Traditional Chinese medicine component full-automatic sample preparation system

Abstract

The application provides a traditional Chinese medicine component full-automatic sample preparation system, which comprises a solvent system, a multi-element high-pressure chromatographic pump, a solid sample loader, a liquid chromatograph, a liquid sample feeding mechanism and a centrifugal mechanism which are connected in sequence; the solid sample loader has a sample loading station, and the sample loading station is provided with a sample loading column containing medicine columns; the multi-element high-pressure chromatographic pump is used for pumping a mobile phase formed by mixing at least two solvents to the solid sample loader, and the mobile phase passes through the sample loading column to dissolve target components in the medicine columns; the liquid chromatograph is used for chromatographic separation, detection and analysis of the target components to elute and prepare different components; the liquid sample feeding mechanism comprises a plurality of enrichment column valve groups, and the centrifugal mechanism comprises a plurality of centrifugal concentration units which are respectively connected with the enrichment column valve groups in correspondence. The traditional Chinese medicine component full-automatic sample preparation system provided by the application can obtain samples of multiple different components at the same time, and can improve the traditional Chinese medicine component sample preparation efficiency.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of traditional Chinese medicine sample preparation automation, and particularly relates to a full-automatic sample preparation system for traditional Chinese medicine components. BACKGROUND

[0002] Traditional Chinese medicine component research is of great significance in revealing chemical substances of traditional Chinese medicine, clarifying effective components and effective parts of traditional Chinese medicine, revealing the mechanism of traditional Chinese medicine, and formulating quality standards of traditional Chinese medicine. Liquid chromatography is a modern separation technology with high efficiency, rapidness and wide application. It is a modern chromatographic analysis method developed by using high-pressure delivery mobile phase, high-efficiency stationary phase and high-sensitivity detector, and is an indispensable tool for analyzing traditional Chinese medicine components.

[0003] At present, the automatic equipment for sample preparation of traditional Chinese medicine components is mostly composed of a liquid chromatograph and some peripheral auxiliary units such as a solvent system and a centrifugal concentration unit, thereby forming a sample preparation process line. However, the existing equipment cannot realize one-time output of different sample solutions of traditional Chinese medicine components, and needs to separately set corresponding equipment to obtain different sample solutions, and then mix the solvent into the mobile phase through a sample feeder and then enter the liquid chromatograph for chromatographic separation and detection. Moreover, the existing equipment also has the problem that the separation and preparation speed of traditional Chinese medicine components is not synchronized with the recovery speed of component solvents, and the component preparation and component solvent recovery are seriously disconnected, cannot realize the integration of the solvent recovery part and the liquid chromatograph, and still rely on manual auxiliary operation in many cases. These are important factors restricting the sample preparation efficiency of traditional Chinese medicine components and must be overcome to realize the complete automation of the sample preparation equipment. SUMMARY

[0004] The embodiment of the application provides a full-automatic sample preparation system for traditional Chinese medicine components, which aims to realize the complete automation of the sample preparation process of traditional Chinese medicine components and can simultaneously prepare a plurality of different powder samples of traditional Chinese medicine components, thereby improving the sample preparation efficiency of traditional Chinese medicine components.

[0005] To achieve the above object, the technical scheme adopted by the application is as follows: a full-automatic sample preparation system for traditional Chinese medicine components is provided, which comprises a solvent system, a multi-element high-pressure chromatograph pump, a solid sample feeder, a liquid chromatograph, a liquid sample feeding mechanism and a centrifugal mechanism which are sequentially connected on a rack; the solvent system comprises a plurality of storage devices for containing different solvents; the solid sample feeder has a sample feeding station, the sample feeding station is provided with a sample column, and the sample column contains a medicine column; the multi-element high-pressure chromatograph pump is used for pumping a mobile phase mixed by at least two solvents to the solid sample feeder, and the mobile phase passes through the sample column to dissolve target components in the medicine column; the liquid chromatograph is used for chromatographic separation and detection analysis of the target components to prepare sample solutions with different traditional Chinese medicine components; the liquid sample feeding mechanism comprises a plurality of enrichment column valve groups, and the centrifugal mechanism comprises a plurality of centrifugal concentration units which are connected with the enrichment column valve groups one by one in a one-to-one correspondence;

[0006] Each of the enrichment column valve groups is used to discharge sample solutions with different traditional Chinese medicine components to each of the corresponding centrifugal concentration units, and each of the centrifugal concentration units is used to concentrate the sample solutions under a centrifugal environment to remove solvents and obtain powder samples of different traditional Chinese medicine components.

[0007] In a possible implementation, the liquid sample feeding mechanism further comprises an injection pump arranged on the rack, and the injection pump is used to sequentially inject eluents into each of the enrichment column valve groups.

