Preloaded sample injector for high performance liquid chromatograph, high performance liquid chromatograph and preloaded sample control method thereof

By designing a pre-loaded sample injector in the high-performance liquid chromatograph, the sample loading and injection process is calculated and completed in advance, which solves the problems of instrument idleness and low analysis efficiency caused by the sample loading process in the existing technology, and achieves a better Efficient sample analysis.

CN112485356BActive Publication Date: 2025-01-21SHANDONG WUKONG INSTR CO LTD
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Patent Information

Application Number
CN202011443117.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-12-08
Publication Date
2025-01-21
Estimated Expiration
2040-12-08

AI Technical Summary

Technical Problem

The instrument is idle during the sample loading process of existing high performance liquid chromatographs, resulting in low analysis efficiency.

Method used

A preloaded sample injector was designed to complete the injection process in advance by calculating the time required for sample loading. Loading of the next sample begins before analysis of the previous sample is completed, and the sample is injected directly when the next sample is loaded.

Benefits of technology

It achieves accurate calculation of the sample loading process time, completes the sample loading process in advance, reduces the sample loading time, and improves the overall analysis efficiency of the high-performance liquid chromatograph.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The present invention provides a pre-loaded sample injector for a high performance liquid chromatograph, a high performance liquid chromatograph and a pre-loaded sample control method thereof, and relates to the field of high performance liquid chromatograph control. The pre-loaded sample injector comprises: a sample tray unit, a sampling mechanism, an injection pump unit, an injection valve and a control unit; the control unit is used to calculate the time required for sample loading, and control the sample tray unit, the sampling mechanism, the injection pump unit, and the injection valve to complete the sample loading operation of the sample to be tested in advance. The high performance liquid chromatograph composed of the pre-loaded sample injector can accurately calculate the time required for the sample loading process, and use the time to complete the injection process in advance, start the loading of the next sample before the previous sample is analyzed, and directly inject the next sample when the loading is completed, so as to minimize the injection time and improve the analysis efficiency of the high performance liquid chromatograph.
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Description

Technical Field

[0001] The invention relates to the field of high performance liquid chromatograph control, and in particular to a preloaded sample injector for a high performance liquid chromatograph, a high performance liquid chromatograph and a preloaded sample control method thereof. Background Art

[0002] High performance liquid chromatography is an important branch of chromatography. It uses liquid as the mobile phase and a high-pressure infusion system to pump a single solvent with different polarities or a mixed solvent with different proportions, buffer solution and other mobile phases together with the sample to be tested into a chromatographic column with a stationary phase. After the components of the sample to be tested are separated in the chromatographic column, they enter the corresponding detector for detection, thereby achieving qualitative and quantitative analysis of the sample. High performance liquid chromatography is widely used in food safety, environment, pharmaceuticals, scientific research and other fields.

[0003] The automatic sampler is an important part of liquid chromatography. Its function is to automatically and accurately inject the set volume of sample into the high-pressure system for separation, analysis and detection. It has the advantages of high automation and quantitative accuracy. Since the sampler needs to load the sample before performing the injection, the robot arm needs to be moved to the specified sample bottle during the loading process, and the sample of the specified volume needs to be punctured or sucked. These all require a certain amount of loading time, which can be as short as tens of seconds or as long as one or two minutes. After the loading is completed, the injection valve can be switched to complete the entire injection action. Traditional samplers will only start the next injection after the analysis of the previous sample is completed. After the loading is completed, the valve is cut to complete the injection action. Only then does the sample analysis process begin. During the entire loading process, the instrument is idle and the analysis efficiency is low.

[0004] In summary, there is still room for further optimization of the injection and loading process of existing HPLC instruments. Summary of the invention

[0005] In view of this, an object of the present invention is to provide a preloading sample injector for a high performance liquid chromatograph, a high performance liquid chromatograph and a preloading sample control method thereof. Through the preloading sample injector, accurate calculation of the time required for the loading process is achieved, and the time is used to complete the injection process in advance. The loading of the next sample is started before the analysis of the previous sample is completed, and the next sample is directly injected when the loading is completed, thereby minimizing the injection time and greatly improving the overall analysis efficiency of the instrument.

