Automatic sample injection-fraction collection-automatic sample application integrated system

Abstract

The utility model provides an automatic sample injection-fraction collection-automatic sample application integrated system, and belongs to the technical field of liquid chromatography. According to the utility model, the sample injection function of the automatic sample injector, the fraction collection function of the fraction collector and the automatic sample application function of the automatic sample application instrument are integrated, sample injection, collection and sample application parameters are set through the control system, the moving mechanism is controlled to drive the sample injection needle to move to required positions according to different stages, and the sample injection function of the sample injector is realized by arranging the two-position three-way valve and the two-position six-way valve. And the complete process of sample introduction, fraction collection and sample application is completed in sequence by switching pipelines of the control system. According to the utility model, automatic sample injection can be realized, after liquid chromatography separation and detection, effluent is collected to a specified collection bottle as required, and after collection, automatic sample application of each fraction on the thin-layer plate is realized.

Description

Technical Field

[0001] The utility model relates to the technical field of liquid chromatography, in particular to an automatic sampling-fraction collection-automatic spotting integrated system. Background Art

[0002] The main function of commercially available analytical liquid chromatographs is to separate and detect samples, and the effluent after detection is directly discharged to waste without being recycled. However, for some important samples, the effluent after analysis needs to be recycled, and in this case, a fraction collection system is generally required, and two sets of instruments may need to be controlled by two sets of software, which will reduce the convenience of operation for staff and increase the possibility of misoperation, which will greatly affect work efficiency and even lead to the loss of important samples.

[0003] For samples with relatively complex components, users sometimes need to perform thin layer chromatography analysis on the collected fractions to quickly understand the chromatographic behavior of the corresponding fractions on the specified stationary phase. At this time, different fractions need to be spotted manually or using an automatic spotter. The spotting process is time-consuming and labor-intensive, and due to the large number of fractions to be spotted, manual spotting or spotting with an automatic spotter is prone to misoperation, such as incorrect spotting positions, repeated spotting of the same fraction, overlapping spotting of different fractions, etc. In addition, the stationary phase coated on the thin layer plate may fall off due to improper use of capillaries by operators during the spotting process, resulting in the scrapping of the thin layer plate, which ultimately affects the experimental results and work efficiency.

[0004] Therefore, there is a need for an automatic sampling-fraction collection-automatic spotting integrated system for liquid chromatography. Utility Model Content

[0005] In order to solve the technical problems existing in the prior art, the utility model provides an automatic injection-fraction collection-automatic spotting integrated system, which integrates the injection function of the automatic sampler, the fraction collection function of the fraction collector, and the automatic spotting function of the automatic spotter. The utility model can realize automatic sample injection, and after liquid chromatography separation and detection, the effluent is collected into a designated collection bottle as needed, and after collection, each fraction is automatically spotted on a thin layer plate.

[0006] The utility model provides an automatic sampling-fraction collection-automatic sampling integrated system, comprising: an automatic sampling-fraction collection-automatic sampling integrated device and a control system;

[0007] The automatic sampling-fraction collection-automatic spotting integrated device is connected to the control system, and the control system sets the sampling parameters, collection parameters and spotting parameters, and controls the automatic sampling-fraction collection-automatic spotting integrated device to complete automatic sampling, fraction collection and automatic spotting according to the set sampling parameters, collection parameters and spotting parameters;

[0008] The automatic sampling-fraction collection-automatic spotting integrated device comprises a moving mechanism, a pipeline device, a thin layer plate placement area, and a sample bottle and collection bottle placement area, and the moving mechanism and the pipeline device are both connected to the control system;

[0009] The thin layer plate placement area is provided with scales in the X direction and the Y direction respectively;

[0010] The moving mechanism is controlled by the control system to drive the injection needle to move in horizontal and vertical directions;

[0011] The pipeline device is controlled by the control system to switch the pipeline connection state, so as to complete the injection, fraction collection and spotting respectively; the pipeline device includes a quantitative loop and a pipeline, and the pipeline device is connected with a syringe, a sampling needle, an infusion pump and a chromatographic column; one end of the chromatographic column is also connected with a detector; the quantitative loop is connected with the syringe and the sampling needle, or the quantitative loop is connected with the infusion pump and the chromatographic column;

[0012] The control system controls the pushing and drawing actions of the syringe according to the set injection parameters, collection parameters and spotting parameters.