[0008] The enrichment column valve group comprises an enrichment column and a two-position six-way valve. The two-position six-way valve has a sample feeding position state in which a first port and a second port are communicated, a third port and a fourth port are communicated, and a fifth port and a sixth port are communicated, and has a sample discharging position state in which the first port and the sixth port are communicated, the second port and the third port are communicated, and the fourth port and the fifth port are communicated. The first port is connected with the multi-element high-pressure chromatography pump, the second port is connected with the centrifugal concentration unit, the enrichment column is connected in series between the third port and the sixth port, the fourth port is used to connect with a solvent recovery device, and the fifth port is connected with a sample injection needle of the injection pump.

[0009] In some embodiments, the solid sample feeder comprises a pressing mechanism, a rotating seat, and a rotary driving member. The pressing mechanism is fixedly connected to the rack, and a pressing end of the pressing mechanism is located directly above the sample loading station. The rotating seat comprises a base and a rotating disc rotatably connected to the rotating seat. A plurality of sample columns are circumferentially arranged on the rotating disc. The plurality of sample columns are cyclically driven by the rotating disc to pass through the sample loading station and sequentially stop at the sample loading station. The rotary driving member is arranged on the rack or the base, and an output end of the rotary driving member is connected to the center of the rotating disc.

[0010] When one of the sample columns stops at the sample loading station, the pressing end of the pressing mechanism seals into the sample column to compress the mixed sample into a medicine column. The mobile phase sequentially passes through the sample column located at the sample loading station.

[0011] For example, the sample column comprises an elastic telescopic assembly and a sample cup. The elastic telescopic assembly is arranged on the rotating disc in a vertical direction. A telescopic end of the elastic telescopic assembly can be contracted downward under an external force and can be reset upward under its own elasticity when the external force is removed. The sample cup is inserted into the elastic telescopic assembly. A top end of the sample cup is open to allow the pressing end of the pressing mechanism to seal into the sample cup. A bottom wall of the sample cup is provided with a liquid inlet.

[0012] The base is provided with a liquid inlet pipe directly below the sample loading station. The liquid inlet pipe is connected with the multi-element high-pressure chromatography pump. The pressing end of the pressing mechanism is provided with a liquid outlet pipe. The liquid outlet pipe is connected with the liquid chromatograph. When the pressing end of the pressing mechanism seals into the sample cup to press the medicine column, the elastic telescopic assembly is contracted to lower the sample cup and insert the liquid inlet pipe into the liquid inlet. When the pressing end of the pressing mechanism is lifted upward, the elastic telescopic assembly drives the sample cup to reset upward to separate the liquid inlet pipe from the liquid inlet.

[0013] For example, the elastic extension assembly comprises two guide sleeves, two guide rods, a sleeve and two elastic members; the two guide sleeves are vertically fixed on the rotary disc and are spaced apart; the two guide rods are respectively slidably arranged in the two guide sleeves, the lower end of the guide rod is provided with a limiting member for limiting the upper sliding limit position of the guide rod; the sleeve is located between the two guide rods and is connected with the top end of the two guide rods, the bottom of the sleeve is provided with a supporting table, the sleeve is suitable for inserting the sample cup and supporting the sample cup through the supporting table; the two elastic members are respectively sleeved on the two guide rods, one end of the elastic member is connected with the guide sleeve, and the other end is connected with the sleeve.

[0014] For example, the sample cup comprises a cup body, a lower connecting flange, a sieve plate and a distribution disc; the upper and lower ends of the cup body are open; the lower connecting flange covers the lower end of the cup body, and the center of the lower connecting flange is provided with a liquid inlet; the sieve plate is arranged in the cup body and abuts against the top wall of the lower connecting flange; the distribution disc is arranged in the cup body and abuts against the sieve plate.

[0015] For example, the pressing mechanism comprises a support, a driving assembly and a piston; the support is fixedly connected to the rack; the driving assembly is vertically fixed on the support, and the output end is downwardly telescopic; the piston is arranged on the output end of the driving assembly and is vertically aligned with the sample loading station, and the piston can be pressed into the sample loading column in the sample loading station under the driving of the driving assembly; wherein the piston is provided with a liquid outlet pipe.

[0016] In some embodiments, the driving assembly comprises two slide rails, a slide seat, a motor and a hollow rod; the two slide rails are respectively vertically fixed on the support and are respectively located on the two sides of the piston; the two ends of the slide seat are respectively slidably connected to the two slide rails, and the middle part is provided with a screw sleeve; a screw rod is vertically screwed in the screw sleeve; the motor is fixedly connected to the support, and the output end is connected to the screw rod; the hollow rod is fixedly connected to the bottom of the slide seat, the hollow rod is vertically aligned with the screw rod, and the inner diameter of the hollow rod is greater than the diameter of the screw rod; wherein the piston is fixedly connected to the bottom end of the hollow rod.

[0017] For example, the periphery of the piston is sleeved with a disengagement ring, and a limiting block is arranged above the disengagement ring on the support; when the piston is inserted into the sample cup, the disengagement ring abuts against the top wall of the sample cup; when the piston is withdrawn from the sample cup, the disengagement ring rises with the piston to abut against the limiting block, thereby abutting against the sample cup to make the sample cup vertically disengage from the piston.

