CN212207226U - A static sample injection and fraction collection device used in conjunction with a liquid chromatograph - Google Patents

Abstract

The utility model relates to a with supporting static advance a kind of use of liquid chromatograph and flow fraction collection device, including programmable controller, autoinjector and flow fraction collector, the autoinjector includes syringe pump, first electronic multichannel diverter valve and electronic six-channel sampling valve, and the flow fraction collector includes programmable controller and the electronic multichannel diverter valve of second, and programmable controller advances a kind and sets for module and DA conversion module including advancing a kind, advances a kind and sets for the module and is connected with DA conversion module. The utility model discloses an automatic sample injector can be fixed arrange the sample container bottom in with the mouth of pipe of advancing the appearance, avoids the common sample of automatic sample injector sold in the market at present to remain, sample loss and mechanical failure scheduling problem, realizes the collection of flow fraction through combining to adopt electronic multichannel diverter valve, makes liquid chromatogram autoinjection and flow fraction collection function integrate into one, and the instrument simple structure, the operation of being convenient for, occupation space are little, can use with the liquid chromatograph of various models is supporting.

Description

A static sample injection and fraction collection device used in conjunction with a liquid chromatograph

technical field

The utility model relates to the field of separation and purification of chemical and biological samples, in particular to a static sample injection and flow fraction collection device matched with a liquid chromatograph.

Background technique

Liquid chromatography is based on the difference in the affinity of the components in the mixture for the two phases to achieve the separation of samples. In recent years, high-efficiency (also known as high-pressure) liquid chromatography with finer stationary phase support and higher mobile phase pressure has been widely used in scientific research and production units, and has become an effective means of separation and purification of chemical and biological samples.

A complete set of high performance liquid chromatography equipment is generally composed of high pressure infusion pump, chromatography column, gradient mixer, column oven, online degasser, detector (ultraviolet/differential/evaporative light scattering/fluorescence, etc.), automatic or manual It consists of a sampler, a fraction collector and corresponding analysis control software. Among them, the automatic sampler and fraction collector can reduce the repetitive operation and long-term duty of experimental and production personnel, improve work efficiency and reduce labor costs.

At present, there are many brands of high performance liquid chromatographs on the market, all of which have certain user groups. However, the existing technical solutions have the following defects:

There are many types of software, and the operation is inconvenient. Among them, the high-pressure infusion pump, automatic sampler, detector, and fraction collector have their own control/analysis software;

Instruments of various brands are produced by different companies and have poor compatibility with each other;

At present, the commercially available autosamplers all use mechanical moving arms, which use X/Y/Z displacement for sample injection. They have strict restrictions on the position of test tubes/vials. If the position is deviated, normal injection cannot be performed. .

At present, commercially available autosamplers usually use metal injection needles, which cannot be inserted into the bottom of the sample vial to absorb the sample, and the sample may be lost during repeated movement.

Fraction collectors mostly use mechanical moving arms, and use X/Y displacement to collect fractions, which has strict restrictions on the position of test tubes/sample bottles. If the position is deviated, fractions cannot be collected normally.

Due to the independent design of the autosampler and the fraction collector, many moving components are used, the instrument occupies a large space, the instrument consumes a lot of power, and the reliability of long-term operation is poor.

Utility model content

In view of the deficiencies of the prior art, the purpose of this utility model is to provide a static sample injection and fraction collection device that is used in conjunction with a liquid chromatograph. It can be realized by sampling injection valve, electric multi-channel distribution valve and corresponding control software; it can realize selective automatic sampling of samples in different sample containers according to needs, and according to needs, the separated fractions can be selectively Collection; since there are no moving components in the traditional design in the instrument, the reliability of long-term operation can be improved, and there is no limit to the amount of samples to be separated, which can realize the separation of a large number of samples for a long time, unattended.