[0013] Preferably, the pipeline device also includes a two-position six-way valve, a first two-position three-way valve and a second two-position three-way valve, the two-position six-way valve can be connected to the first two-position three-way valve, the two-position six-way valve is connected to the quantitative ring and the syringe, the first two-position three-way valve is connected to the second two-position three-way valve, and the control system controls the communication position of the two-position six-way valve, the first two-position three-way valve and the second two-position three-way valve according to the set injection parameters, collection parameters and spotting parameters.

[0014] Preferably, when injecting and not collecting fractions, the first two-position three-way valve is connected to the two-position six-way valve, and the second two-position three-way valve is connected to the waste liquid collection bucket, and when collecting fractions, the second two-position three-way valve is connected to the collection bottle; when injecting, the syringe is connected to the quantitative loop through the two-position six-way valve, the quantitative loop is connected to the injection needle through the two-position six-way valve, and the injection needle is connected to the sample bottle.

[0015] Preferably, the moving mechanism includes a transmission mechanism, a driving mechanism and a needle seat, the transmission mechanism includes a horizontal transmission mechanism and a vertical transmission mechanism, the needle seat is connected to both the horizontal transmission mechanism and the vertical transmission mechanism, the horizontal transmission mechanism can drive the needle seat to move in the horizontal direction, and the vertical transmission mechanism can drive the needle seat to move in the vertical direction.

[0016] Preferably, the moving mechanism comprises a stepping motor, and the stepping motor is connected to both the horizontal transmission mechanism and the vertical transmission mechanism.

[0017] Preferably, the horizontal transmission mechanism includes a mounting seat, a synchronous belt and two synchronous pulleys, the synchronous belt and the two synchronous pulleys are installed above the mounting seat, the synchronous belt is connected to the synchronous pulleys, the needle seat is connected to the bottom of the mounting seat, and can move horizontally along the bottom of the mounting seat.

[0018] Preferably, the vertical transmission mechanism comprises a screw rod and a guide rail, the screw rod and the guide rail are parallel and are both connected to the mounting seat, and the needle seat is connected to the screw rod through the nut.

[0019] Preferably, the injection parameters include: sample position, injection mode, injection volume, quantitative loop volume and additional volume, the additional volume is the volume from the injection needle to the two-position six-way valve, and the sample position is a preset position in the sample bottle and collection bottle placement area.

[0020] Preferably, the collection parameters include: collection position, collection mode, automatic bottle cutting switch, starting threshold, ending threshold, collection volume, and liquid chromatography system flow rate. The starting threshold and the ending threshold are set when the collection mode is set to threshold collection.

[0021] Preferably, the spotting parameters include the length of the thin layer plate, the width of the thin layer plate, the distance between the spotting point and the bottom edge, the sample height, the spotting direction, the spotting method, the number of spotting times, and the single spotting volume.

[0022] Preferably, before performing automatic sampling-fraction collection-automatic spotting, the control system sets the injection parameters, collection parameters and spotting parameters.

[0023] Preferably, when setting the spotting parameters, the thin layer plate is placed in the thin layer plate placement area, and the scales in the X and Y directions of the thin layer plate placement area are read to obtain the length and width of the thin layer plate. The control system divides the spotting area and sorts it according to the specifications of the thin layer plate and the number of spotting times.

[0024] Preferably, the automatic sampling process comprises:

[0025] The control system controls the moving mechanism to move horizontally according to the injection parameters, so that the injection needle moves to above the sample bottle, and then controls the moving mechanism to move vertically downward, so that the injection needle vertically enters the sample bottle;

[0026] The control system controls the pipeline device to switch the pipeline according to the injection parameters, so that the injection needle is connected to the syringe through the quantitative loop;

[0027] The control system controls the syringe to perform an extraction operation according to the injection parameters, draws the sample into the quantitative loop, and completes the injection.

