WO2024011790A1

WO2024011790A1 - Continuous countercurrent extraction device and method for traditional chinese medicines

Info

Publication number: WO2024011790A1
Application number: PCT/CN2022/129302
Authority: WO
Inventors: 臧恒昌; 林泊然; 孙钟毓; 张梦琪; 陈忠鑫; 马晓博; 张惠; 李连; 聂磊
Original assignee: 山东大学
Priority date: 2022-07-11
Filing date: 2022-11-02
Publication date: 2024-01-18
Also published as: CN114849277A; CN114849277B

Abstract

A continuous countercurrent extraction device and method for traditional Chinese medicines. A single-screw apparatus is used to convey medicinal materials; a heating apparatus (29), an ultrasonic apparatus (28) and a stirring apparatus (30) are provided to perform continuous countercurrent extraction on traditional Chinese medicines; the continuous countercurrent extraction process is monitored in real time by monitoring a medicinal liquid by means of a second near-infrared spectrum sampling apparatus (18), so as to determine a traditional Chinese medicine extraction end point; and a medicinal material extraction end point is determined by monitoring extracted medicine residues by means of a first near-infrared spectrum sampling apparatus (19). When it is detected that the extraction of the medicinal materials is completed, the medicine residues are continuously discharged by means of the single-screw apparatus, and in the extraction process, a solvent and the medicinal materials continuously enter an extraction tank body (1), and a traditional Chinese medicine extract and the medicine residues are continuously discharged out of the extraction tank body (1), thereby achieving efficient, rapid and economical continuous extraction of traditional Chinese medicines.

Description

A kind of continuous countercurrent extraction equipment and method of traditional Chinese medicine

The present invention claims the priority of the Chinese patent application submitted to the China Patent Office on July 11, 2022, with the application number 202210806974.3 and the invention name "A continuous countercurrent extraction equipment and method of traditional Chinese medicine", the entire content of which is incorporated herein by reference. Inventing.

Technical field

The invention relates to the technical field of separation and extraction of traditional Chinese medicine, and in particular to a continuous countercurrent extraction equipment and method of traditional Chinese medicine.

Background technique

The statements in this section merely provide background technical information related to the present invention and do not necessarily constitute prior art.

In the production process of modern traditional Chinese medicine, extraction is a key step in "removing the coarse and extracting the essence" and is a key link in the pharmaceutical process of traditional Chinese medicine. The extraction methods of traditional Chinese medicine include decoction, percolation, dipping, etc. With the development of modern Chinese medicine, modern Chinese medicine extraction technology has gradually developed new methods such as ultrasonic extraction, microwave extraction, and supercritical fluid extraction. However, no matter what method is used to extract traditional Chinese medicine, most of the current traditional Chinese medicine extraction processes are unit extraction, and there is a lack of effective means to effectively monitor the extraction process and scientifically judge the extraction endpoint. The extraction efficiency is low, energy consumption is high, and the quality is low. Uncontrollable and unable to produce continuously.

Contents of the invention

In order to solve the above problems, the present invention proposes a continuous countercurrent extraction equipment and method of traditional Chinese medicine, which can determine the end point of extraction of traditional Chinese medicine on the basis of realizing continuous extraction of traditional Chinese medicine.

In order to achieve the above objects, the present invention adopts the following technical solutions:

In the first aspect, a continuous countercurrent extraction equipment for traditional Chinese medicine is proposed, which includes an extraction tank main body that is tilted relative to the horizontal plane. The extraction tank main body includes a high end and a low end. The high end of the extraction tank main body is provided with an extraction liquid inlet pipe and a slag discharge pipe. The lower end of the tank body is provided with an inlet pipe and a liquid outlet pipe. A single screw device is installed in the main body of the extraction tank. The single screw device includes a motor and a screw conveyor rod. The screw conveyor rod is connected to the output shaft of the motor. The screw conveyor rod is used to transfer the medicine. The slag is transported back and forth between the feed pipe and the slag discharge pipe. The first near-infrared spectrum sampling device for obtaining the spectrum of the slag is set at the high end of the main body of the extraction tank. The first near-infrared spectrum sampling device is connected to the continuous countercurrent extraction integrated control system. , the continuous counter-current extraction integrated control system is connected to the motor. The continuous counter-current extraction integrated control system can judge whether the end point of medicinal material extraction has been reached based on the spectrum of the medicinal residue. When the end point of medicinal material extraction is reached, the medicinal residue will be discharged from the slag discharge pipe. When the end point of medicinal material extraction is reached, the motor is controlled to perform repeated reverse and forward rotation until the end point of medicinal material extraction is reached.