The above-mentioned purpose of the present utility model is achieved through the following technical solutions:

A static sample injection and fraction collection device used in conjunction with a liquid chromatograph, comprising a programmable controller, an automatic sampler and a fraction collector, the automatic sampler comprising a syringe pump and a first electric multi-channel switching valve and the electric six-channel sampling valve; the outlet of the first electric multi-channel switching valve is connected to the electric six-channel sampling valve through the main line, and the other five interfaces of the electric six-channel sampling valve are respectively connected to the syringe pump and the one that occupies two interfaces. The quantitative loop, the mobile phase of the liquid chromatography pump and the inlet of the chromatographic column are connected; the fraction collector is composed of the programmable controller and the second electric multi-channel switching valve, and the main line of the second electric multi-channel switching valve is connected with the detection The mobile phase of the second electric multi-channel switching valve is connected to the mobile phase of the second electric multi-channel switching valve, and the branch lines of the second electric multi-channel switching valve are respectively connected to the fraction collection container and the waste liquid collection container; the programmable controller includes a sample injection setting module and a D/A conversion module. The fixed module is connected with the D/A conversion module, and the D/A conversion module is respectively connected with the first electric multi-channel switching valve, the electric six-channel sampling valve and the syringe pump in the automatic sampler, and the second in the fraction collector. Electric multi-channel switching valve connection.

By adopting the above technical scheme, the static sample injection and fraction collection device of the present invention used together with the liquid chromatograph controls the channel switching of the first electric multi-channel switching valve through the sample injection setting module and the D/A conversion module, Furthermore, the samples in different sample containers can be selectively injected automatically without moving the mechanical arm according to the needs.

In a preferred example of the present invention, it can be further configured to further include a detector disposed outside for detecting the components of the fraction, the inlet of the detector is connected with the outlet of the chromatographic column through a pipeline, and the outlet of the detector is connected to the second The inlets of the electric multi-channel switching valves are connected by pipelines.

By adopting the above technical scheme, the component detection of the fractions separated by the chromatographic column can be carried out.

In a preferred example of the present invention, the programmable controller further includes an A/D conversion module, an information identification module and an information storage module, and the information identification module is respectively connected with the A/D conversion module, the information storage module and the D The /A conversion module is connected, and the detector is electrically connected with the A/D conversion module to transmit the detected analog signal of the flow component to the programmable controller.

By adopting the above technical solution, the detector, the A/D conversion module, the information identification module, the information storage module and the D/A conversion module can be used to control the switching of the channels of the second electric multi-channel switching valve, so as to separate out the The different components of the sample are collected separately, and the different components in the fraction can be accurately collected separately, and the separation effect of various components in the sample is better.

In a preferred example, the present invention can be further configured to further include a touch display screen, and the touch display screen is connected to the programmable controller.

In a preferred example of the present invention, it can be further configured that the programmable controller further includes a wireless sending module and a wireless receiving module.

By adopting the above technical scheme, the remote control of the system and the automatic upgrade of the software can be realized, and each control and analysis function can be integrated by using a single control software to facilitate the control of each component.

In a preferred example of the present invention, it can be further configured that the sample introduction system further includes a sample introduction line arrangement seat, and the sample introduction line arrangement seat is arranged above the first electric multi-channel switching valve.

By adopting the above technical solution, the pipelines connected to the first electric multi-channel switching valve are arranged to be neat and orderly.

In a preferred example of the present invention, it can be further configured that the flow-division collection system further comprises a flow-distribution pipeline arrangement seat, and the flow-disconnection pipeline arrangement seat is arranged above the second electric multi-channel switching valve.

In a preferred example of the present invention, it can be further configured that the programmable controller is further provided with a communication interface.

By adopting the above technical solutions, the system can be connected with external PC devices.

In a preferred example of the present invention, it can be further configured that the touch screen and the programmable controller are integrated and set together.

By adopting the above technical solutions, the size of the system is reduced and its appearance effect is enhanced.

Description of drawings

1 is a schematic diagram of a static sample injection and fraction collection device used in conjunction with a liquid chromatograph according to an embodiment of the present invention.