[0028] Preferably, the fraction collection process comprises:

[0029] After the injection is completed, the control system controls the pipeline device to switch the pipeline according to the collection parameters, so that the quantitative loop is connected to the infusion pump and the chromatographic column, and the detector is connected to the waste liquid bucket or the collection bottle according to whether collection is required;

[0030] The mobile phase is input into the quantitative loop via the infusion pump, and the sample is flushed from the quantitative loop into the chromatographic column, and then enters the detector after separation by the chromatographic column. The components enter the waste liquid barrel or collection bottle through the detector, and the part entering the collection bottle is the collected component, thus completing the fraction collection.

[0031] Preferably, when collection is required, the fraction collection process includes:

[0032] After the injection is completed, the control system controls the moving mechanism to move to the top of the collection bottle according to the set starting threshold, ending threshold and collection position, and then controls the moving mechanism to move vertically downward so that the injection needle vertically enters the collection bottle;

[0033] The control system switches the pipeline connection relationship so that the detector is connected to the collection bottle and the effluent begins to be collected;

[0034] When the automatic bottle cutting function is turned on, the control system automatically switches the injection needle to the next collection position according to the flow rate and the volume of the collection bottle;

[0035] When the collection is completed, the control system switches the pipeline connection relationship, cuts off the connection between the detector and the collection bottle, the moving mechanism moves vertically upward, and the injection needle moves out of the collection bottle to complete the collection.

[0036] Preferably, the spotting process comprises:

[0037] After the fraction collection is completed, the control system controls the moving mechanism to move horizontally, so that the injection needle moves to the top of the first collection bottle, the control system controls the moving mechanism to move vertically downward, so that the injection needle vertically enters the collection bottle, and the control system controls the syringe to perform an extraction operation to absorb a set volume of the spot sample;

[0038] The control system controls the moving mechanism to move, so that the injection needle moves to the first spotting area. The control system controls the moving mechanism to move vertically downward, so that the injection needle drops to the set spotting height. The control system controls the syringe to push the sample sucked therein to discharge it to the first spotting area, thus completing one "spotting" operation.

[0039] Repeat the above process to complete the set number of spotting times for each sample;

[0040] After all fractions have been spotted, the automatic spotting is complete.

[0041] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0042] (1) The automatic sampling, fraction collection and automatic spotting of the utility model are controlled by the operating system alone, which effectively avoids the problems of poor compatibility and low synchronization of multiple control systems;

[0043] (2) The utility model has a high degree of automation. The entire process only requires manual setting of parameters, placement of samples and thin layer plates of required specifications, and the remaining steps can be completed automatically by the system, effectively avoiding the waste of samples, solvents, thin layer plates, time and other costs due to human error. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 This is a schematic diagram of the sample bottle, collection bottle, and thin layer plate placement area of ​​an embodiment of the utility model;

[0045] Figure 2 It is a schematic diagram of the X-axis, two positions of the Y-axis, and the position of the Z-axis of an embodiment of the utility model;

[0046] Figure 3 It is a front view schematic diagram of a moving mechanism of an embodiment of the utility model;

[0047] Figure 4 This is a schematic diagram of pipeline connection during sample injection in one embodiment of the utility model;

[0048] Figure 5 This is a schematic diagram of pipeline connection when the fraction collection of one embodiment of the utility model uses a waste liquid barrel to collect waste liquid;

[0049] Figure 6 This is a schematic diagram of pipeline connection when a collection bottle is used to collect samples for fraction collection in one embodiment of the utility model;

[0050] Figure 7 It is a schematic diagram of the setting interface of injection parameters of an embodiment of the utility model;

[0051] Figure 8 It is a schematic diagram of a setting interface of collection parameters of an embodiment of the utility model;

[0052] Fig. 9 It is a schematic diagram of a setting interface of spotting parameters of an embodiment of the utility model;