[0006] In a first aspect, an embodiment of the present invention provides a preloaded sample injector for a high performance liquid chromatograph, the preloaded sample injector comprising: a sample tray unit, a sampling mechanism, a syringe pump unit, an injection valve and a control unit;

[0007] The sample tray unit is located at the bottom of the preload sample injector and is used to place sample bottles containing samples to be tested;

[0008] The sampling mechanism is located above the sample tray unit; the built-in sampling needle in the sampling mechanism is used to absorb the sample to be tested in the sample bottle;

[0009] The injection pump unit is connected to the sampling mechanism, and the sample to be tested drawn by the injection needle enters the infusion pump in the high performance liquid chromatograph through the injection valve;

[0010] The control unit is connected to the sampling mechanism, the injection pump unit and the injection valve respectively; the control unit is used to calculate the time required for sample loading and control the sample to be tested to perform the sample loading operation in advance.

[0011] In some embodiments, the above-mentioned preloaded sample injector further includes: an input power supply; the input power supply is used to supply power to the sample tray unit, the sampling mechanism, the injection pump unit, the injection valve and the control unit respectively.

[0012] In some embodiments, the above-mentioned injection pump unit consists of a injection pump or a metering pump.

[0013] In some embodiments, the sampling mechanism is a three-axis sampling mechanism.

[0014] In some embodiments, the sample tray unit comprises a plurality of sample bottles; the plurality of sample bottles are provided with different numbers; and the control unit is used to calculate the running time of the sampling mechanism to run to each sample bottle and the time required for the injection needle to draw the sample to be tested.

[0015] In some embodiments, the running time of the sampling mechanism running to each sample bottle is calculated by the following formula:

[0016]

[0017] Among them, T locate v is the running time from the sampling mechanism to the sample bottle; x is the movement speed of the x-axis motor; v y is the movement speed of the y-axis motor; v z is the movement speed of the z-axis motor; S x S is the distance on the x-axis when the sampling mechanism moves to the location of the sample bottle; y S is the distance on the y-axis when the sampling mechanism moves to the location of the sample bottle; z It is the distance on the z-axis when the sampling mechanism moves to the position of the sample bottle.

[0018] In some embodiments, the time required for the injection needle to absorb the sample to be tested is calculated by the following formula:

[0019]

[0020] Among them, T pumpS is the time required for the injection needle to absorb the sample to be tested; p v is the distance that the motor corresponding to the injection needle runs when sucking the sample to be tested; p is the running speed of the motor corresponding to the injection needle.

[0021] In a second aspect, an embodiment of the present invention provides a high performance liquid chromatograph, comprising: a preloaded sample injector, an infusion pump, a chromatographic column and a detector; wherein the preloaded sample injector is a preloaded sample injector for a high performance liquid chromatograph mentioned in any possible embodiment of the first aspect; the input end of the preloaded sample injector is connected to the infusion pump; the output end of the preloaded sample injector is connected to the inlet of the chromatographic column; the outlet of the chromatographic column is connected to the detector;

[0022] A pre-loaded sample injector is used to complete the loading of the sample to be tested before the detector in the continuous detection state completes the current detection according to a predetermined loading time;

[0023] An infusion pump is used to push the sample to be tested into the chromatographic column under the impetus of the pumped mobile phase;

[0024] A chromatographic column, used to separate the sample to be tested;

[0025] The detector is used to perform chromatographic detection on the sample to be tested output by the chromatographic column and determine the chromatogram of the sample to be tested.

[0026] In a third aspect, an embodiment of the present invention provides a method for controlling a preload sample of a high performance liquid chromatograph, the method being applied to the high performance liquid chromatograph mentioned in the second aspect, the method comprising:

[0027] Determine the pre-loading time by using the pre-loading sample injector in the high performance liquid chromatograph;

[0028] Determine whether the detector in the current high performance liquid chromatograph is in a detection state;

[0029] If the detector is in the detection state, before the first sample to be tested in the detector is detected, the second sample to be tested is injected through the pre-loading injector; wherein the first sample to be tested is detected before the second sample to be tested; and the time from the start of injection of the second sample to be tested to the completion of the detection of the first sample to be tested is not less than the pre-loading time;

[0030] After the second sample to be tested is injected, it enters the chromatographic column for separation under the action of the infusion pump, and the separated second sample to be tested is subjected to chromatographic detection by the detector.