In the second aspect, a continuous extraction method of traditional Chinese medicine is proposed, including:

The solvent is transported to the main body of the extraction tank through the extraction liquid inlet pipe, and the medicinal materials are transported to the main body of the extraction tank through the feed pipe;

The medicinal materials and solvent are mixed in the main body of the extraction tank;

The medicinal liquid flows out from the outlet pipe;

The chemical slag is transported to the direction of the slag discharge pipe through a single screw device;

Obtain the medicinal residue spectrum through the first near-infrared spectrum sampling device;

The continuous countercurrent extraction integrated control system analyzes the spectrum of the medicinal residue to determine whether the end point of medicinal material extraction has been reached;

When the end point of medicinal material extraction is reached, the medicinal residue is discharged from the slag discharge pipe;

When the end point of medicinal material extraction is not reached, the motor is controlled to perform repeated reverse and forward rotation until the end point of medicinal material extraction is reached.

Compared with the prior art, the beneficial effects of the present invention are:

The present invention uses a single screw device to transport medicinal materials, and can be equipped with ultrasonic, heating and stirring devices on the single screw device, thereby realizing continuous counter-current extraction of traditional Chinese medicine.

The present invention obtains the medicinal residue spectrum by setting a first near-infrared spectrum sampling device at the high end of the main body of the extraction tank, and can then determine the end point of medicinal material extraction based on the medicinal residue spectrum. Only when the medicinal material extraction end point is reached can the medicinal residue be released, thereby ensuring The adequacy of extraction of traditional Chinese medicines, improving the quality of traditional Chinese medicines and reducing the cost of extraction of traditional Chinese medicines.

The present invention is provided with a second near-infrared spectrum sampling device at the low end of the main body of the extraction tank to obtain the liquid spectrum of traditional Chinese medicine. It can then perform component analysis of the liquid medicine based on the spectrum of the medicinal liquid, realize the process monitoring of the extraction of traditional Chinese medicine, and can The traditional Chinese medicine extraction endpoint is judged based on the spectrum of the medicinal liquid, and the real-time release of the traditional Chinese medicine extraction liquid is controlled based on the determined traditional Chinese medicine extraction endpoint.

The present invention realizes continuous counter-current extraction of traditional Chinese medicine by arranging the main body of the extraction tank tilted with respect to the horizontal plane. , achieves effective control of the solvent content in the medicinal residue, and avoids affecting the accuracy of judging the end point of medicinal extraction due to different solvent contents in the medicinal residue, thereby affecting the quality of traditional Chinese medicine extraction.

The present invention sets the pitch of the single-screw device in a manner that gradually decreases from the feeding pipe to the slag discharge pipe, which can squeeze the medicinal residue, further control the solvent content in the medicinal residue, and effectively ensure the determination of the end point of medicinal material extraction. accuracy.

The ultrasonic device, the heating device and the spiral conveying rod of the present invention are detachable, and the ultrasonic device or the heating device can be selected according to the different processing techniques of different traditional Chinese medicines, thereby being able to adapt to the extraction of different traditional Chinese medicines and improve the adaptability of the equipment of the present invention. .

The motor of the present invention is a forward and reverse bidirectional rotating motor, which can realize repeated squeezing and extraction of medicinal residue through forward and reverse rotation of the motor, ensuring the adequacy of extraction of medicinal residue, ensuring the extraction quality of traditional Chinese medicine, and reducing the cost of extracting traditional Chinese medicine.

The present invention is equipped with a cleaning liquid inlet pipe at the high end of the main body of the extraction tank. The liquid outlet pipe is connected to a three-way valve. The other two ends of the three-way valve are connected to the concentration device and the sewage pipe respectively. The cleaning liquid inlet pipe can be used to clean the liquid inlet pipe into the main body of the extraction tank. Inject cleaning liquid to clean the main body of the extraction tank. The cleaned liquid enters the sewage pipe through the three-way valve and is discharged. On the basis of continuous extraction of traditional Chinese medicine, automatic cleaning of the main body of the extraction tank is realized.