[0018] In some embodiments, the solvent system comprises three storage containers respectively for storing water, methanol and 5% methanol; wherein the mobile phase is a mixed liquid of water and methanol, and the multi-element high-pressure chromatographic pump can pump 5% methanol to the liquid sample loading mechanism.

[0019] The traditional Chinese medicine component full-automatic sample preparation system provided by the application has the beneficial effects that, compared with the prior art, the traditional Chinese medicine component full-automatic sample preparation system adopts a multi-element high-pressure chromatographic pump to mix different solvents in a solvent system to obtain a mobile phase with a specified proportion, the mobile phase enters a sample column of a solid sample feeder under high pressure to penetrate the medicine column, the target traditional Chinese medicine components in the medicine column are dissolved into the mobile phase and enter a liquid chromatograph under high pressure, the target components are mixed into the mobile phase in the form of the mobile phase flushing and dissolving the medicine column, and a corresponding device for preparing a traditional Chinese medicine sample solution is no longer needed, so that automatic solid sample feeding can be realized; the mobile phase is subjected to chromatographic analysis and detection separation by the liquid chromatograph, so that sample solutions with different traditional Chinese medicine components are discharged in sections, and each section is discharged in a quantitative manner to a corresponding centrifugal concentration unit through a corresponding enrichment column valve group by a liquid sample feeding mechanism, so that the sample solutions with different traditional Chinese medicine components are concentrated in a centrifugal environment to remove solvents and obtain powder samples with different traditional Chinese medicine components, the removed solvents can be directly recycled, the speed of traditional Chinese medicine component separation and preparation can be matched with the speed of component solvent recycling, powder samples with multiple different components can be obtained in a full-automatic manner, the device has low energy consumption and small solvent consumption, is conducive to energy saving and environmental protection, and can improve the traditional Chinese medicine component sample preparation efficiency and reduce labor costs. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 A structure schematic diagram of the traditional Chinese medicine component full-automatic sample preparation system provided by the embodiment of the application is provided.

[0021] Figure 2 A structure schematic diagram of the enrichment column valve group adopted by the embodiment of the application is provided.

[0022] Figure 3 Two working state schematic diagrams of the two-position six-way valve provided by the embodiment of the application are provided, wherein the A view is a sample feeding position state, and the B view is a sample discharging position state.

[0023] Figure 4 A three-dimensional structure schematic diagram of the solid sample feeder adopted by the embodiment of the application is provided.

[0024] Figure 5 A cross-sectional structure schematic diagram of the sample column adopted by the embodiment of the application is provided.

[0025] Figure 6 A structure schematic diagram of the pressing mechanism adopted by the embodiment of the application is provided.

[0026] In the figure: 10, rack; 20, solvent system; 21, storage; 30, multi-element high-pressure chromatographic pump; 40, solid sample loader; 400, sample loading column; 4000, liquid inlet; 401, elastic telescopic assembly; 4011, guide sleeve; 4012, guide rod; 4013, sleeve; 4014, elastic member; 4015, limiting member; 402, sample loading cup; 4021, cup body; 4022, lower flange; 4023, sieve plate; 4024, distribution disc; 41, pressing mechanism; 410, liquid outlet pipe; 411, support; 412, driving assembly; 4121, slide rail; 4122, slide base; 4123, motor; 4124, hollow rod; 4125, screw sleeve; 4126, screw rod; 413, piston; 414, disengagement ring; 415, limiting block; 42, transfer seat; 421, base; 4211, liquid inlet pipe; 422, rotary disc; 43, rotary driving member; 50, liquid chromatograph; 51, preparative chromatographic column; 52, ultraviolet detector; 53, data processing system; 60, liquid sample feeding mechanism; 61, enrichment column valve group; 611, enrichment column; 612, two-position six-way valve; 6121, first port; 6122, second port; 6123, third port; 6124, fourth port; 6125, fifth port; 6126, sixth port; 62, syringe pump; 621, sample injection needle; 70, centrifugal concentration unit; 80, solvent recovery device; 90, medicine column. DETAILED DESCRIPTION

[0027] In order to make the technical problems to be solved by the present application, technical solutions and beneficial effects clearer, the present application will be further described in detail below in combination with the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not used to limit the present application.

[0028] It should be noted that when an element is referred to as being "disposed on" another element, it can be directly on the other element or indirectly on the other element. It should be understood that the terms "length", "width", "upper", "lower", "front", "back", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only used to facilitate the description of the present application and simplify the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application. The terms "first", "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features limited by "first", "second" can explicitly or implicitly include one or several of the features. In the description of the present application, the meaning of "a plurality of", "several" is two or more, unless otherwise explicitly specified.