[0031] In some embodiments, the above method comprises:

[0032] Determine the pre-loading time by using the pre-loading sample injector in the high performance liquid chromatograph;

[0033] Determine whether the detector in the current high performance liquid chromatograph is in a detection state;

[0034] If the detector is in a non-detection state, the sample to be tested in the current pre-loaded sample injector is introduced into the chromatographic column through the infusion pump for separation, and the separated sample to be tested is passed through the detector to complete chromatographic detection.

[0035] The embodiments of the present invention bring the following beneficial effects:

[0036] The present invention provides a pre-loaded sample injector for a high performance liquid chromatograph, a high performance liquid chromatograph and a pre-loaded sample control method thereof. The pre-loaded sample injector comprises: a sample tray unit, a sampling mechanism, a syringe pump unit, an injection valve and a control unit; the sample tray unit is located at the bottom of the pre-loaded sample injector and is used for placing a sample bottle containing a sample to be tested; the sampling mechanism is located above the sample tray unit; a built-in injection needle in the sampling mechanism is used for sucking the sample to be tested in the sample bottle; the syringe pump unit is connected to the sampling mechanism, and the sample to be tested sucked by the injection needle enters an infusion pump through the injection valve; the control unit is respectively connected to the sampling mechanism, the syringe pump unit and the injection valve; the control unit is used for calculating the time required for sample loading and controlling the sample to be tested to perform a sample loading operation in advance. In the process of pre-loading sample control, firstly, the pre-loading sample time is determined by the pre-loading sample injector in the high performance liquid chromatograph; then, it is determined whether the detector in the current high performance liquid chromatograph is in the detection state; if the detector is in the detection state, before the first sample to be tested in the detector is detected, the second sample to be tested is injected by the pre-loading sample injector; wherein, the first sample to be tested is detected before the second sample to be tested; the time from the start of injection of the second sample to the completion of the detection of the first sample to be tested is not less than the pre-loading sample time. Finally, after the injection of the second sample to be tested is completed, it enters the chromatographic column for separation under the action of the infusion pump, and the separated second sample to be tested is passed through the detector to complete the chromatographic detection. Under the action of the pre-loading sample injector, the high performance liquid chromatograph realizes the accurate calculation of the time required for the loading process, and uses this time to complete the injection process in advance, starts to execute the loading of the next sample before the analysis of the previous sample is completed, and directly injects the next sample when the loading is completed, so as to minimize the injection time and improve the analysis efficiency of the high performance liquid chromatograph.

[0037] Other features and advantages of the present invention will be set forth in the following description, or some features and advantages may be inferred or unambiguously determined from the description, or may be learned by implementing the above-mentioned technology of the present invention.

[0038] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, preferred embodiments are specifically listed below and described in detail with reference to the attached drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0040] Figure 1 A schematic structural diagram of a preloaded sample injector for a high performance liquid chromatograph provided in an embodiment of the present invention;

[0041] Figure 2 A schematic diagram of the structure of a high performance liquid chromatograph provided in an embodiment of the present invention;

[0042] Figure 3 A comparison diagram of the high performance liquid chromatograph provided in the embodiment of the present invention and the high performance liquid chromatograph in the prior art during sample injection;

[0043] Figure 4 A flow chart of a method for controlling sample preloading of a high performance liquid chromatograph is provided for an embodiment of the present invention;

[0044] Figure 5 A flow chart of another method for controlling sample preloading of a high performance liquid chromatograph provided in an embodiment of the present invention.