[0053] As shown in the figure, 1-sample bottle and collecting bottle placement area; 2-thin layer plate placement area; 3-X direction area ruler; 4-Y direction area ruler; 5-X axis; 6-Y axis first position; 7-Y axis second position; 8-Z axis; 9-needle seat; 10-injection needle; 11-guide rail; 12-screw rod; 13-nut; 14-synchronous pulley; 15-synchronous belt; 16-stepping motor; 17-syringe; 18-quantitative loop; 19-first two-position three-way valve; 20-infusion pump; 21-chromatographic column; 22-detector; 23-second two-position three-way valve; 24-waste liquid; 25-waste liquid barrel; 26-sample bottle; 27-collecting bottle; 28-two-position six-way valve. DETAILED DESCRIPTION

[0054] The specific implementation of the utility model is described in detail below in conjunction with the accompanying drawings.

[0055] The utility model provides an automatic sampling-fraction collection-automatic sampling integrated system, comprising: an automatic sampling-fraction collection-automatic sampling integrated device and a control system;

[0056] The automatic sampling-fraction collection-automatic spotting integrated device is connected to the control system, and the control system sets the sampling parameters, collection parameters and spotting parameters, and controls the automatic sampling-fraction collection-automatic spotting integrated device to complete automatic sampling, fraction collection and automatic spotting according to the set sampling parameters, collection parameters and spotting parameters;

[0057] The automatic sampling-fraction collection-automatic spotting integrated device comprises a moving mechanism, a pipeline device, a thin layer plate placement area 2 and a sample bottle and collection bottle placement area 1, and the moving mechanism and the pipeline device are both connected to the control system;

[0058] The thin layer plate placement area 2 is provided with an X-direction area scale 3 and a Y-direction area scale 4 in the X-direction and the Y-direction respectively;

[0059] The moving mechanism is controlled by the control system to drive the injection needle 10 to move in the horizontal and vertical directions;

[0060] The pipeline device is controlled by the control system to switch the pipeline connection state, so as to complete the injection, fraction collection and spotting respectively; the pipeline device includes a quantitative loop 18 and a pipeline, and the pipeline device is connected with the syringe 17, the injection needle 10, the infusion pump 20 and the chromatographic column 21; one end of the chromatographic column 21 is also connected with a detector 22; the quantitative loop 18 is connected with the syringe 17 and the injection needle 10, or the quantitative loop 18 is connected with the infusion pump 20 and the chromatographic column 21;

[0061] The control system controls the pushing and withdrawing action of the syringe 17 according to the set injection parameters, collection parameters and spotting parameters.

[0062] In some embodiments of the present invention, the pipeline device also includes a two-position six-way valve 28, a first two-position three-way valve 19 and a second two-position three-way valve 23, the two-position six-way valve 28 can be connected to the first two-position three-way valve 19, the two-position six-way valve 28 is connected to the quantitative ring 18 and the syringe 17, the first two-position three-way valve 19 is connected to the second two-position three-way valve 23, and the control system controls the connection position of the two-position six-way valve 28, the first two-position three-way valve 19 and the second two-position three-way valve 23 according to the set injection parameters, collection parameters and spotting parameters.

[0063] In some embodiments of the utility model, when injecting and not collecting fractions, the first two-position three-way valve 19 is connected to the two-position six-way valve 28, and the second two-position three-way valve 23 is connected to the waste liquid 24 collection barrel; when collecting fractions, the second two-position three-way valve 23 is connected to the collection bottle 27; when injecting, the syringe 17 is connected to the quantitative ring 18 through the two-position six-way valve 28, the quantitative ring 18 is connected to the injection needle 10 through the two-position six-way valve 28, and the injection needle 10 is connected to the sample bottle 26.

[0064] In some embodiments of the present utility model, the moving mechanism includes a transmission mechanism, a driving mechanism and a needle seat 9, the transmission mechanism includes a horizontal transmission mechanism and a vertical transmission mechanism, the needle seat 9 is connected to both the horizontal transmission mechanism and the vertical transmission mechanism, the horizontal transmission mechanism can drive the needle seat 9 to move in the horizontal direction, and the vertical transmission mechanism can drive the needle seat 9 to move in the vertical direction.