[0029] Please refer toFigures 1 to 6 The present application provides a traditional Chinese medicine component full-automatic sample preparation system. The traditional Chinese medicine component full-automatic sample preparation system comprises a solvent system 20, a multi-element high-pressure chromatographic pump 30, a solid sample loader 40, a liquid chromatograph 50, a liquid sample feeding mechanism 60, and a centrifugal mechanism, which are sequentially connected on a rack 10. The solvent system 20 comprises a plurality of storage containers 21 for containing different solvents. The solid sample loader 40 has a sample loading station provided with a sample loading column 400 in which a medicine column 90 is placed. The multi-element high-pressure chromatographic pump 30 is used to pump a mobile phase formed by mixing at least two solvents to the solid sample loader 40, and the mobile phase passes through the sample loading column 400 to dissolve the target components in the medicine column 90. The liquid chromatograph 50 is used to perform chromatographic separation and detection analysis on the mobile phase in which the target components are dissolved, so as to elute and prepare sample solutions with different traditional Chinese medicine components. The liquid sample feeding mechanism 60 comprises a plurality of enrichment column valve groups 61, and the centrifugal mechanism comprises a plurality of centrifugal concentration units 70 connected with the enrichment column valve groups 61 one by one. Each enrichment column valve group 61 is used to discharge the sample solution with different traditional Chinese medicine components to each corresponding centrifugal concentration unit 70, and each centrifugal concentration unit 70 is used to concentrate the sample solution to remove the solvent and obtain a powder sample with different traditional Chinese medicine components under a centrifugal environment.

[0030] It should be noted that in the present embodiment, the solvent system 20 specifically comprises three storage containers 21 containing methanol, 5% methanol, and water respectively. The storage container 21 is a sealed tank structure with a liquid level window and an inlet and outlet liquid pipeline interface. The multi-element high-pressure chromatographic pump 30 specifically comprises four high-pressure pumps configured with an online mixer, which can work independently. The working mode is that the four high-pressure pumps are connected in parallel, and four mobile phases can be simultaneously fed into the mixer after the pump according to the preset ratio. The mobile phase is mixed under high pressure, and the mixing ratio is accurate with few bubbles. There is no need to repeatedly clean for switching the mobile phase, which not only saves solvent but also improves work efficiency. The multi-element high-pressure chromatographic pump 30 is a mature device in the prior art, and will not be described in detail here.

[0031] It should be explained that the liquid chromatograph 50 is a common device in the art, and in the embodiment, the liquid chromatograph 50 at least includes a preparative chromatographic column 51, an ultraviolet detector 52, and a data processing system 53 with an operation interface; wherein the mobile phase in which the target component is dissolved enters the preparative chromatographic column 51 to undergo repeated adsorption and desorption distribution processes, that is, different components are separated by using the difference in moving speed, and after separation, they are discharged from the preparative chromatographic column 51 into the ultraviolet detector 52. In the ultraviolet detector 52, the component concentration is converted into an electrical signal and transmitted to the data processing system 53, and the data is displayed in the form of a graph on the operation interface. After the ultraviolet detector 52, the separated traditional Chinese medicine components are cut and segmented into the respective enrichment column valve groups 61.

[0032] Compared with the prior art, the multi-element high-pressure chromatographic pump 30 provided in the embodiment can mix different solvents in the solvent system 20 to obtain a mobile phase with a specified proportion. The mobile phase enters the sample loading column 400 of the solid sample loader 40 under high pressure to penetrate the medicine column 90, so that the target traditional Chinese medicine component in the medicine column 90 is dissolved into the mobile phase and enters the liquid chromatograph 50 under high pressure. In this way, the target component is mixed into the mobile phase by flushing and dissolving the medicine column 90 with the mobile phase, and there is no need to separately configure a corresponding device to prepare a traditional Chinese medicine sample solution, so that automatic solid sample loading can be realized. The liquid chromatograph 50 can perform chromatographic separation and detection analysis on the mobile phase, so that sample solutions with different traditional Chinese medicine components can be eluted and discharged in segments, and each segment is quantitatively discharged to the corresponding centrifugal concentration unit 70 through the corresponding enrichment column valve group 61 by the liquid sample feeding mechanism 60. In this way, the sample solutions with different traditional Chinese medicine components are concentrated in a centrifugal environment to remove the solvent and obtain powder samples with corresponding traditional Chinese medicine components. The removed solvent can be directly recycled, which can ensure that the speed of traditional Chinese medicine component separation and preparation matches the speed of component solvent recovery, realize the simultaneous acquisition of sample solutions with multiple different components in a fully automated manner, reduce energy consumption and solvent consumption, be conducive to energy saving and environmental protection, and improve the efficiency of traditional Chinese medicine component sample preparation and reduce labor costs.