Additional advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.

Description of drawings

The description and drawings that constitute a part of this application are used to provide a further understanding of this application. The illustrative embodiments and their descriptions of this application are used to explain this application and do not constitute an improper limitation of this application.

Figure 1 is a schematic diagram of the overall structure of the disclosed equipment in Embodiment 1;

Figure 2 is a schematic structural diagram of the continuous countercurrent extraction tank of the disclosed equipment in Embodiment 1;

Figure 3 is a schematic connection diagram of the stirring device of the disclosed equipment in Embodiment 1;

Figure 4 is a module diagram of the continuous countercurrent extraction integrated control system of the disclosed equipment in Embodiment 1;

Figure 5 is a flow chart for establishing a traditional Chinese medicine NIRS model of the disclosed equipment in Embodiment 1;

Figure 6 is a schematic diagram of medicinal material extraction endpoint control of the disclosed equipment in Embodiment 1;

Figure 7 is a work flow chart of the disclosed equipment in Embodiment 1;

Figure 8 is the original NIRS of the Tibetan Artemisia arborescens extraction process disclosed in Example 1;

Figure 9 is a diagram showing the results of the NIRS model of Gentianopicroside disclosed in Example 1;

Figure 10 is a diagram showing the results of the NIRS model of Swertia swertiensis disclosed in Example 1;

Figure 11 is a diagram of the NIRS model results of Yincheng mangiferin disclosed in Example 1;

Figure 12 is the spectrum of the medicinal residue disclosed in Example 1;

Figure 13 is a graph showing the change trend of MBSD and relative concentration change rate (RCCR) over time during the extraction process of Tibetan Artemisia cordata disclosed in Example 1.

Among them: 1. Extraction tank main body, 2. Fixed bracket, 3. Feed pipe, 4. Slag discharge pipe, 5. Cleaning liquid inlet pipe, 6. Extraction liquid inlet pipe, 7. Liquid outlet pipe, 8. First valve , 9. The second valve, 10. The third valve, 11. The first delivery pump, 12. The fourth valve, 13. The second delivery pump, 14. The fifth valve, 15. Three-way valve, 16. Remote control terminal , 17. Continuous countercurrent extraction integrated control system, 18. Second near-infrared spectrum sampling device, 19. First near-infrared spectrum sampling device, 20. Filter, 21. Limiting device, 22. Top cover, 23. Rotating shaft , 24. Motor, 25. Transmission block, 26. Rotating rod body, 27. External thread, 28. Ultrasonic device, 29. Heating device, 30. Stirring device.

Detailed ways

The present invention will be further described below in conjunction with the accompanying drawings and examples.

It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless otherwise defined, all technical and scientific terms used herein have the same meanings commonly understood by one of ordinary skill in the art to which this application belongs.

It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, the singular forms are also intended to include the plural forms unless the context clearly indicates otherwise. Furthermore, it will be understood that when the terms "comprises" and/or "includes" are used in this specification, they indicate There are features, steps, operations, means, components and/or combinations thereof.

In the present invention, terms such as "upper", "lower", "left", "right", "front", "back", "vertical", "horizontal", "side", "bottom", etc. The orientation or positional relationship is based on the orientation or positional relationship shown in the drawings. It is only a relative word determined to facilitate the description of the structural relationship of various components or elements of the present invention. It does not specifically refer to any component or element of the present invention and cannot be understood as a reference to the present invention. Limitations of Invention.

In the present invention, terms such as "fixed", "connected", "connected", etc. should be understood in a broad sense, indicating that it can be a fixed connection, an integral connection or a detachable connection; it can be a direct connection or an intermediate connection. Media are indirectly connected. For relevant scientific researchers or technicians in the field, the specific meanings of the above terms in the present invention can be determined according to specific circumstances, and should not be understood as limitations of the present invention.