FIG. 2 is a schematic structural diagram of the integrated sample processor in FIG. 1 from one perspective.

FIG. 3 is a schematic structural diagram of the integrated sample processor in FIG. 1 from another perspective.

FIG. 4 is a schematic diagram of the internal structure of the integrated sample processor in FIG. 2 .

FIG. 5 is an internal system diagram of the programmable controller of the integrated sample processor of FIG. 1 .

In the figure, 1. Touch screen; 2. Sampling pipeline arrangement seat; 3. Electric six-way injection valve; 4. The first electric multi-channel switching valve; 5. Electric three-way valve; 6. Syringe pump; 7 , injection syringe; 8, flow branch line arrangement seat; 9, second electric multi-channel switching valve; 10, electrical signal input terminal; 11, switch; 12, RS232 communication interface; 13, cleaning waste liquid collection bottle; 14, Quantitative loop; 15, chromatographic column; 16, sample container; 17, detector; 18, liquid chromatography pump; 19, eluent bottle; 20, fraction collection container; 21, waste liquid collection bottle; 22, switching power supply ; 23, the main control circuit board; 24, the stepper motor driver; 25, the screw; 26, the stepper motor; 27, the casing.

Detailed ways

The present utility model will be further described in detail below in conjunction with the accompanying drawings.

1 to 4, the present utility model discloses a static sample injection and fraction collection device used in conjunction with a liquid chromatograph, including an integrated sample processor, a chromatographic column 15, a liquid chromatographic pump 18, an elution A liquid bottle 19 and a detector 17 for detecting the fraction components. The integrated sample processor includes a programmable controller, sample introduction system, and fraction collection system. The sampling system includes a sample container 16, a syringe pump 6, an electric three-way valve 5, an electric six-way sampling valve 3, a first electric multi-channel switching valve 4, and a sampling needle 7 connected to the syringe pump 6. Through the sampling system The sample in the sample container 16 is aspirated. The capacity of the sample injection needle 7 can be selected by the user as required and set in the software of the touch screen 1 , and its function is to draw the sample in the sample container 16 . The function of the electric three-way valve 5 is to select sample injection or to exclude the waste liquid in the sample injection needle 7 according to the needs. The electric six-way sampling valve 3 is also provided with a quantitative loop 14 for sucking and accommodating samples, and the electric six-way sampling valve 3 can realize automatic cleaning of the pipeline and the sampling needle. The syringe pump 6 is arranged in the casing 27 and includes a stepping motor 26 , a screw rod 25 , a switching power supply 22 , a main control circuit board 23 , and a stepping motor driver 24 . The fraction collection system includes a fraction collection container 20 and a waste liquid container, and the waste liquid container includes a cleaning waste liquid collection bottle 13 and a fraction waste liquid collection bottle 21 . The first electric multi-channel switching valve 4 includes 10 channels, and the sample container 16 is provided with 10 channels, and each sample container 16 is marked with a label, and each sample container 16 passes through each channel port of the first electric multi-channel switching valve 4 respectively. Each branch line is connected. The outlet of the first electric multi-channel switching valve 4 is connected to the inlet of the external chromatographic column 15 through the main line, and the syringe pump 6 is arranged on the pipeline of the main line. In other embodiments, when the device is only used for repeated injection of a single sample, as a simplified device, the first motorized multi-channel switching valve in the autosampler portion can be eliminated, and the sample connected to the motorized six-channel switching valve can be used. The injection line directly sucks the sample solution to be separated.