[0033] It should be noted that in the embodiment, referring to Figures 1 to 3The liquid sample feeding mechanism 60 further comprises an injection pump 62 arranged on the frame 10, and the injection pump 62 is used for sequentially injecting different components of eluent into each enrichment column valve group 61; wherein the enrichment column valve group 61 comprises an enrichment column 611 and a two-position six-way valve 612; the two-position six-way valve 612 has a sample feeding state in which the first port 6121 and the second port 6122 are communicated, the third port 6123 and the fourth port 6124 are communicated, and the fifth port 6125 and the sixth port 6126 are communicated, and has a sample discharging state in which the first port 6121 and the sixth port 6126 are communicated, the second port 6122 and the third port 6123 are communicated, and the fourth port 6124 and the fifth port 6125 are communicated; the first port 6121 is connected with the multi-element high-pressure chromatographic pump 30, the second port 6122 is connected with the centrifugal concentration unit 70, the enrichment column 611 is connected in series between the third port 6123 and the sixth port 6126, the fourth port 6124 is used for connecting the solvent recovery device 80, and the fifth port 6125 is connected with the injection needle 621 of the injection pump 62.

[0034] In the sample feeding state, the injection pump 62 injects sample solution with corresponding traditional Chinese medicine components from the fifth port 6125 through the injection needle 621, and when the solvent sequentially passes through the sixth port 6126 and the third port 6123 and is discharged from the fourth port 6124 to the solvent recovery device 80, it indicates that the enrichment column 611 is filled with sample solution with the traditional Chinese medicine components. At the same time, one of the high-pressure pumps of the multi-element high-pressure chromatographic pump 30 discharges eluent into the first port 6121 and discharges it from the second port 6122 into the centrifugal concentration unit 70; in the sample discharging state, the eluent enters the sixth port 6126 from the first port 6121, then passes through the enrichment column 611 and enters the second port 6122 from the third port 6123, and then enters the centrifugal concentration unit 70. In this process, the traditional Chinese medicine components in the enrichment column 611 that have been quantitatively enriched are eluted into the centrifugal concentration unit 70, thereby realizing the quantitative transfer of the traditional Chinese medicine components.

[0035] In some possible implementation manners, refer to Figures 4 to 6 The solid sample feeder 40 comprises a pressing mechanism 41, a rotating seat 42, and a rotary driving member 43; the pressing mechanism 41 is fixedly connected to the frame 10, and a pressing end of the pressing mechanism 41 is located directly above the sample loading station; the rotating seat 42 comprises a base 421 and a rotating disc 422 rotatably connected to the rotating seat 42, and a plurality of sample loading columns 400 are circumferentially arranged on the rotating disc 422; the plurality of sample loading columns 400 are driven by the rotating disc 422 to cyclically pass through the sample loading station and sequentially stop at the sample loading station; the rotary driving member 43 is arranged on the frame 10 or the base 421, and an output end thereof is connected to the center of the rotating disc 422; wherein when one of the sample loading columns 400 stops at the sample loading station, the pressing end of the pressing mechanism 41 sealingly extends into the sample loading column 400 to compress the sample filling material (i.e., the traditional Chinese medicine sample solidified by the filling material) into a medicine column 90; the mobile phase sequentially passes through the sample loading column 400 located at the sample loading station.

[0036] The quantitative mixed sample filler is directly put into the sample column 400, and then the pressing end of the pressing mechanism 41 is inserted into the sample column 400 to press the mixed sample filler to form a certain density to form the sample column 90, and a constant pressure is continuously and stably applied to ensure that the sample column 90 does not appear to be locally collapsed, and the target components in the sample column 90 are dissolved into the flow phase by the process of the flow phase passing through the sample column 400, and then enter the liquid chromatograph 50 for chromatographic separation. When the Chinese medicine components contained in the sample column 90 in one sample column 400 are dissolved and carried away by the flow phase, the next sample column 400 enters the sample loading position by rotating the rotating drive 43 to drive the rotating seat 42 to rotate, thereby realizing the integration and automation of solid sample loading and chromatographic detection, and continuously and uninterruptedly loading the solid sample, thereby improving the sample preparation efficiency.

[0037] It should be understood that a position for loading and unloading can be arranged on the side of the solid sample loader 40, and manual operation or automatic operation of a mechanical hand can be used to replace the sample column 400 that has completed the solid sample loading in the position.

[0038] In the embodiment, referring to Figure 5 The sample column 400 includes an elastic telescopic assembly 401 and a sample cup 402. The elastic telescopic assembly 401 is arranged on the rotating disc 422 in the vertical direction, and the telescopic end can be contracted downward under the action of an external force and reset upward under the action of its own elasticity when the pressing force is removed. The sample cup 402 is inserted into the elastic telescopic assembly 401. The top end of the sample cup 402 is open to allow the pressing end of the pressing mechanism 41 to be sealingly inserted, and the bottom wall of the sample cup 402 is provided with a liquid inlet 4000.

[0039] The bottom seat 421 is provided with a liquid inlet pipe 4211 below the sample loading position, the liquid inlet pipe 4211 is connected with the multi-element high-pressure chromatographic pump 30, the pressing end of the pressing mechanism 41 is provided with a liquid outlet pipe 410, and the liquid outlet pipe 410 is connected with the liquid chromatograph 50. When the pressing end of the pressing mechanism 41 is inserted into the sample cup 402 to press the sample column 90, the elastic telescopic assembly 401 is contracted to lower the sample cup 402 and insert the liquid inlet pipe 4211 with the liquid inlet 4000. When the pressing end of the pressing mechanism 41 is lifted upward, the elastic telescopic assembly 401 drives the sample cup 402 to reset upward to separate the liquid inlet pipe 4211 from the liquid inlet 4000.