Example 1

In order to achieve continuous counter-current extraction of traditional Chinese medicine, a continuous counter-current extraction equipment for traditional Chinese medicine is disclosed in this embodiment, which includes an extraction tank main body that is tilted relative to the horizontal plane. The extraction tank main body includes a high end and a low end, and the high end of the extraction tank main body is set Extract the liquid inlet pipe and the slag outlet pipe. The low end of the main body of the extraction tank is provided with the feed pipe and the liquid outlet pipe. A single screw device is installed in the main body of the extraction tank. The single screw device includes a motor and a screw conveyor rod. The output of the screw conveyor rod and the motor is The shaft is connected, and the screw conveyor rod is used to transport the dregs back and forth between the feed pipe and the slag discharge pipe. The first near-infrared spectrum sampling device for obtaining the spectrum of the dregs is set at the high end of the main body of the extraction tank. The first near-infrared spectrum The sampling device is connected to the continuous countercurrent extraction integrated control system, and the continuous countercurrent extraction integrated control system is connected to the motor. The continuous countercurrent extraction integrated control system can judge whether the medicinal material extraction end point is reached based on the spectrum of the medicinal residue. When the medicinal material extraction end point is reached, the medicinal material extraction end point is reached. The slag is discharged from the slag discharge pipe. When the end point of medicinal material extraction is not reached, the motor is controlled to repeatedly rotate in reverse and forward directions until the end point of medicinal material extraction is reached.

Further, an interface is provided on the spiral conveying rod, and the interface is used to connect with the ultrasonic device or the heating device.

Further, the screw conveyor rod includes a rotating rod main body, an external thread is provided on the rotating rod main body, and the pitch of the external thread gradually becomes smaller from the feed pipe to the slag discharge pipe.

Further, a stirring device is connected to the external thread.

Further, a cleaning liquid inlet pipe is provided at the high end of the main body of the extraction tank, and a fourth valve is provided on the cleaning liquid inlet pipe. The fourth valve is connected to the continuous countercurrent extraction integrated control system.

Further, a filter screen is connected to one end of the screw conveyor rod close to the slag discharge pipe.

Further, a second near-infrared spectrum sampling device for obtaining the spectrum of the medicinal liquid is provided at the low end of the main body of the extraction tank. The second near-infrared spectrum sampling device is connected to the continuous counter-current extraction integrated control system. The continuous counter-current extraction integrated control system also uses The extraction end point of the Chinese medicine is judged based on the spectrum of the medicinal liquid. When the end point of the extraction of the Chinese medicine is reached, the Chinese medicine extraction liquid is discharged from the outlet tube.

Further, a first valve is provided on the feed pipe, a second valve is provided on the slag discharge pipe, a third valve is provided on the extraction liquid inlet pipe, and a fifth valve is provided on the liquid outlet pipe. The first valve and the second valve are provided on the liquid outlet pipe. The valve, the third valve, and the fifth valve are all connected to the continuous countercurrent extraction integrated control system.

Further, the liquid outlet pipe is connected to the three-way valve, and the other two ends of the three-way valve are connected to the concentration device and the sewage pipe respectively.

The continuous counter-current extraction equipment for traditional Chinese medicine disclosed in this embodiment will be described in detail. As shown in Figures 1-3, the continuous counter-current extraction equipment for traditional Chinese medicine includes a continuous counter-current extraction tank, a continuous counter-current extraction integrated control system 17 and a remote control terminal 16.

As shown in Figure 2, the continuous counter-current extraction tank includes an extraction tank main body 1 that is inclined relative to the horizontal plane. The extraction tank main body 1 includes a high end and a low end. Among them, the end of the extraction tank main body 1 away from the horizontal plane is the high end, and the extraction tank main body 1 is close to the horizontal plane. One end of the horizontal plane is the low end.

The extraction tank body 1 is fixed on the ground through the fixing bracket 2. The preferred angle of inclination of the extraction tank body 1 relative to the horizontal plane is 15°.

