A derivatization instrument for high performance liquid chromatography

Abstract

This invention discloses a high-performance liquid chromatography (HPLC) derivatization instrument, comprising: a reaction module including at least one derivatization reaction chamber and an injection port connected thereto; a temperature control system integrated around the reaction module; a mobile phase control unit including a gradient pump and an online mixer; an automation control module including a PLC controller and a robotic arm; a wireless communication module; and an anomaly handling module including an ultrasonic cleaning device. The HPLC derivatization instrument provided by this invention significantly improves the efficiency and reproducibility of the derivatization process through automated injection and reaction control. The high integration of the HPLC derivatization instrument with an HPLC system makes the analysis process smoother and reduces analysis time. The precise control of derivatization conditions ensures the consistency and accuracy of the derivatization reaction, improving the reliability of the analytical results.

Description

Technical Field

[0001] This utility model relates to the field of high performance liquid chromatography (HPLC) technology, and in particular to a derivatizer for HPLC. Background Technology

[0002] High-performance liquid chromatography (HPLC) is an analytical technique for separating and analyzing components in complex mixtures. It uses a liquid as the mobile phase and separates the components in the mixture for qualitative and quantitative analysis through physical and chemical interactions in a stationary phase (such as a packed column). Specifically, HPLC not only efficiently separates components in complex mixtures but also allows for qualitative and quantitative analysis of the components by analyzing retention times and peak areas in the chromatogram; retention time is used to identify components, and peak area is used for quantitative analysis. Furthermore, HPLC detectors have high sensitivity, capable of detecting extremely low concentrations of components, making it suitable for trace analysis. Compared to traditional chromatography techniques, HPLC offers faster analysis speeds, enabling the completion of complex analytical tasks in a shorter time. Therefore, HPLC can be applied to the analysis of various types of samples, including organic compounds, biomolecules, pharmaceuticals, and environmental samples. It can be said that HPLC technology has become one of the most important tools in the field of chemical analysis. However, in certain specific analyses, the analyte may be difficult to detect directly due to a lack of sufficient ultraviolet absorption, fluorescence characteristics, or stability. To address this issue, derivatization technology has emerged, which involves converting the analyte into a derivative with stronger detection properties through a chemical reaction. However, existing derivatization processes often rely on manual operation, resulting in complexity, poor reproducibility, and low efficiency. While some automated derivatization devices exist on the market, they are typically separate from high-performance liquid chromatography (HPLC), exhibiting low integration and difficulty in achieving precise control of derivatization conditions. Therefore, this patent application is filed. Utility Model Content

[0003] The purpose of this invention is to provide a derivatization instrument for high performance liquid chromatography.

[0004] To achieve the above objectives, the solution of this utility model is:

[0005] A derivatizer for high performance liquid chromatography, comprising:

[0006] The reaction module includes at least one derivatization reaction chamber and an injection port connected thereto;

[0007] Temperature control system, which is integrated into the periphery of the reaction module;

[0008] The mobile phase control unit includes a gradient pump and an in-line mixer;

[0009] An automation control module, comprising a PLC controller and a robotic arm;

[0010] The wireless communication module supports Bluetooth 5.0 or ZigBee 3.0 protocols;

[0011] An anomaly handling module includes an ultrasonic cleaning device.

[0012] Preferably, the reaction module adopts a microfluidic chip structure, and the surface of the microfluidic chip is silanized.

[0013] Preferably, the injection port is connected to a high-performance liquid chromatograph.

[0014] Preferably, the gradient pump is a quaternary low-pressure gradient pump with multiple channels.

[0015] Preferably, the injection port includes at least three reagent injection ports, configured to connect to a derivatizing agent, a catalyst, and a cleaning solution, respectively.

[0016] Preferably, the temperature control system includes:

[0017] Peltier element arrays cover 60-90% of the surface area of ​​the reaction module;

[0018] Infrared temperature measurement unit, sampling frequency ≥10Hz;

[0019] A PID controller configured to establish a temperature-power feedback loop with a response time ≤0.5s.

[0020] Preferably, the temperature control system further includes a phase change material layer, which is made of paraffin-based composite phase change material, and the phase change temperature is set to three adjustable levels: 40°C, 60°C, and 80°C.

[0021] Preferably, the mobile phase control unit is configured as follows:

[0022] Provide a low flow rate of 0.01-0.1 mL / min during the derivatization stage;

[0023] During the rinsing phase, switch to a high flow rate of 1-5 mL / min;

[0024] The high-low flow rate switching time is ≤0.1s.