[0040] The liquid inlet 4000 and the liquid inlet pipe 4211 are inserted and separated by the up-and-down telescoping of the sample cup 402 in the elastic telescopic assembly 401, the liquid inlet pipe 4211 can realize the liquid inlet communication with each sample column 400 through one liquid inlet pipe 4211, the structure is simple and reliable, the action is logical, and the automatic control is easy.

[0041] Specifically, in the present embodiment, please refer to Figure 5 The elastic extension assembly 401 comprises two guide sleeves 4011, two guide rods 4012, a sleeve 4013, and two elastic members 4014; the two guide sleeves 4011 are respectively fixed vertically on the rotating disc 422 and are spaced apart; the two guide rods 4012 are respectively slidably arranged in the two guide sleeves 4011, the lower end of the guide rod 4012 is provided with a limiting member 4015 for limiting the uppermost position of the guide rod 4012; the sleeve 4013 is located between the two guide rods 4012 and is connected with the top ends of the two guide rods 4012, the bottom of the sleeve 4013 is provided with a receiving table, the sleeve 4013 is suitable for inserting the sample cup 402 and supporting the sample cup 402 through the receiving table; the two elastic members 4014 are respectively sleeved on the two guide rods 4012, one end of the elastic member 4014 is connected with the guide sleeve 4011, and the other end is connected with the sleeve 4013.

[0042] When the pressing end of the pressing mechanism 41 extends into the sample cup 402 and presses downward, the sleeve 4013 and the two guide rods 4012 move downward relative to the two guide sleeves 4011 to form a plug-in connection between the liquid inlet pipe 4211 and the liquid inlet 4000; after the sample is loaded, the pressing end of the pressing mechanism 41 is lifted, the sleeve 4013 and the guide rod 4012 are lifted upward and reset under the elastic force of the elastic member 4014 such as a spring, so that the liquid inlet pipe 4211 is separated from the liquid inlet 4000; the cooperation of the two guide rods 4012 and the two sleeves 4013 can ensure the stability and precision of the up-down movement, and the reset by the elastic member 4014 can improve the response sensitivity of the action.

[0043] As a specific embodiment of the sample cup 402, please refer to Figure 5 The sample cup 402 comprises a cup body 4021, a lower connecting flange 4022, a sieve plate 4023, and a distribution disc 4024; the upper and lower ends of the cup body 4021 are open; the lower connecting flange 4022 covers the lower end of the cup body 4021, and the center of the lower connecting flange 4022 is provided with a liquid inlet 4000; the sieve plate 4023 is arranged in the cup body 4021 and abuts against the top wall of the lower connecting flange 4022; the distribution disc 4024 is arranged in the cup body 4021 and abuts against the sieve plate 4023.

[0044] When the mobile phase enters the sample cup 402, it needs to pass through the sieve plate 4023 and the distribution disc 4024 for filtration to reduce or avoid impurities from entering, so as to ensure the cleanliness of the mobile phase and help improve the purity and quality of the final sample.

[0045] In some embodiments, the above-mentioned pressing mechanism 41 adopts, for example, Figure 6The lower pressing mechanism 41 includes a support 411, a driving assembly 412, and a piston 413; the support 411 is fixedly connected to the rack 10; the driving assembly 412 is vertically fixed to the support 411, and the output end thereof extends downward and is retractable; the piston 413 is arranged at the output end of the driving assembly 412 and is vertically aligned with the upper sample station, and the piston 413 can be pressed into the sample column 400 in the upper sample station under the driving of the driving assembly 412; wherein a liquid outlet pipe 410 is arranged on the piston 413.

[0046] The output end of the driving assembly 412 is provided with the piston 413 capable of being sealingly and plug-in connected with the sample column 400, which can not only extrude the mixed sample in the sample column 400 into the medicine column 90, but also ensure the sealing of the sample column 400, so as to avoid leakage during the flowing of the mobile phase through the sample column 400; in addition, the bottom wall of the piston 413 in the embodiment can be attached with a filter element to filter the impurities insoluble in the mobile phase, so as to avoid the impurities entering the liquid chromatograph 50 with the mobile phase, thereby ensuring the normal service life of the liquid chromatograph 50.