[0045] icon:

[0046] 10-preloaded sample injector; 11-sample tray unit; 12-sampling mechanism; 13-syringe pump unit; 14-injection valve; 15-control unit; 16-input power supply; 21-infusion pump; 22-chromatographic column; 23-detector. DETAILED DESCRIPTION

[0047] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0048] High performance liquid chromatography is an important branch of chromatography. It uses liquid as the mobile phase and a high-pressure infusion system to pump a single solvent with different polarities or a mixed solvent with different proportions, buffer solution and other mobile phases together with the sample to be tested into a chromatographic column with a stationary phase. After the components of the sample to be tested are separated in the chromatographic column, they enter the corresponding detector for detection, thereby achieving qualitative and quantitative analysis of the sample. High performance liquid chromatography is widely used in food safety, environment, pharmaceuticals, scientific research and other fields.

[0049] The automatic sampler is an important part of liquid chromatography. Its function is to automatically and accurately inject samples of a set volume into the high-pressure system for separation, analysis and detection. It has the advantages of high automation and precise quantitative analysis. Since the sampler needs to load the sample before performing the injection, the robot arm needs to be moved to the specified sample bottle during the loading process, and the sample of the specified volume needs to be punctured or absorbed. These require a certain amount of loading time, which can be as short as tens of seconds or as long as one or two minutes. Only after the loading is completed can the injection valve be switched to complete the entire injection action. Traditional samplers will only start loading the next needle after the analysis of the previous sample is completed. After the loading is completed, the valve is cut to complete the injection action, and the sample analysis process begins at this time. During the entire loading process, the instrument is in an idle state and the analysis efficiency is low.

[0050] The sample injector generally consists of three actions: sample loading, sample injection or sample loading, sample injection, and needle washing. The traditional sample injection and analysis methods are as follows:

[0051] In the process of injection and sample analysis of traditional HPLC, after all instruments are ready, the workstation sends an injection command to the injector, and the injector starts to load the sample; after the loading is completed, a signal is given to the HPLC, and the HPLC starts to let the pump run the gradient, starts to record the detector signal, and performs sample analysis. At the same time, the injector performs the needle washing action. After the needle washing is completed, the injector is in an idle waiting state. When the current sample analysis is completed, the HPLC continues to send injection commands and repeat the above process.

[0052] It can be seen that in the traditional injection scheme, when the sample is analyzed for the second time, the workstation needs to send the injection command first, and then wait for the sampler to load the sample before the sample analysis can be performed. That is, if the sample loading time is T1 and the sample analysis time is T2, the time for two consecutive sample analyses = (T1+T2)*2.

[0053] It can be seen that when analyzing two samples twice, the sample loading time T1 will be consumed twice, and during the sample loading process, the instrument is in an idle state, so one more time T1 will be consumed. In summary, there is still room for further optimization of the sample loading process of the existing high performance liquid chromatograph.

[0054] Based on this, an embodiment of the present invention provides a preloading sample injector for a high performance liquid chromatograph, a high performance liquid chromatograph and a preloading sample control method thereof. Through the preloading sample injector, the time required for the loading process is accurately calculated, and the time is used to complete the injection process in advance. The loading of the next sample is started before the analysis of the previous sample is completed, and the next sample is directly injected when the loading is completed, thereby minimizing the injection time and greatly improving the overall analysis efficiency of the instrument.

[0055] To facilitate understanding of this embodiment, a preloaded sample injector for a high performance liquid chromatograph disclosed in an embodiment of the present invention is first introduced in detail.

[0056] See also Figure 1 The illustrated example is a preloaded sample injector 10 for a high performance liquid chromatograph, comprising a sample tray unit 11 , a sampling mechanism 12 , a syringe pump unit 13 , an injection valve 14 and a control unit 15 .

[0057] The sample tray unit 11 is located at the bottom of the pre-loaded sample injector 10 and is used to place a sample bottle containing a sample to be tested;

[0058] The sampling mechanism 12 is located above the sample tray unit 11; the built-in injection needle in the sampling mechanism 12 is used to absorb the sample to be tested in the sample bottle;

[0059] The syringe pump unit 13 is connected to the sampling mechanism 12, and the sample to be tested drawn by the injection needle enters the infusion pump in the high performance liquid chromatograph through the injection valve 14;

[0060] The control unit 15 is connected to the sampling mechanism 12, the injection pump unit 13 and the injection valve 14 respectively; the control unit 15 is used to calculate the time required for sample loading and control the sample to be tested to perform the sample loading operation in advance.