[0025] Preferably, the ultrasonic power of the ultrasonic cleaning device is 50-120 W.

[0026] Preferably, the online mixer is a supershear static online mixer.

[0027] The principle of this utility model is as follows:

[0028] First, the high-performance liquid chromatography (HPLC) derivatization instrument provided by this invention employs automated sample introduction technology to achieve precise and automatic sample and derivatization reagent aspiration and mixing. Second, the HPLC derivatization instrument provided by this invention utilizes precise temperature control technology: through the coordinated control of heating / cooling devices and a microprocessor, the reaction temperature is precisely adjusted. Third, the HPLC derivatization instrument provided by this invention employs efficient stirring technology: using a specially designed stirrer, it ensures that the reaction mixture is uniformly heated during the reaction process, improving reaction efficiency. Fourth, the HPLC derivatization instrument provided by this invention features an integrated design: the derivatization instrument can be directly connected to the HPLC instrument, achieving seamless integration of the analytical workflow.

[0029] The gain effect of this invention is as follows:

[0030] 1. The high-performance liquid chromatography derivatizer provided by this utility model significantly improves the efficiency and reproducibility of the derivatization process through automated sample injection and reaction control.

[0031] 2. The derivatizer for high performance liquid chromatography provided by this utility model can be highly integrated with the high performance liquid chromatograph, making the analysis process smoother and reducing analysis time.

[0032] 3. The high-performance liquid chromatography derivatizer provided by this utility model can ensure the consistency and accuracy of the derivatization reaction through precise control of derivatization conditions, thereby improving the reliability of the analytical results. Attached Figure Description

[0033] Figure 1 This is a schematic diagram of the utility model.

[0034] Explanation of reference numerals in the attached diagram: 1. Reaction module; 2. Derivatization reaction chamber; 3. Sample inlet; 4. Injection port; 5. Temperature control system; 6. Mobile phase control unit; 7. Gradient pump; 8. In-line mixer; 9. Automation control module; 10. PLC controller; 11. Robotic arm; 12. Wireless communication module; 13. Anomaly handling module; 14. Ultrasonic cleaning device; 15. Peltier element array; 16. Infrared temperature measurement unit; 17. PID controller. Detailed Implementation

[0035] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments. It should also be understood that the following embodiments are only for further illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Specific mass, reaction time, temperature, process parameters, etc., in the examples are merely examples within a suitable range. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention.

[0036] like Figure 1 The diagram shown is a structural schematic of the high-performance liquid chromatography derivatizer provided by this utility model. To clearly show the connection method of each part, a gap is left between the reaction module and the temperature control system, but this does not represent the actual design; the actual design is that the temperature control system is tightly integrated into the periphery of the reaction module.

[0037] The high-performance liquid chromatography derivatization instrument includes:

[0038] The reaction module includes at least one derivatization reaction chamber and an injection port connected thereto;

[0039] A temperature control system, integrated on the periphery of the reaction module, is configured to maintain the reaction chamber temperature at 20-150℃±0.5℃;

[0040] The mobile phase control unit includes a gradient pump and an online mixer, with a flow rate range of 0.01-5 mL / min;

[0041] The automation control module, including a PLC controller and a robotic arm, is configured to perform automatic sample injection, reaction parameter adjustment, and waste liquid discharge.

[0042] The wireless communication module supports Bluetooth 5.0 or ZigBee 3.0 protocols;

[0043] An anomaly handling module includes an ultrasonic cleaning device.

[0044] The reaction module adopts a microfluidic chip structure, and the surface of the microfluidic chip is silanized.

[0045] The injection port is connected to a high-performance liquid chromatograph.

[0046] The gradient pump is a quaternary low-pressure gradient pump with multiple channels.

[0047] The injection port includes at least three reagent injection ports, configured to connect to a derivatizing agent, a catalyst, and a cleaning solution, respectively.

[0048] The temperature control system includes:

[0049] Peltier element arrays cover 60-90% of the surface area of ​​the reaction module;

[0050] Infrared temperature measurement unit, sampling frequency ≥10Hz;

[0051] A PID controller configured to establish a temperature-power feedback loop with a response time ≤0.5s.

[0052] The temperature control system also includes a phase change material layer, which is made of paraffin-based composite phase change material, and the phase change temperature is set to three adjustable levels: 40℃, 60℃, and 80℃.