An extraction liquid inlet pipe 6, a slag discharge pipe 4 and a cleaning liquid inlet pipe 5 are set at the high end of the extraction tank body 1, and a feed pipe 3 and a liquid outlet pipe 7 are set at the low end of the extraction tank body 1. On the feed pipe 3 Set the first valve 8, set the second valve 9 on the slag discharge pipe 4, connect the extraction liquid inlet pipe 6 with the first delivery pump 11, and pump the solvent into the extraction tank body 1 through the first delivery pump 11. During the extraction A third valve 10 is provided on the liquid inlet pipe 6 to connect the cleaning liquid inlet pipe 5 with the second delivery pump 13. The cleaning liquid is pumped into the extraction tank body 1 through the second delivery pump 13. A third valve 10 is provided on the cleaning liquid inlet pipe 5. The fourth valve 12 connects the liquid outlet pipe 7 with the three-way valve 15. The other two ends of the three-way valve 15 are connected to the concentration device and the sewage pipe respectively. A fifth valve 14 is provided on the liquid outlet pipe 7.

The solvent is transported into the main body 1 of the extraction tank through the extraction liquid inlet pipe 6, and the medicinal materials are transported into the main body 1 of the extraction tank through the inlet pipe 3. The solvent and medicinal materials are mixed in the main body 1 of the extraction tank, and the Chinese medicine extract liquid is obtained from the liquid outlet pipe. 7 flows out, and the obtained slag is discharged from the slag discharge pipe 4. The medicinal liquid flows out from the liquid outlet pipe 7 and enters the concentration device for concentration to obtain the concentrated Chinese medicine. After the Chinese medicine is obtained, the cleaning liquid is injected into the main body 1 of the extraction tank through the cleaning liquid inlet pipe 5 for cleaning. The cleaned liquid passes through the outlet After the liquid pipe 7 flows out, it enters the sewage pipe and flows out through the sewage pipe.

A single screw device is provided inside the main body 1 of the extraction tank. The single screw device includes a motor 24 and a screw conveyor rod connected to the output shaft of the motor 24. The motor 24 can rotate in both forward and reverse directions. The forward and reverse rotation of the motor 24 can drive the screw conveyor rod to The slag is transported back and forth between the feed pipe 3 and the slag discharge pipe 4.

The spiral conveyor rod includes a rotating rod main body 26. The rotating rod main body 26 is provided with an external thread 27. One end of the rotating rod main body 26 is connected to the filter screen. After the filter screen is connected to the rotating rod main body 26, the filter screen is fixed through the limiting device 21. The limiting device 21 can be a nut. Through the setting of the filter, the Chinese medicine extract is filtered out to ensure the purity of the Chinese medicine extract.

The other end of the rotating rod body 26 is connected to the rotating shaft 23 through the transmission block 25. The rotating shaft 23 is connected to the output shaft of the motor 24. When the output shaft of the motor rotates, the rotating shaft 23 is driven to rotate, which in turn drives the rotating rod main body 26 to rotate. The transmission block 25 is fixed on the top cover 22, and the top cover 22 is connected to the high end of the extraction tank body 1.

In order to adapt to the requirements of different traditional Chinese medicine processing techniques, multiple interfaces are provided on the main body 26 of the rotating rod. The interfaces can be connected to the ultrasonic device 28 or the heating device 29. When ultrasonic processing technology is required, the interfaces are connected to the ultrasonic device 28 to control the traditional Chinese medicine. Carry out ultrasonic extraction. When a heating process is required, connect the interface to the heating device 29 to perform heating and extraction of the Chinese medicine. When ultrasonic and heating are required at the same time, connect the ultrasonic device 28 and the heating device 29 to the rotating rod body 26 through the interface, and The ultrasonic device 28 and the heating device 29 are arranged on the rotating rod 26 at intervals to perform ultrasonic heating and extraction.

The interface may be a threaded interface through which the ultrasonic device 28 or the heating device 29 is threadedly connected.

The ultrasonic device 28 uses an ultrasonic transducer, and the heating device 29 uses an electric heater.

In order to ensure that the medicinal materials and the solvent are fully mixed, and can be fully ultrasonic or heated, so as to make the Chinese medicine more fully extracted, a stirring device 30 is provided on the external thread 27, and the mixture of the medicinal materials and the solvent is stirred by the stirring device 30.

The stirring device can use a connected second motor and a fan blade, and the second motor drives the fan blade to rotate to achieve stirring of the mixture of medicinal materials and solvent.