[0061] The control unit 15 can accurately calculate the time when the injection needle reaches the sample bottle according to the position of the sample bottle, and then calculate the injection time in combination with the injection process of the injection needle. Therefore, the total time consumed by one injection can be calculated by the control unit 15, which is the sum of the time when the injection needle reaches the sample bottle and the time consumed by the injection process of the injection needle.

[0062] After calculating the time consumed by the injection process (denoted as T) through the pre-loading sample injector, the loading of the next sample is performed T time before the analysis of the previous sample is completed, that is, the loading of the next sample is performed simultaneously during the analysis process of the previous sample, saving the loading time of the next sample.

[0063] From the pre-loading sample injector for high performance liquid chromatograph mentioned in this embodiment, it can be known that the pre-loading sample injector can realize accurate calculation of the time required for the loading process, and use this time to complete the injection process in advance, start loading the next sample before the previous sample is completed, and directly inject the next sample when the loading is completed, thereby minimizing the injection time and greatly improving the overall analysis efficiency of the instrument.

[0064] In some embodiments, the preloaded sample injector 10 further includes: an input power supply 16; the input power supply 16 is used to supply power to the sample tray unit 11, the sampling mechanism 12, the injection pump unit 13, the injection valve 14 and the control unit 15 respectively.

[0065] The circuit involved in the input power supply 16 in the preloaded sample injector 10 can be independent of the power supply system of the high performance liquid chromatograph, and the working state of the preloaded sample injector 10 can still be guaranteed when the power supply of the high performance liquid chromatograph is abnormal; the input power supply 16 in the preloaded sample injector 10 can also be directly powered by the power supply system of the high performance liquid chromatograph, so as to ensure the circuit unification of the power supply system.

[0066] In some embodiments, the above-mentioned injection pump unit consists of a injection pump or a metering pump.

[0067] A metering pump is a hydraulic pump that keeps the volume of oil (i.e. displacement) constant when the pump shaft rotates one circle. The injection pump is composed of a stepper motor and its driver, a screw and a bracket, etc., with a reciprocating screw and nut. The nut is connected to the piston of the syringe, which contains the liquid medicine, to achieve high-precision, smooth and pulsation-free liquid transmission.

[0068] In some embodiments, the sampling mechanism is a three-axis sampling mechanism. The coordinate system corresponding to the three-axis sampling mechanism can be used to accurately determine the coordinates of the injection needle, sample bottle and other related equipment.

[0069] Specifically, the sample tray unit usually includes a plurality of sample bottles; the plurality of sample bottles are provided with different numbers; the control unit is used to calculate the running time of the sampling mechanism running to each sample bottle and the time required for the injection needle to absorb the sample to be tested. In some embodiments, the running time of the sampling mechanism running to each sample bottle is calculated by the following formula:

[0070]

[0071] Among them, T locate v is the running time from the sampling mechanism to the sample bottle; x is the movement speed of the x-axis motor; v y is the movement speed of the y-axis motor; v z is the movement speed of the z-axis motor; S x S is the distance on the x-axis when the sampling mechanism moves to the location of the sample bottle; y S is the distance on the y-axis when the sampling mechanism moves to the location of the sample bottle; z It is the distance on the z-axis when the sampling mechanism moves to the position of the sample bottle.

[0072] The time required for the injection needle to absorb the sample to be tested is calculated by the following formula:

[0073]

[0074] Among them, T pump S is the time required for the injection needle to absorb the sample to be tested; pv is the distance that the motor corresponding to the injection needle runs when sucking the sample to be tested; p is the running speed of the motor corresponding to the injection needle.

[0075] From this, the total time consumed for injection can be calculated as T = T locate +T pump After the total injection time T is calculated by the pre-loading sample injector, the loading of the next sample is performed T time before the analysis of the previous sample is completed, that is, the loading of the next sample is performed simultaneously during the analysis of the previous sample, saving the loading time of the next sample.