[0065] In some embodiments of the present invention, the moving mechanism includes a stepping motor 16, and the stepping motor 16 is connected to both the horizontal transmission mechanism and the vertical transmission mechanism.

[0066] In some embodiments of the utility model, the horizontal transmission mechanism includes a mounting seat, a synchronous belt 15 and two synchronous pulleys 14, the synchronous belt 15 and the two synchronous pulleys 14 are installed above the mounting seat, the synchronous belt 15 is connected to the synchronous pulleys 14, and the needle seat 9 is connected to the bottom of the mounting seat and can move horizontally along the bottom of the mounting seat.

[0067] In some embodiments of the present invention, the vertical transmission mechanism includes a screw rod 12 and a guide rail 11 , the screw rod 12 and the guide rail 11 are parallel and are both connected to the mounting seat, and the needle seat 9 is connected to the screw rod 12 through the nut 13 .

[0068] In some embodiments of the present invention, the injection parameters include: sample position, injection method, injection volume, volume of the quantitative loop 18 and additional volume, the additional volume is the volume from the injection needle 10 to the two-position six-way valve 28, and the sample position is the preset position in the sample bottle and collection bottle placement area 1.

[0069] In some embodiments of the present invention, the collection parameters include: collection position, collection mode, automatic bottle cutting switch, starting threshold, ending threshold, collection volume, and liquid chromatography system flow rate. The starting threshold and the ending threshold are set when the collection mode is set to threshold collection.

[0070] In some embodiments of the present invention, the spotting parameters include the length of the thin layer plate, the width of the thin layer plate, the distance between the spotting point and the bottom edge, the sample height, the spotting direction, the spotting method, the number of spotting times, and the single spotting volume.

[0071] In some embodiments of the present invention, before performing automatic injection-fraction collection-automatic spotting, the control system sets injection parameters, collection parameters and spotting parameters.

[0072] In some embodiments of the utility model, when setting the spotting parameters, the thin layer plate is placed in the thin layer plate placement area 2, the X-direction area scale 3 and the Y-direction area scale 4 of the thin layer plate placement area 2 are read to obtain the length and width of the thin layer plate, and the control system divides the spotting areas and sorts them according to the specifications of the thin layer plate and the number of spotting times.

[0073] In some embodiments of the present invention, the automatic injection process includes:

[0074] The control system controls the moving mechanism to move horizontally according to the injection parameters, so that the injection needle 10 moves to above the sample bottle 26, and then controls the moving mechanism to move vertically downward, so that the injection needle 10 vertically enters the sample bottle 26;

[0075] The control system controls the pipeline device to switch the pipeline according to the injection parameters, so that the injection needle 10 is connected to the syringe 17 through the quantitative ring 18;

[0076] The control system controls the injector 17 to perform extraction operation according to the injection parameters, and draws the sample into the quantitative ring 18 to complete the injection.

[0077] In some embodiments of the present invention, the fraction collection process comprises:

[0078] After the injection is completed, the control system controls the pipeline device to switch the pipeline according to the collection parameters, so that the quantitative loop 18 is connected to the infusion pump 20 and the chromatographic column 21, and the detector 22 is connected to the waste liquid bucket 25 or the collection bottle 27 according to whether collection is required;

[0079] The mobile phase is input into the quantitative loop 18 via the infusion pump 20, and the sample is flushed from the quantitative loop 18 into the chromatographic column 21, and then enters the detector 22 after separation by the chromatographic column 21. The components enter the waste liquid barrel 25 or the collection bottle 27 through the detector 22, and the part entering the collection bottle is the collected component, thereby completing the fraction collection.