In order to realize automatic control of the extraction of traditional Chinese medicine, a continuous countercurrent extraction integrated control system, a first near-infrared spectrum sampling device 19 and a second near-infrared spectrum sampling device 18 are set up, and the first valve 8, the second valve 9, the third The valve 10, the fourth valve 12, and the fifth valve 14 are all configured as electric valves, and the three-way valve 15 is configured as an electric three-way valve.

The first near-infrared spectrum sampling device 19 and the second near-infrared spectrum sampling device 18 both use near-infrared spectrometers.

The first near-infrared spectrum sampling device 19 is arranged at the high end of the extraction tank body 1 to obtain the spectrum of the medicinal residue, and the second near-infrared spectrum sampling device 18 is arranged at the low end of the extraction tank body 1 to obtain the spectrum of the liquid of the traditional Chinese medicine.

Connect the motor 24, the first near-infrared spectrum sampling device 19, the second near-infrared spectrum sampling device 18, the first valve 8, the second valve 9, the third valve 10, the fourth valve 12, the fifth valve 14, and the three-way valve. 15. The ultrasonic device, heating device, second motor, first delivery pump, and second delivery pump are all communicatively connected to the continuous countercurrent extraction integrated control system 17.

The continuous countercurrent extraction integrated control system 17 analyzes the acquired medicinal residue spectrum and medicinal liquid spectrum, determines the medicinal material extraction end point by analyzing the medicinal residue spectrum, controls the second valve according to the medicinal material extraction end point, and controls the medicinal liquid spectrum by analyzing the medicinal liquid spectrum. Analyze and determine the extraction end point of the traditional Chinese medicine, and control the fifth valve 14 according to the extraction end point of the traditional Chinese medicine.

As shown in Figure 4, the continuous countercurrent extraction integrated control system 17 includes a continuous extraction process monitoring and end-point judgment system, and an intelligent control system. Among them, the intelligent control system is connected with each valve, three-way valve, motor and the first near-infrared spectrum sampling device 19 , the second near-infrared spectrum sampling device 18 is connected.

The end-point judgment model and key quality parameter prediction model are stored in the continuous extraction process monitoring and end-point judgment system. The end-point judgment model is used to analyze the spectrum of the medicinal residue to determine whether the end point of medicinal material extraction has been reached, and the key quality parameter prediction model is used to analyze and judge the spectrum of the medicinal liquid. Whether the end point of traditional Chinese medicine extraction has been reached.

When near-infrared spectroscopy (NIRS) is applied in the field of traditional Chinese medicine, it is often combined with chemometrics to establish a critical quality parameter prediction model. The critical quality parameter prediction model uses a chemometrics model. The model establishment process is shown in Figure 5. As shown, in order to train the constructed chemometrics model through existing medicinal liquid samples and corresponding medicinal liquid composition data, obtain the critical quality parameter prediction model, analyze the medicinal liquid spectrum through the critical quality parameter prediction model, and obtain the traditional Chinese medicine The key quality parameter data is used to monitor the ingredients of traditional Chinese medicine. Based on the key quality parameter data, it is judged whether the end point of extraction of traditional Chinese medicine has been reached. When the key quality parameter data reaches the set standard value, it is judged that the end point of extraction of traditional Chinese medicine has been reached, and the fifth valve opens. Discharge the Chinese medicine extract.

The end point judgment model can be constructed using the moving block standard deviation (MBSD) method, but it is not limited to this method. The construction method of the end point judgment model can be selected according to actual needs, so that the constructed end point judgment model can be constructed based on The medicinal residue spectrum can be used to judge the extraction end point of medicinal materials. In this embodiment, the end point judgment model constructed by the moving window standard deviation method is used as an example to describe the end point judgment model in detail.

The moving window standard deviation method is used to construct the end point judgment model. This method uses n consecutive drug residue spectra as windows, calculates the standard deviation (SD) value of the window, and then calculates the average SD as the MBSD value of the window. The window moves forward by a new spectrum to obtain a new window, and the updated MBSD value is calculated according to the above method. The calculation formulas are as shown in (1) and (2).