[0047] Specifically, referring to Figure 6 In the embodiment, the optional structure of the driving assembly 412 is that the driving assembly 412 includes two slide rails 4121, a slide base 4122, a motor 4123, and a hollow rod 4124; the two slide rails 4121 are vertically fixed on the support 411 and are respectively located at two sides of the piston 413; the slide base 4122 is slidably connected to the two slide rails 4121 at two ends thereof and is provided with a threaded sleeve 4125 in the middle portion, and a threaded rod 4126 is vertically screwed in the threaded sleeve 4125; the motor 4123 is fixedly connected to the support 411 and is connected to the threaded rod 4126 at the output end; the hollow rod 4124 is fixedly connected to the bottom of the slide base 4122, the hollow rod 4124 is vertically aligned with the threaded rod 4126, and the inner diameter of the hollow rod 4124 is greater than the diameter of the threaded rod 4126; wherein the piston 413 is fixedly connected to the bottom end of the hollow rod 4124.

[0048] The motor 4123 rotates to drive the threaded rod 4126 to rotate relative to the threaded sleeve 4125, and since the threaded rod 4126 cannot move axially, the threaded sleeve 4125 drives the slide base 4122 to slide up and down along the slide rails 4121, so as to drive the hollow rod 4124 fixed to the slide base 4122 to move up and down, thereby realizing the lifting of the piston 413; in this process, the part of the threaded rod 4126 downwardly penetrating through the threaded sleeve 4125 can be accommodated in the hollow rod 4124, and the outer diameter of the hollow rod 4124 is preferably less than or equal to the diameter of the piston 413, so as to avoid the collision between the hollow rod 4124 and the sample column 400.

[0049] It should be noted that, referring to Figure 6In the embodiment, the periphery of the piston 413 is sleeved with a disengagement ring 414, and the support 411 is provided with a limiting block 415 directly above the disengagement ring 414. When the piston 413 extends into the sample cup 402, the disengagement ring 414 is pressed against the top end wall of the sample cup 402. When the piston 413 exits the sample cup 402, the disengagement ring 414 is lifted with the piston 413 to abut against the limiting block 415, thereby pressing against the sample cup 402 to separate the sample cup 402 from the piston 413.

[0050] Since the piston 413 and the sample cup 402 are relatively tightly matched to achieve sealing, the piston 413 will lift the sample cup 402 when the piston 413 is lifted, thereby causing difficulty in separating the piston 413 from the sample cup 402. To avoid the phenomenon that the piston 413 and the sample cup 402 cannot be smoothly separated, the disengagement ring 414 is sleeved on the piston 413, and the limiting block 415 is arranged on the support 411 to limit the upward movement of the disengagement ring 414. When the piston 413 is lifted to abut the disengagement ring 414 against the limiting block 415, the piston 413 continues to be lifted upward, but the disengagement ring 414 cannot move upward any more. Since the disengagement ring 414 is pressed against the top end wall of the sample cup 402, the sample cup 402 cannot move upward with the piston 413, thereby achieving stable separation of the piston 413 from the sample cup 402. The structure is simple and reliable.

[0051] For example, referring to Figure 1 , the solvent system 20 includes three storage containers 21 for storing water, methanol and 5% methanol respectively. The mobile phase is a mixed liquid of water and methanol, and the multi-component high-pressure pump 30 can pump 5% methanol to the liquid sample feeding mechanism 60.

[0052] Specifically, as shown in Figure 1 , the enrichment column valve group 61 is provided with fifteen groups in the embodiment, and the centrifugal concentration unit 70 is also provided with fifteen groups correspondingly. Each group of the enrichment column valve group 61 includes two enrichment columns 611 and two two-position six-way valves 612 corresponding to each other. Each group of the centrifugal concentration unit 70 has two stations for receiving sample solutions of different components discharged by the two two-position six-way valves 612. That is, the embodiment can simultaneously realize sample preparation of thirty kinds of traditional Chinese medicine components, and the process is completely automated.