[0080] In some embodiments of the present invention, when collection is required, the fraction collection process includes:

[0081] After the injection is completed, the control system controls the moving mechanism to move to the top of the collection bottle 27 according to the set starting threshold, ending threshold and collection position, and then controls the moving mechanism to move vertically downward, so that the injection needle 10 vertically enters the collection bottle 27;

[0082] The control system switches the pipeline connection relationship so that the detector 22 is connected to the collection bottle 27, and the outflow liquid begins to be collected;

[0083] When the automatic bottle cutting function is turned on, the control system automatically switches the injection needle 10 to the next collection position according to the flow rate and the volume of the collection bottle 27;

[0084] When the collection is completed, the control system switches the pipeline connection relationship, cuts off the connection between the detector 22 and the collection bottle 27, the moving mechanism moves vertically upward, and the injection needle 10 moves out of the collection bottle 27 to complete the collection.

[0085] In some embodiments of the present invention, the spotting process includes:

[0086] After the fraction collection is completed, the control system controls the moving mechanism to move horizontally, so that the injection needle 10 moves to the top of the first collection bottle 27, and the control system controls the moving mechanism to move vertically downward, so that the injection needle 10 vertically enters the collection bottle 27, and the control system controls the syringe 17 to perform an extraction operation to absorb a set volume of the spot sample;

[0087] The control system controls the moving mechanism to move, so that the injection needle 10 moves to the first spotting area. The control system controls the moving mechanism to move vertically downward, so that the injection needle 10 drops to the set spotting height. The control system controls the syringe 17 to push the sample sucked therein to discharge it to the first spotting area, thus completing a "spotting" operation.

[0088] Repeat the above process to complete the set number of spotting times for each sample;

[0089] After all fractions have been spotted, the automatic spotting is complete.

[0090] According to a specific implementation scheme of the present invention, the implementation process of automatic sampling - fraction collection - automatic spotting of the automatic sampling - fraction collection - automatic spotting integrated system of the present invention is described in detail below.

[0091] 1. Place the sample Figure 1 Place the sample and collection bottles in area 1, as shown in Figure 7 The injection parameter setting interface shown is used to fill in the injection parameters; for example, the parameters in the figure are set as follows: injection position: a (can be filled in according to the actual needs of the operator, and can be any one of the preset positions in the system), injection volume: bμL, additional volume (the volume from the injection needle 10 to the two-position six-way valve 28): cμL, injection mode: full-loop injection, quantitative loop volume: dμL; the full-loop injection mode is one of the liquid chromatography injection modes, and there are also but not limited to "injection mode without sample loss" and "injection mode with sample loss" (different modes can be set in different embodiments).

[0092] 2. Press Figure 8 The collection parameter setting interface shown is used to set the collection parameters; for example, the settings in the figure are: collection position: e (can be filled in according to the actual needs of the operator, which can be any of the preset positions in the system), automatic bottle cutting: on, collection volume: fμL, system flow rate: vmL / min, collection mode: threshold collection, starting threshold: jmAU, ending threshold: kmAU;

[0093] 3. Place the thin layer plate Figure 1In the thin layer plate placement area 2, read the X-direction area ruler 3 to get the thin layer plate length, recorded as "l", read the Y-direction area ruler 4 to get the thin layer plate width, recorded as "w", according to Fig. 9 Fill in the spotting parameters in the spotting parameter setting interface shown; for example, the settings in the figure are: thin layer plate length: lmm, thin layer plate width: wmm, bottom edge height (the height of the spotting point from the bottom edge): hmm, number of samples: m, spotting direction: horizontal, spotting method: strip, number of spots: n times / sample, single volume: pμL; the thin layer plate length, thin layer plate width and bottom edge height are used to "inform" the control system of the initial position of the thin layer plate, so as to calculate the starting spotting position and the spacing between multiple spotting points.