Referring to FIGS. 1 to 4 , the fraction collection system further includes a second electric multi-channel switching valve 9 , and the second electric multi-channel switching valve 9 includes 10 channels. There are 9 fraction collection containers 20, and each fraction collection container 20 is labelled. The inlet of the second electric multi-channel switching valve 9 is connected to the outlet of the chromatographic column 15 through the main line. The second electric multi-channel switching valve Each channel of 9 is connected to the waste liquid container and each fraction collection container 20 through each branch line. The sampling system also includes a sampling line arrangement seat 2, which is arranged above the first electric multi-channel switching valve 4, and the sampling line arrangement seat 2 is marked with a pipeline number, and the sampling line arrangement seat 2 It is used to organize the branch pipelines connected to the first electric multi-channel switching valve 4 to make them neat and orderly. The fractional collection system also includes a fractionation pipeline arrangement seat 8, which is arranged above the second electric multi-channel switching valve 9, and the fractionation pipeline arrangement seat 8 is marked with a pipeline number. 8 is used to organize the branch pipelines connected to the second electric multi-channel switching valve 9 to make them neat and orderly. In addition, the back panel of the integrated sample processor is also provided with a power socket and a switch, on which a power switch and a fuse are integrated; the back panel is also provided with an electrical signal input terminal 10 connected to the detector 17, and an electrical signal input terminal 10 connected to the PC RS232 communication interface 12 , power socket and switch 11 .

When the static sample injection and fraction collection device of the present invention is used in conjunction with a liquid chromatograph, the inlet of the first electric multi-channel switching valve 4 is connected to each branch pipeline, and the sample injection pipeline tidying seat 2 is connected to the sample. The container 16 is connected; the outlet of the first electric multi-channel switching valve 4 is connected with the inlet of the electric six-way sampling valve 3 with the main line; Connect the 6 ports of the electric six-way injection valve 3 to the inlet of the electric three-way valve 5 with the pipeline; connect the outlet of the electric three-way valve 5 to the cleaning waste liquid collection bottle 13 with the pipeline; Installed on the syringe pump 6, the inlet of the injection needle 7 is connected with the bottom port of the electric three-way valve 5; the 2 ports of the electric six-way injection valve 3 are connected with the external liquid chromatography pump 18 with the pipeline; The 3 ports of the six-way injection valve 3 are connected to the external chromatographic column 15 with a pipeline; the outlet below the external chromatographic column 15 is connected to the inlet of the external detector 17 with a pipeline; the outlet of the external detector 17 is connected with a pipeline Connect with the inlet of the second electric multi-channel switching valve 9; connect the signal output of the external detector 17 with the electrical signal input terminal 10; connect the outlet of the second electric multi-channel switching valve 9 with a pipeline through the flow branch line The finishing seat 8 is connected to the fraction collection container 20, and the last outlet of the second electric multi-channel switching valve 9 is connected to a large fraction waste liquid collection bottle 21 with a pipeline. When in use, the sample is injected through the injection needle 7 on the syringe pump 6. After the injection is completed, the eluent in the eluent bottle 19 is injected into the chromatographic column through the electric six-way injection valve 3 through the liquid chromatography pump 18. Inside, using the principle that the adsorption force of the chromatographic column to different sample components is different, the sample components are separated, and then the fractions enter the detector 17 for component detection, and the detection information is fed back to the controller.

