rinsing reagents 11 and 25 are quantitatively extracted and passed sequentially through extraction columns 4 and 19 to clean and equilibrate the extraction columns. Then, ten-way valves 3 and 18 are switched to interface A, and injection needles 8 and 22 are moved to a specific position on the sample tube rack 13 and 27 to collect the cleaning solution. Syringe pumps 1 and 16 are started to draw up the cleaning solution. Subsequently, ten-way valves 3 and 18 are switched to interface C, and syringe pumps 1 and 16 inject the cleaning waste liquid into waste liquid collection bottles 12 and 26. After completion, the direction of ten-way valves 3 and 18 is switched again. Under the instruction of control system 29, robotic arms 5 and 20 move injection needles 8 and 22 to the designated position to start the next sample loading.

[0040] Example 2:

[0041] Step 1, activate the extraction column: the process is the same as in Example 1.

[0042] Step 2, Sample loading of extraction column assembly 4: The digested sample solution is transferred to centrifuge tubes and placed on sample tube rack 13. Robotic arm 5 drives injection needle 7 to the designated position on sample tube rack 13. Solution is quantitatively aspirated by injection pump assembly 1. The solution enters solution buffer tube assembly 2 through ports A and J of ten-way valve assembly 3. Ten-way valve assembly 3 is switched to port B. Injection pump assembly 1 pumps the solution out of solution buffer tube assembly 2 and into extraction column 4 through ports J and B of ten-way valve assembly 3.

[0043] Step 3, rinsing and sample collection of extraction column assembly 4: the 10-way valve assembly 3 is switched to any of the ports from D to I. Under the action of injection pump assembly 1, different rinsing reagent groups 11 are quantitatively extracted and passed through extraction column assembly 4. The extracted solution reaches solution collection needle 10 through the pipeline. The robotic arm 5 controls the solution collection needle to collect the solution at a designated position on solution collection rack 14. The solution that does not need to be collected is moved from solution collection needle 10 to waste tank 15 and discharged.

[0044] Step 4, Sample loading of extraction column assembly 19: Robotic arm 20 drives injection needle 21 to the designated position of solution collection tube rack 14, quantitatively aspirates solution through injection pump assembly 16, and enters solution buffer tube assembly 17 through ports A and J of ten-way valve assembly 18. Ten-way valve assembly 18 is then switched to port B, and injection pump assembly 16 pumps the solution out of solution buffer tube assembly 17 through ports J and B of ten-way valve assembly 18, and into extraction column 19.

[0045] Step 5, rinsing and sample collection of extraction column assembly 19 (No. 2): The 10-way valve assembly 18 (No. 2) is switched to any of the ports from D to I. Under the action of the injection pump assembly 16 (No. 2), different rinsing reagent groups 25 (No. 2) are quantitatively extracted and sequentially passed through the extraction column assembly 19 (No. 2). The extracted solution reaches the solution collection injection needle 24 (No. 2) through the pipeline. The robotic arm 20 (No. 2) controls the solution injection needle to collect the solution at a designated position on the solution collection tube rack 14. The solution that does not need to be collected is moved by the solution collection needle 24 (No. 2) to the waste liquid tank 28 (No. 2) for discharge.

[0046] Step 6, Cleaning of extraction columns 4 and 19 and pipelines: The process is the same as step 4 in Example 1.

[0047] Adaptive changes made according to actual needs, including but not limited to changes in system materials and changes in the number of extraction modules, are all within the scope of protection of this invention.

[0048] It should be noted that, for those skilled in the art, it is obvious that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