[0094] 4. After setting the injection, collection and spotting methods, save the set parameters;

[0095] 5. Start the operation. After the moving mechanism moves along the X-axis 5 and the first position 6 of the Y-axis (the injection moving range of the moving mechanism in the Y direction) to the top of the sample bottle 26 at the injection position a, the moving mechanism moves downward along the Z-axis 8 (vertical direction) (see Figure 3 ), so that the injection needle 10 vertically enters the sample bottle 26;

[0096] 6. The control system controls the pipeline device to switch the pipeline connection state. The pipeline connection switches to Figure 4 In the state shown, the control system controls the syringe 17 to process the extraction operation, and a total of (c+d) μL of sample is drawn. The sample in the sample bottle 26 is passed from the injection needle 10 to the first two-position three-way valve 19 to the two-position six-way valve 28 to the quantitative loop (18); the automatic injection is completed;

[0097] 7. The control system controls the pipeline device to switch the pipeline connection state. The pipeline connection switches to Figure 5 State, after the sample enters the chromatographic system, the mobile phase is input into the two-position six-way valve 28 via the infusion pump 20, and the sample is flushed from the quantitative loop 18 into the chromatographic column 21, and then enters the detector 22 after being separated by the chromatographic column 21;

[0098] 8-1. If the effluent from the detector 22 does not need to be collected, the waste liquid 24 is directly discharged into the waste liquid bucket 25;

[0099] 8-2. If the effluent from the detector 22 needs to be collected, according to the set threshold collection signal (collection starts when the response value reaches jmAU, and collection stops when the response value reaches kmAU) and the collection position e, the moving mechanism moves horizontally along the X-axis 5 and the second position 6 of the Y-axis to move the injection needle 10 to the top of the collection bottle 27, and the moving mechanism moves vertically downward along the Z-axis 8, and the injection needle 10 vertically enters the collection bottle 27, and the first two-position three-way valve 19 and the second two-position three-way valve 23 are switched to the II position (such as Figure 6), the effluent begins to be collected. When the automatic bottle cutting function is on, the control system can automatically switch the injection needle to the next collection position (current collection position number + 1) according to the flow rate v and the collection bottle volume f to prevent the effluent from overflowing; the collection is completed;

[0100] 9. After the collection is completed, the control system switches the first two-position three-way valve 19 and the second two-position three-way valve 23 to position I, and the moving mechanism moves vertically upward along the Z axis 8, so that the injection needle 10 moves out of the collection bottle 27 and stands by;

[0101] 10. After all fractions are collected, the control system controls the moving mechanism to move along the X-axis 5 and the first position 6 of the Y-axis so that the injection needle 10 moves to the top of the first collection bottle 27, and the moving mechanism moves vertically downward along the Z-axis 8, and the injection needle 10 vertically enters the collection bottle 27, and the syringe 17 performs an extraction operation to absorb a single volume of sample set for sampling;

[0102] 11. According to the set parameters such as the thin layer plate specifications (l×w), the number of samples m, and the spotting direction, the control system divides the thin layer plate into equal areas. The control system controls the moving mechanism to automatically move to the first spotting area along the X-axis 5 and the second position 7 of the Y-axis (the spotting moving range of the moving mechanism in the Y direction), and the moving mechanism moves vertically downward along the Z-axis 8. After the injection needle 10 drops to the spotting height x, the syringe 17 performs a pushing operation to discharge the sample absorbed in step 10 to the spotting area, thus completing a "spot spotting". Repeat steps 10 and 11 to complete the spotting action n times / sample;

[0103] 12. After all fractions are spotted, the entire process of automatic injection - fraction collection - automatic spotting is completed.

[0104] The above description is only a preferred embodiment of the utility model and is not intended to limit the utility model. For those skilled in the art, the utility model may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model are included in the protection scope of the utility model.