Referring to FIG. 5 , the static sample injection and fraction collection device used together with the liquid chromatograph of the present invention further includes a touch display screen 1, and the touch display screen 1 has a built-in Android system or a windows operating system, and the touch screen The system control software is installed on display 1. The control software can control the sampling system, the first electric multi-channel switching valve 4, the electric six-way sampling valve 3, and the second electric multi-channel switching valve 9, and can also use the electrical signal input terminal 10 to transmit the signal from an external detector 17. The level signal draws the absorbance curve. It can control the injection volume, injection speed, injection times, injection interval, etc. of the injection system. By matching the injection time interval with the separation time of the chromatographic column 15, uninterrupted and repeated automatic injection can be realized. Unattended, long-term sample separation can be achieved. The touch display screen 1 is connected with the programmable controller, and the touch screen display 1 and the programmable controller are integrated and set together. The programmable controller also includes an A/D conversion module, an information identification module and an information storage module. The A/D conversion module is used for receiving the analog signal fed back by the detector 17 and converting the analog signal into a digital signal. The information identification module is respectively connected with the A/D conversion module, the information storage module and the D/A conversion module. The D/A conversion module is respectively electrically connected with the first electric multi-channel switching valve 4 , the second electric multi-channel switching valve 9 and the syringe pump 6 to realize control. The detector 17 is electrically connected to the A/D conversion module to transmit the detected analog signal of the flow component to the programmable controller. The information identification module is connected with the A/D conversion module for receiving the converted digital signal and identifying whether the same signal has been stored in the information storage module. If there is, query the storage information of the stored signal through the information storage module, for example, which fraction collection container 20 is stored in, and send a digital signal to the D/A conversion module, and the D/A conversion module converts the digital signal into The analog signal is transmitted to the second electric multi-channel switching valve 9, and the second electric multi-channel switching valve 9 is controlled to collect the fraction into the fraction collection container 20 of the same fraction that has been collected before; The fractional component signal is transmitted to the information storage module to store and record, and at the same time, a digital signal is sent to the D/A conversion module to control the second electric multi-channel switching valve 9 to collect the fraction into a new fraction collection container 20 . The programmable controller also includes an injection setting module, which is used to set single or multiple injection types, injection sequences, repeated injection times, injection time intervals and injection volumes as required, and Fraction collection containers 20 may be designated for each sample. By reasonably setting the injection time interval, the separation capacity of the chromatographic column 15 can be fully and effectively utilized, the separation efficiency can be improved, and the effective separation of the samples can be realized. The sample injection setting module is connected with the D/A conversion module, so as to control the on-off of each channel of the first electric multi-channel switching valve 4 and the second electric multi-channel switching valve 9, thereby realizing the set content. The programmable controller also includes a wireless sending module and a wireless receiving module, which can realize remote control and software upgrade of the system, and can monitor the operation of the equipment in real time.

The A/D conversion circuit can collect data from the signal of the detector 17, and display the separation curve of the fractional components on the display screen. The collection of fractional fractions can be controlled by threshold method, timing method and peak shape method. The threshold method is to set a threshold on the system software of the touch screen, and the peaks higher than the threshold belong to the samples to be collected, which can be collected in sequence by controlling the second electric multi-channel switching valve 9 . The principle of the timing method is based on the high repeatability of the separation of the same sample by the chromatographic column 15. After determining the peak appearance time of each peak shape, the software can set the sample within a specific time period after each injection. collection, and can designate the collection container 20 for the collection. The peak shape method is determined according to the characteristics of the peak. It is collected according to the inflection point of the peak shape. Compared with the threshold method, the sample collection is more efficient, and two adjacent peaks can also be collected separately. This is something the threshold method cannot do.

The static sample injection and fraction collection device of the utility model used in conjunction with a liquid chromatograph, when in use, first set parameters in the system software program of the touch display screen 1, including setting the type of the sample to be injected, the type of the sample to be injected Sequence, injection speed and injection volume, set injection interval time, set data collection time, set sampling repetition times; set sample collection method, timing method, threshold method or peak shape splitting method. After the setting is completed, click "Start" to perform sample injection, separation and sample fraction collection.

The implementation principle of this embodiment is as follows: the static sample injection and fraction collection device of the present invention used in conjunction with a liquid chromatograph controls the flow of the first electric multi-channel switching valve 4 through a sample injection setting module and a D/A conversion module. Channel switching, and then optional automatic sampling of samples in different sample containers 16 can be selected according to needs; moreover, through the detector 17, the A/D conversion module, the information identification module, the information storage module and the D/A conversion module, control The switching of the channels of the second electric multi-channel switching valve 9 can automatically separate and collect different components separated in the fraction, which can accurately separate and collect the different components in the fraction. In addition, the static sample injection and fraction collection device of the utility model used together with the liquid chromatograph can realize automatic repeated sample injection of multiple samples, realize fully automatic sample separation operation, greatly reduce labor costs and improve production efficiency. , and ensure the consistency of sample separation effect. In addition, the instrument can realize remote equipment monitoring, remote data collection and online upgrade of the system. Moreover, the sample introduction system, fraction collection system, detector 17, touch display screen 1 and wireless transceiver module are integrated into one, each component has better adaptability, and can share a set of control system, a set of power supply, a set of Control software, one chassis, so the overall cost can be greatly reduced, and the after-sales and equipment maintenance are also greatly simplified, which is more convenient for users to operate and use, and has a higher cost performance.