[0076] The present invention also provides a high performance liquid chromatograph. Figure 2 As shown, the high performance liquid chromatograph comprises: a preloaded sample injector 10, an infusion pump 21, a chromatographic column 22 and a detector 23; wherein the preloaded sample injector 10 is the preloaded sample injector for the high performance liquid chromatograph mentioned in the above embodiment; the input end of the preloaded sample injector 10 is connected to the infusion pump 21; the output end of the preloaded sample injector 10 is connected to the inlet of the chromatographic column 22; the outlet of the chromatographic column 22 is connected to the detector 23;

[0077] The pre-loaded sample injector 10 is used to complete the loading of the sample to be tested before the detector 23 in the continuous detection state completes the current detection according to the predetermined loading time;

[0078] The infusion pump 21 is used to push the sample to be tested into the chromatographic column 22 under the impetus of the pumped mobile phase;

[0079] Chromatographic column 22, used for separating the sample to be tested;

[0080] The detector 23 is used to perform chromatographic detection on the sample to be tested output by the chromatographic column 22 to determine the chromatogram of the sample to be tested.

[0081] The preloaded sample injector in this embodiment has the same technical features as the preloaded sample injector for high performance liquid chromatograph provided in the above embodiment, so it can solve the same technical problems and achieve the same technical effects. For the sake of brief description, the corresponding contents in the above embodiment can be referred to for the parts not mentioned in the embodiment.

[0082] Combine the following Figure 3A comparison chart is provided to compare the injection process in the prior art with the injection process of the preloaded sample injector. In the injection and sample analysis process of the traditional HPLC, after each instrument is ready, the workstation sends an injection command to the injector, and the injector starts to load the sample; after the loading is completed, a signal is given to the HPLC, and the HPLC starts to let the pump run the gradient, starts to record the detector signal, and performs sample analysis. At the same time, the injector performs the needle washing action. After the needle washing is completed, the injector is in an idle waiting state. When the analysis of this sample is completed, the HPLC continues to send injection commands and repeats the above process.

[0083] It can be seen that in the traditional injection scheme, when the sample is analyzed for the second time, the workstation needs to send the injection command first, and then wait for the sampler to load the sample before the sample analysis can be performed. That is, if the sample loading time is T1 and the sample analysis time is T2, the time for two consecutive sample analyses = (T1+T2)*2.

[0084] In this embodiment, the high performance liquid chromatograph can calculate the time T1 required for sample injection in advance according to the speed of each execution unit of the sample injection mechanism. The high performance liquid chromatograph can perform sample loading at time T1 before the first sample analysis is completed. In this way, during the first sample analysis, the second sample loading is performed at the same time, saving the sample loading time before the second sample analysis. That is, if the sample loading time is T1 and the sample analysis time is T2, the time for two consecutive sample analyses = T1 + T2*2.

[0085] It can be seen from the high performance liquid chromatograph mentioned in this embodiment that, under the action of the pre-loading sample injector, the high performance liquid chromatograph realizes the accurate calculation of the time required for the sample loading process, and uses the time to complete the sample injection process in advance, and starts the sample loading of the next sample before the analysis of the previous sample is completed, and directly injects the next sample when the loading is completed, which can reduce the sample loading time once and improve the analysis efficiency of the high performance liquid chromatograph.

[0086] The embodiment of the present invention also provides a method for controlling the preload sample of a high performance liquid chromatograph, which is applied to the high performance liquid chromatograph mentioned in the above embodiment, such as Figure 4 As shown, the method includes:

[0087] Step S401, determining the pre-loading time through the pre-loading sample injector in the high performance liquid chromatograph.

[0088] The pre-loading time can be calculated by the preset bottle number in the sample bottle and the injection volume. The specific calculation process can be seen in the calculation method of the total injection consumption time mentioned in the above embodiment.

[0089] Step S402, determining whether the detector in the current high performance liquid chromatograph is in a detection state.

[0090] The purpose of this step is to ensure that the detector in the current HPLC instrument has samples under detection. If the detector is not in the detection state, it means that there are no samples under detection, and the pre-loading process cannot be performed.

[0091] Step S403, if the detector is in the detection state, before the first sample to be tested in the detector is detected, the second sample to be tested is injected through the pre-loading injector; wherein, the first sample to be tested is detected before the second sample to be tested; and the time from the start of injection of the second sample to be tested to the completion of detection of the first sample to be tested is not less than the pre-loading time.