Claims

1. An automatic sampling-fraction collection-automatic spotting integrated system, characterized in that: include: Automatic sampling-fraction collection-automatic spotting integrated device and control system; The automatic sampling-fraction collection-automatic spotting integrated device is connected to the control system, and the control system sets the sampling parameters, collection parameters and spotting parameters, and controls the automatic sampling-fraction collection-automatic spotting integrated device to complete automatic sampling, fraction collection and automatic spotting according to the set sampling parameters, collection parameters and spotting parameters; The automatic sampling-fraction collection-automatic spotting integrated device comprises a moving mechanism, a pipeline device, a thin layer plate placement area, and a sample bottle and collection bottle placement area, and the moving mechanism and the pipeline device are both connected to the control system; The thin layer plate placement area is provided with scales in the X direction and the Y direction respectively; The moving mechanism is controlled by the control system to drive the injection needle to move in horizontal and vertical directions; The moving mechanism includes a transmission mechanism, a driving mechanism, a stepping motor and a needle seat, the transmission mechanism includes a horizontal transmission mechanism and a vertical transmission mechanism, the needle seat is connected to both the horizontal transmission mechanism and the vertical transmission mechanism, the horizontal transmission mechanism can drive the needle seat to move in the horizontal direction, and the vertical transmission mechanism can drive the needle seat to move in the vertical direction; the stepping motor is connected to both the horizontal transmission mechanism and the vertical transmission mechanism; The pipeline device is controlled by the control system to switch the pipeline connection state, so as to complete the injection, fraction collection and spotting respectively; the pipeline device includes a quantitative loop, a pipeline, a two-position six-way valve, a first two-position three-way valve and a second two-position three-way valve, and the pipeline device is connected with a syringe, a sample injection needle, an infusion pump and a chromatographic column; one end of the chromatographic column is also connected with a detector; the quantitative loop is connected with the syringe and the sample injection needle, or the quantitative loop is connected with the infusion pump and the chromatographic column; The two-position six-way valve is connectable to the first two-position three-way valve, the two-position six-way valve is connected to the quantitative loop and the syringe, the first two-position three-way valve is connected to the second two-position three-way valve, and the control system controls the communication positions of the two-position six-way valve, the first two-position three-way valve and the second two-position three-way valve according to the set injection parameters, collection parameters and spotting parameters; The control system controls the pushing and drawing actions of the syringe according to the set injection parameters, collection parameters and spotting parameters.

2. The automatic sampling-fraction collection-automatic spotting integrated system according to claim 1, characterized in that: When injecting and not collecting fractions, the first two-position three-way valve is connected to the two-position six-way valve, and the second two-position three-way valve is connected to the waste liquid collection bucket. When collecting fractions, the second two-position three-way valve is connected to the collection bottle. When injecting, the syringe is connected to the quantitative loop through the two-position six-way valve, the quantitative loop is connected to the injection needle through the two-position six-way valve, and the injection needle is connected to the sample bottle.

3. The automatic sampling-fraction collection-automatic spotting integrated system according to claim 1, characterized in that: The horizontal transmission mechanism includes a mounting seat, a synchronous belt and two synchronous pulleys, the synchronous belt and the two synchronous pulleys are installed above the mounting seat, the synchronous belt is connected to the synchronous pulleys, the needle seat is connected to the bottom of the mounting seat and can move horizontally along the bottom of the mounting seat; the vertical transmission mechanism includes a screw rod and a guide rail, the screw rod and the guide rail are parallel and are both connected to the mounting seat, and the needle seat is connected to the screw rod through a nut.

4. The automatic sampling-fraction collection-automatic spotting integrated system according to claim 1, characterized in that: The injection parameters include: sample position, injection mode, injection volume, quantitative loop volume and additional volume. The additional volume is the volume from the injection needle to the two-position six-way valve. The sample position is the preset position in the sample bottle and collection bottle placement area.

5. The automatic sampling-fraction collection-automatic spotting integrated system according to claim 4, characterized in that: The collection parameters include: collection position, collection mode, automatic bottle cutting switch, starting threshold, ending threshold, collection volume, and liquid chromatography system flow rate. The starting threshold and the ending threshold are set when the collection mode is set to threshold collection.

6. The automatic sampling-fraction collection-automatic spotting integrated system according to claim 5, characterized in that: The spotting parameters include the length of the thin layer plate, the width of the thin layer plate, the distance between the spotting point and the bottom edge, the sample height, the spotting direction, the spotting method, the number of spotting times, and the single spotting volume.

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