[0053] The above only describes the preferred embodiments of the present application and is not intended to limit the present application. Any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A traditional Chinese medicine component full-automatic sample preparation system, characterized in that, The device comprises a rack, a solvent system, a multi-element high-pressure chromatographic pump, a solid sample loader, a liquid chromatograph, a liquid sample feeding mechanism, and a centrifugal mechanism, which are sequentially connected to the rack; the solvent system comprises a plurality of storage units for containing different solvents; the solid sample loader has a sample loading station, which is provided with a sample loading column containing a medicine column; the multi-element high-pressure chromatographic pump is used to pump a mobile phase formed by mixing at least two solvents to the solid sample loader, and the mobile phase passes through the sample loading column to dissolve target components in the medicine column; the liquid chromatograph is used for chromatographic separation and detection analysis of the target components to elute and prepare sample solutions with different traditional Chinese medicine components; the liquid sample feeding mechanism comprises a plurality of enrichment column valve groups, and the centrifugal mechanism comprises a plurality of centrifugal concentration units respectively connected to the enrichment column valve groups; each enrichment column valve group is used to discharge the sample solution with different traditional Chinese medicine components to each corresponding centrifugal concentration unit, and each centrifugal concentration unit is used to concentrate the sample solution to remove solvents and obtain powder samples with different traditional Chinese medicine components in a centrifugal environment. The solid sample loader comprises: a pressing mechanism fixedly connected to the rack, wherein a pressing end of the pressing mechanism is located directly above the sample loading station; a rotating seat comprising a base and a rotating disc rotatably connected to the rotating seat, wherein a plurality of sample loading columns are circumferentially arranged on the rotating disc, and the sample loading columns are driven by the rotating disc to cyclically pass through the sample loading station and sequentially stop at the sample loading station; a rotating driving member arranged on the rack or the base, and having an output end connected to the center of the rotating disc; wherein when one of the sample loading columns stops at the sample loading station, the pressing end of the pressing mechanism seals into the sample loading column to compress the sample filler into the medicine column, and the mobile phase sequentially passes through the sample loading column located at the sample loading station. The sample loading column comprises: an elastic telescopic assembly arranged on the rotating disc in a vertical direction, wherein a telescopic end can be contracted downward under an external force and reset upward under its own elasticity when the external force is removed; a sample loading cup inserted into the elastic telescopic assembly, wherein a top end of the sample loading cup is open to allow the pressing end of the pressing mechanism to seal into the sample loading cup, and a bottom wall of the sample loading cup is provided with a liquid inlet; wherein the base is provided with a liquid inlet pipe directly below the sample loading station, the liquid inlet pipe is connected to the multi-element high-pressure chromatographic pump, the pressing end of the pressing mechanism is provided with a liquid outlet pipe, and the liquid outlet pipe is connected to the liquid chromatograph; when the pressing end of the pressing mechanism extends into the sample loading cup to press the medicine column, the elastic telescopic assembly is contracted to lower the sample loading cup and insert the liquid inlet pipe into the liquid inlet; when the pressing end of the pressing mechanism is lifted upward, the elastic telescopic assembly drives the sample loading cup to reset upward to separate the liquid inlet pipe from the liquid inlet. The liquid sample feeding mechanism further comprises:

2. The traditional Chinese medicine component full-automatic sample preparation system according to claim 1, characterized in that, an injection pump arranged on the rack, which is used to sequentially inject an eluent into each enrichment column valve group. ​ The enrichment column valve group comprises an enrichment column and a two-position six-way valve. The first port of the two-position six-way valve is connected with the multi-component high-pressure chromatographic pump, the second port is connected with the centrifugal concentration unit, the enrichment column is connected in series between the third port and the sixth port, the fourth port is used for connecting a solvent recovery device, and the fifth port is connected with a sample injection needle of the injection pump.

3. The traditional Chinese medicine component full-automatic sample preparation system according to claim 1, characterized in that, The elastic telescopic assembly comprises: Two guide sleeves are vertically fixed on the rotary disc and are spaced apart. Two guide rods are slidably arranged in the two guide sleeves. A sleeve is arranged between the two guide rods and is connected with the top ends of the two guide rods. Two elastic members are sleeved on the two guide rods.

4. The traditional Chinese medicine component full-automatic sample preparation system according to claim 1, characterized in that, The sample cup comprises: A cup body with open upper and lower ends. A lower flange is arranged at the lower end of the cup body. A sieve plate is arranged in the cup body and abuts against the top wall of the lower flange. A distribution disc is arranged in the cup body and abuts against the sieve plate.

5. The traditional Chinese medicine component full-automatic sample preparation system according to claim 1, characterized in that, The lower pressing mechanism comprises: A support is fixedly connected to the rack. A driving assembly is vertically fixed to the support and has a downwardly extending output end. A piston is arranged at the output end of the driving assembly and is vertically aligned with the sample loading station. The piston is arranged in the sample loading column in the sample loading station under the driving of the driving assembly.

6. The traditional Chinese medicine component full-automatic sample preparation system according to claim 5, characterized in that, The piston is provided with a liquid outlet pipe. The driving assembly comprises: Two slide rails are vertically fixed to the support and are located on the two sides of the piston. A slide seat is slidably connected to the two slide rails at the two ends and is provided with a screw sleeve at the middle part. A motor is fixedly connected to the support and has an output end connected with the screw rod. A hollow rod is fixedly connected to the bottom of the slide seat and is vertically aligned with the screw rod.

7. The traditional Chinese medicine component full-automatic sample preparation system according to claim 5, characterized in that, The piston is fixedly connected to the bottom end of the hollow rod. A disengagement ring is sleeved on the periphery of the piston. A limiting block is arranged above the disengagement ring on the support. When the piston is inserted into the sample cup, the disengagement ring abuts against the top wall of the sample cup. When the piston is withdrawn from the sample cup, the disengagement ring is lifted with the piston to abut against the limiting block, thereby abutting against the sample cup to separate the sample cup from the piston.

8. The traditional Chinese medicine component full-automatic sample preparation system according to any one of claims 1-7, characterized in that, The solvent system comprises three storage containers for storing water, methanol and 5% methanol respectively; wherein the mobile phase is a mixed liquid of water and methanol, and the multi-component high-pressure chromatographic pump can pump 5% methanol to the liquid sample feeding mechanism.

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