[0092] The pre-loading time in this step is the total injection time mentioned in the above embodiment. In this way, the second sample to be tested is loaded while the first sample to be tested is still being analyzed, saving the loading time of the second sample to be tested during analysis.

[0093] Step S404, after the second sample to be tested is injected, it enters the chromatographic column for separation under the action of the infusion pump, and the separated second sample to be tested is subjected to chromatographic detection by the detector.

[0094] The high performance liquid chromatograph in this embodiment has the same technical features as the high performance liquid chromatograph provided in the above embodiment, so it can also solve the same technical problems and achieve the same technical effects. For the sake of brief description, the parts not mentioned in the embodiment section can be referred to the corresponding contents in the above embodiment.

[0095] The detector in the above method embodiment is in a detection state, indicating that the first sample to be tested is present in the detector, so that the second sample to be tested can be loaded while the first sample to be tested is still being analyzed. In some embodiments, the detector of the high performance liquid chromatograph is in a non-detection state, indicating that the detector does not contain the first sample to be tested. In this case, the pre-loading control method is as follows: Figure 5 As shown, the following steps are included:

[0096] Step S501, determining the pre-loading time through the pre-loading sample injector in the high performance liquid chromatograph.

[0097] Step S502, determining whether the detector in the current high performance liquid chromatograph is in a detection state.

[0098] Step S503, if the detector is not in the detection state, after the second sample to be tested is injected, it enters the chromatographic column for separation under the action of the infusion pump, and the separated second sample to be tested is subjected to chromatographic detection by the detector.

[0099] Since the first sample to be tested is not included, the pre-sample process is not performed in this step, and the second sample to be tested is directly separated by the chromatographic column, and then the chromatographic detection is completed by the detector.

[0100] From the pre-loading sample control method of the high performance liquid chromatograph mentioned in this embodiment, it can be seen that the high performance liquid chromatograph in this method, under the action of the pre-loading sample injector, realizes the accurate calculation of the time required for the loading process, and uses this time to complete the injection process in advance, starts the loading of the next sample before the analysis of the previous sample is completed, and directly injects the next sample when the loading is completed, thereby minimizing the injection time and improving the analysis efficiency of the high performance liquid chromatograph.

[0101] In the several embodiments provided in the present application, it should be understood that the disclosed systems, devices and methods can be implemented in other ways. The device embodiments described above are merely schematic. For example, the division of the units is only a logical function division. There may be other division methods in actual implementation. For example, multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. Another point is that the mutual coupling or direct coupling or communication connection shown or discussed can be through some communication interfaces, indirect coupling or communication connection of devices or units, which can be electrical, mechanical or other forms.

[0102] The units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in one place or distributed on multiple network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the solution of this embodiment.

[0103] In addition, each functional unit in each embodiment of the present invention may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit.

[0104] If the functions are implemented in the form of software functional units and sold or used as independent products, they can be stored in a non-volatile computer-readable storage medium that is executable by a processor. Based on this understanding, the technical solution of the present invention can essentially or in other words, the part that contributes to the prior art or the part of the technical solution can be embodied in the form of a software product. The computer software product is stored in a storage medium and includes several instructions for enabling a computer device (which can be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the methods described in each embodiment of the present invention. The aforementioned storage medium includes: various media that can store program codes, such as a USB flash drive, a mobile hard disk, a read-only memory (ROM), a random access memory (RAM), a magnetic disk or an optical disk.