The embodiments of this specific embodiment are all preferred embodiments of the present invention, and are not intended to limit the protection scope of the present invention, therefore: all equivalent changes made according to the structure, shape and principle of the present invention are It should be covered within the protection scope of the present invention.

Claims (9)

1. The utility model provides a with supporting static advance a kind of use of liquid chromatograph and flow fraction collection device which characterized in that: the automatic sampler comprises a programmable controller, an automatic sampler and a flow collector, wherein the automatic sampler comprises an injection pump (6), a first electric multi-channel switching valve (4) and an electric six-channel sampling valve (3); an outlet of the first electric multi-channel switching valve (4) is connected with an electric six-channel sample injection valve (3) through a main pipeline, and the other five interfaces of the electric six-channel sample injection valve (3) are respectively connected with an injection pump (6), a quantitative ring (14) occupying 2 interfaces, a mobile phase of a liquid chromatographic pump and an inlet of a chromatographic column (15); the flow fraction collector comprises the programmable controller and a second electric multi-channel switching valve (9), a main pipeline of the second electric multi-channel switching valve (9) is connected with a mobile phase of the detector (17), and branch pipelines of the second electric multi-channel switching valve (9) are respectively connected with a flow fraction collecting container (20) and a waste liquid collecting container; the programmable controller comprises a sample setting module and a D/A conversion module, the sample setting module is connected with the D/A conversion module, and the D/A conversion module is respectively connected with a first electric multi-channel switching valve (4), an electric six-channel sample valve (3) and an injection pump (6) in the automatic sample injector and a second electric multi-channel switching valve (9) in the flow collector.

2. The static sample introduction and fraction collection device of claim 1 for use with a liquid chromatograph, wherein: the device also comprises a detector (17) which is arranged outside and used for detecting the components of the flow, wherein the inlet of the detector (17) is connected with the outlet of the chromatographic column (15) through a pipeline, and the outlet of the detector (17) is connected with the inlet of the second electric multi-channel switching valve (9) through a pipeline.

3. The static sample introduction and fraction collection device for use with a liquid chromatograph of claim 1 or 2, wherein: the programmable controller also comprises an A/D conversion module, an information identification module and an information storage module, wherein the information identification module is respectively connected with the A/D conversion module, the information storage module and the D/A conversion module, and the detector (17) is electrically connected with the A/D conversion module so as to transmit the detected stream components to the programmable controller as analog signals.

4. The static sample introduction and fraction collection device for use with a liquid chromatograph of claim 1 or 2, wherein: the touch control display screen (1) is further included, and the touch control display screen (1) is connected with the programmable controller.

5. The static sample introduction and fraction collection device for use with a liquid chromatograph of claim 1 or 2, wherein: the programmable controller also comprises a wireless transmitting module and a wireless receiving module.

6. The static sample introduction and fraction collection device for use with a liquid chromatograph of claim 1 or 2, wherein: the automatic sample injector further comprises a sample injection pipeline arranging seat (2), and the sample injection pipeline arranging seat (2) is arranged above the first electric multi-channel switching valve (4).

7. The static sample introduction and fraction collection apparatus of claim 6 for use with a liquid chromatograph, wherein: the flow collector further comprises a flow distribution pipeline arranging seat (8), and the flow distribution pipeline arranging seat (8) is arranged above the second electric multi-channel switching valve (9).

8. The static sample introduction and fraction collection device for use with a liquid chromatograph of claim 1 or 2, wherein: and the programmable controller is also provided with a communication interface.

9. The static sample introduction and fraction collection apparatus of claim 4 for use with a liquid chromatograph, wherein: the touch display screen (1) and the programmable controller are integrated together.

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