Claims

1. A dual-robotic-arm automated solid-phase extraction system, characterized in that, Includes two sets of injection pump assemblies (1, 16), two sets of solution buffer tube assemblies (2, 17), two sets of ten-way valve assemblies (3, 18), two sets of extraction columns (4, 19), two sets of robotic arms (5, 20), a drive belt (6), two sets of injection robotic arm assemblies (7, 21), two sets of injection needles (8, 22), two sets of solution collection robotic arms (9, 23), two sets of solution collection needles (10, 24), two sets of elution reagent sets (11, 25), two sets of waste liquid collection bottles (12, 26), two sets of sample tube racks (13, 27), a 3×16-digit solution collection tube rack (14), two sets of waste liquid tanks (15, 28), and a control system (29). The two sets of injection needles (8, 22) and solution collection needles (10, 24) are connected to the robotic arms. The robotic arms (5, 20), the injection robotic arm (7, 21), and the solution collection robotic arm (9, 23) are combined to form a dual-robotic arm type automatic injection and solution collection module. On each side of the dual robotic arms, an independent solid-phase extraction component is set up. The ten-way valve assembly (3, 18) is connected to the injection pump assembly (1, 16), the injection needle (8, 22), the solution collection needle (10, 24), the elution reagent group (11, 25), and the waste liquid collection bottle (12, 26), respectively. The ten-way valve assembly (3, 18) includes a ten-way valve. A solution buffer tube assembly (2, 17) is provided between the J port of the ten-way valve and the injection pump (1, 16). An extraction column assembly is provided between the ten-way valve assembly (3, 18) and the solution collection needle (10, 24). The injection pump assembly includes at least three injection pumps connected to one end of the solution buffer tube assembly, and the other end of the solution buffer tube assembly is connected to the ten-way valve. The rinsing reagent group includes six rinsing reagent tubes, which are respectively connected to ports D to I on the ten-way valve assembly; The B port of the ten-way valve is connected to the 3×16-digit solution collection tube; The syringe pump, solution buffer tube assembly, extraction column, solution tubing, injection needle, solution collection needle, and ten-way valve assembly are all made of corrosion-resistant materials.

2. The dual-robotic-arm automated solid-phase extraction system according to claim 1, characterized in that, The C port of the ten-way valve is connected to the waste liquid collection bottle.

3. The dual-robotic-arm automated solid-phase extraction system according to claim 1, characterized in that, The A port of the ten-way valve is connected to the sample tube.

4. The dual-robotic-arm automated solid-phase extraction system according to claim 1, characterized in that, The ten-way valve assembly includes at least three of the ten-way valves.

5. A method of using a dual-robotic-arm automated solid-phase extraction device, characterized in that, Includes the following steps: Under the command of the control system, the robotic arms (5, 20) and their side components constitute two sets of single-arm automated solid-phase extraction systems, which can complete the following steps in a synchronous or asynchronous manner: Sample loading: The digested sample solution is transferred to a centrifuge tube and placed on the sample tube rack (13, 27). The injection robotic arm (7, 21) drives the injection needle (8, 22) to the designated position on the sample tube rack (13, 27). The solution is quantitatively drawn up through the syringe pump assembly (1, 16) and the flow rate of the solution in the pipeline is controlled. The solution enters the solution buffer tube assembly (2, 17) through the A and J ports of the ten-way valve assembly (3, 18). The ten-way valve assembly is switched to port B. The syringe pump assembly pumps the solution out of the buffer tube assembly and through the J and B ports of the ten-way valve assembly into the extraction column (4, 19). Eluting and Sample Collection: The ten-way valve (3, 18) is switched to any of the ports from D to I. Under the action of the syringe pump (1, 16), different elution reagents (11, 25) are quantitatively extracted and sequentially passed through the extraction column (4, 19). The extracted solution reaches the solution collection injection needle (10, 24) through the pipeline. The robotic arm (5, 20) controls the solution injection needle to collect the solution at the designated position on the 3×16-digit solution collection tube rack (14). During the extraction of a single sample, 16 groups of solution fractions can be collected to monitor the changes in elemental composition in the fractions. This can be applied to the optimization of the isotope sample pretreatment process. Solutions that do not need to be collected are moved by the solution collection needle (10, 24) to the waste liquid tank (15, 28) and discharged. Extraction column and tubing cleaning: After the rinsing process is completed, under the action of the syringe pump (1, 16) and the ten-way valve (3, 18), different rinsing reagents (11, 25) are extracted quantitatively and passed through the extraction column (4, 19) in sequence to clean and balance the extraction column. Then, the ten-way valve (3, 18) is switched to interface A, and the injection needle (8, 22) is moved to a specific position on the sample tube rack (13, 27) to obtain the cleaning solution. The syringe pump (1, 16) is started to draw up the cleaning solution. Then, the ten-way valve (3, 18) is switched to interface C, and the syringe pump (1, 16) injects the cleaning waste liquid into the waste liquid collection bottle (12, 26). After completion, the direction of the ten-way valve (3, 18) is switched again. Under the instruction of the control system (29), the robotic arm (5, 20) moves the injection needle (8, 22) to the designated position to start the next sample loading.

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