[0105] Finally, it should be noted that the above-described embodiments are only specific implementations of the present invention, which are used to illustrate the technical solutions of the present invention, rather than to limit them. The protection scope of the present invention is not limited thereto. Although the present invention is described in detail with reference to the above-described embodiments, ordinary technicians in the field should understand that any technician familiar with the technical field can still modify the technical solutions recorded in the above-described embodiments within the technical scope disclosed by the present invention, or can easily think of changes, or make equivalent replacements for some of the technical features therein; and these modifications, changes or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention, and should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. A method for controlling a preloaded sample of a high performance liquid chromatograph, characterized in that: The method is applied to a high performance liquid chromatograph, which comprises: a pre-loaded sample injector, an infusion pump, a chromatographic column and a detector; wherein the input end of the pre-loaded sample injector is connected to the infusion pump; the output end of the pre-loaded sample injector is connected to the inlet of the chromatographic column; the outlet of the chromatographic column is connected to the detector; the pre-loaded sample injector is used to complete the loading of the sample to be tested before the detector in a continuous detection state completes the current detection according to a predetermined loading time; the infusion pump is used to push the sample to be tested into the chromatographic column under the impetus of the pumped mobile phase; the chromatographic column is used to separate the sample to be tested; the detector is used to perform chromatographic detection on the sample to be tested output by the chromatographic column to determine the chromatogram of the sample to be tested; The preloaded sample injector comprises: a sample tray unit, a sampling mechanism, a syringe pump unit, an injection valve and a control unit; the sample tray unit is located at the bottom of the preloaded sample injector and is used to place a sample bottle containing a sample to be tested; the sampling mechanism is located above the sample tray unit; the built-in injection needle in the sampling mechanism is used to absorb the sample to be tested in the sample bottle; the syringe pump unit is connected to the sampling mechanism, and the sample to be tested absorbed by the injection needle enters the infusion pump in the high performance liquid chromatograph through the injection valve; the control unit is respectively connected to the sampling mechanism, the syringe pump unit and the injection valve; the control unit is used to calculate the time required for loading the sample and control the sample to be tested to be loaded in advance; the syringe pump unit is composed of a syringe pump or a metering pump; the sampling mechanism is a three-axis sampling mechanism; the control unit is also used to calculate the running time of the sampling mechanism to each sample bottle and the time required for the injection needle to absorb the sample to be tested; the running time of the sampling mechanism to each sample bottle is calculated by the following formula: Among them, T locate v is the running time of the sampling mechanism running to the sample bottle; x is the movement speed of the x-axis motor; v y is the movement speed of the y-axis motor; v z is the movement speed of the z-axis motor; S x S is the distance on the x-axis when the sampling mechanism moves to the position of the sample bottle; y S is the distance on the y-axis when the sampling mechanism moves to the position where the sample bottle is located; z is the distance on the z-axis when the sampling mechanism moves to the position where the sample bottle is located; The time required for the injection needle to absorb the sample to be tested is calculated by the following formula: Among them, T pump S is the time required for the injection needle to absorb the sample to be tested; p v is the distance that the motor corresponding to the injection needle runs when sucking the sample to be tested; p is the running speed of the motor corresponding to the injection needle; The preloaded sample injector further comprises: an input power supply; the input power supply is used to supply power to the sample tray unit, the sampling mechanism, the injection pump unit, the injection valve and the control unit respectively; The sample tray unit comprises a plurality of sample bottles; the plurality of sample bottles are provided with different numbers; The method comprises: Determining the pre-loading time by means of a pre-loading sample injector in the high performance liquid chromatograph; Determining whether the detector in the high performance liquid chromatograph is currently in a detection state; If the detector is in a detection state, before the first sample to be tested in the detector is detected, the second sample to be tested is injected by the pre-loading injector; wherein the first sample to be tested is detected before the second sample to be tested; and the time from the start of injection of the second sample to be tested to the completion of the detection of the first sample to be tested is not less than the pre-loading time; After the injection of the second sample is completed, it enters the chromatographic column for separation under the action of the infusion pump, and the separated second sample is subjected to chromatographic detection by the detector.

2. The method for controlling the preload sample of a high performance liquid chromatograph according to claim 1, characterized in that: The method comprises: Determining the pre-loading time by means of a pre-loading sample injector in the high performance liquid chromatograph; Determining whether the detector in the high performance liquid chromatograph is currently in a detection state; If the detector is in a non-detection state, the sample to be tested in the pre-loaded sample injector is introduced into the chromatographic column through the infusion pump for separation, and the separated sample to be tested is passed through the detector to complete chromatographic detection.

Citation Information

Patent Citations

  • Preloading sample injector for high performance liquid chromatograph and high performance liquid chromatograph

    CN214374533U