[0053] The mobile phase control unit is configured as follows:

[0054] Provide a low flow rate of 0.01-0.1 mL / min during the derivatization stage;

[0055] During the rinsing phase, switch to a high flow rate of 1-5 mL / min;

[0056] The high-low flow rate switching time is ≤0.1s.

[0057] The ultrasonic power of the ultrasonic cleaning device is 50-120 W.

[0058] The online mixer is a supershear static online mixer.

[0059] The specific operating steps of the derivatizer for high performance liquid chromatography are as follows:

[0060] Taking the derivatization reaction of a specific compound A as an example, the implementation process of this utility model is specifically explained.

[0061] S1. Based on the derivatization reaction characteristics of compound A, the reaction derivatization reaction temperature is set to 80℃, the reaction time to 30 minutes, and the stirring speed to 200 rpm on a mobile phone or a computer with wireless communication function via a wireless communication module.

[0062] S2. Load sample vials using a robotic arm;

[0063] S3. The temperature control system is used to raise the reaction chamber to the target temperature ±0.5℃ at a rate of 2-5℃ / min;

[0064] S4. Inject the sample and derivatizing agent at the first flow rate and maintain the reaction for time t1;

[0065] S5. Monitor the amount of product generated by an online detector, and trigger HPLC injection when the preset threshold is reached;

[0066] S6. After HPLC injection, switch to the second flow rate to rinse the reaction chamber. The second flow rate is 50-100 times that of the first flow rate. The specific cleaning steps are as follows:

[0067] a) Rinse with an alkaline cleaning solution for 30-60 seconds;

[0068] b) Switch to organic solvent rinsing for 20-40 seconds;

[0069] c) Finally, purge with carrier gas for 10-15 seconds at a pressure of 0.1-0.3 MPa.

[0070] In addition, when a reaction pressure fluctuation is detected to exceed a set threshold, the exception handling module is triggered and the following operations are performed automatically:

[0071] i) Pause the current process and start the backup flow path;

[0072] ii) Record abnormal data points and label the sample numbers;

[0073] iii) Activate the ultrasonic cleaning module to handle the blocked flow path.

[0074] The above description is only a preferred embodiment of the present utility model, but the scope of protection of the present utility model is not limited thereto. Any modifications, equivalent substitutions and improvements made on the basis of the overall concept of the present utility model shall fall within the scope of protection of the present utility model.

Claims

1. A derivatizer for high-performance liquid chromatography, characterized in that, include: The reaction module (1) includes at least one derivatization reaction chamber (2) and a sample injection port (3) and an injection port (4) connected thereto. Temperature control system (5), the temperature control system is integrated on the periphery of the reaction module; The flow phase control unit (6) includes a gradient pump (7) and an online mixer (8); The automation control module (9) includes a PLC controller (10) and a robotic arm (11). The wireless communication module (12) supports Bluetooth 5.0 or ZigBee 3.0 protocols; An anomaly handling module (13) includes an ultrasonic cleaning device (14).

2. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The reaction module adopts a microfluidic chip structure, and the surface of the microfluidic chip is silanized.

3. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The injection port is connected to a high-performance liquid chromatograph.

4. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The gradient pump is a quaternary low-pressure gradient pump with multiple channels.

5. The derivatizer for high performance liquid chromatography according to claim 2, characterized in that, The injection port includes at least three reagent injection ports, configured to connect to a derivatizing agent, a catalyst, and a cleaning solution, respectively.

6. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The temperature control system includes: Peltier element array (15) covers 60-90% of the surface area of ​​the reaction module; Infrared temperature measurement unit (16), sampling frequency ≥10Hz; The PID controller (17) is configured to establish a temperature-power feedback loop with a response time ≤0.5s.

7. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The temperature control system also includes a phase change material layer, which is made of paraffin-based composite phase change material, and the phase change temperature is set to three adjustable levels: 40℃, 60℃, and 80℃.

8. The derivatizer for high performance liquid chromatography according to claim 5, characterized in that, The mobile phase control unit is configured as follows: Provide a low flow rate of 0.01-0.1 mL / min during the derivatization stage; During the rinsing phase, switch to a high flow rate of 1-5 mL / min; The high-low flow rate switching time is ≤0.1s.

9. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The ultrasonic power of the ultrasonic cleaning device is 50-120 W.

10. The derivatizer for high performance liquid chromatography according to claim 1, characterized in that, The online mixer is a supershear static online mixer.

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