Among them, Aij is the absorbance of the jth spectrum at wavelength point i;

is the average absorbance of all spectra in the window at wavelength point i; m is the number of wavelength points, and n is the number of windows. The change of different MBSD values over time is an indicator of whether the end point of medicinal material extraction has been reached. The time point when the MBSD value tends to be stable is considered to have reached the end point of medicinal material extraction.

As shown in Figure 6, the continuous countercurrent extraction integrated control system controls the second valve to open when it detects that the end point of medicinal material extraction has been reached, and discharges the medicinal residue through the slag discharge pipe. When it detects that the end point of medicinal material extraction has not been reached, it controls the motor to repeatedly Reverse and forward rotation until the second valve is controlled to open when the end point of medicinal material extraction is reached to discharge the medicinal residue.

In order to ensure the accuracy of judging the end point of medicinal material extraction and to control the moisture content of the medicinal residue, in addition to setting the main body of the extraction tank at an angle to the horizontal plane and setting the slag discharge pipe at the high-end position of the main body of the extraction tank, the external thread 27 is also set to be In the form of variable pitch, the pitch of the external thread 27 gradually becomes smaller from the feeding pipe to the slag discharge pipe. By setting the external thread 27 to the form of variable pitch, the slag can be fully squeezed and the moisture content of the slag can be controlled. Control to effectively ensure the accuracy of the endpoint judgment of medicinal material extraction.

The continuous countercurrent extraction integrated control system 17 is also connected to the remote control terminal 16, and various data obtained by the continuous countercurrent extraction integrated control system are displayed through the remote control terminal 16 to facilitate remote monitoring of the continuous countercurrent extraction process of traditional Chinese medicine.

The remote control terminal 16 can be a computer.

The work flow of a traditional Chinese medicine countercurrent extraction equipment disclosed in this embodiment is shown in Figure 7. Add solvent into the main body of the extraction tank through the extraction liquid inlet pipe, turn on the motor of the single screw device, control the rotation of the screw conveyor rod, turn on the heating device or After the ultrasonic device is processed to the set conditions, the medicinal materials are added to the main body of the extraction tank through the feeding pipe, and the medicinal residue spectrum and the medicinal liquid spectrum are obtained. The medicinal material extraction end point is judged through the medicinal residue spectrum, and the traditional Chinese medicine extraction end point is determined through the medicinal liquid spectrum. It is judged that when the end point of extraction of traditional Chinese medicine is reached, the fifth valve on the liquid outlet pipe is opened. When the end point of extraction of medicinal materials is reached, the second valve on the slag outlet pipe is opened, and the first valve on the feed pipe and the extraction liquid inlet pipe are closed. The third valve on the liquid outlet pipe and the fifth valve on the liquid outlet pipe. After all the medicinal residues are discharged, turn off the heating or ultrasonic device, open the fifth valve on the liquid outlet pipe, discharge all the medicinal liquid, and clean the liquid inlet pipe to Add cleaning fluid to the main body of the extraction tank, open the fifth valve on the liquid outlet pipe, and discharge the cleaning fluid after cleaning the extraction tank into the sewage pipe.

The continuous countercurrent extraction equipment for traditional Chinese medicine disclosed in this embodiment will be described in detail by taking Artemisia vulgaris as an example.

A key quality parameter prediction model was constructed based on the original NIRS spectrum of Tibetan Artemisia miltiorrhiza as shown in Figure 8. The original spectra were preprocessed respectively, and the best modeling interval was selected. Key parameter prediction models were performed on the three key quality parameters of Tibetan wormwood. Modeling was used to quantitatively monitor three key quality parameters of Artemisia arborescens during the extraction process. The model evaluation parameters are shown in Table 1, and the model results of the three key quality parameter prediction models are shown in Figures 9, 10 and 11. Among them, Figure 9 shows the results of the gentiopicrin model, Figure 10 shows the results of the swertidin model, and Figure 11 shows the results of the mangiferin model.

Table 1 Evaluation parameters of the key quality parameter prediction model for the Tibetan Artemisia extract process

A single-screw device is used to transport medicinal materials, equipped with heating, ultrasonic and stirring devices, for continuous counter-current extraction of Chinese medicines;

The medicinal residue spectrum is acquired by the first near-infrared spectrum sampling device to determine the medicinal material extraction end point, and the medicinal liquid spectrum is acquired by the second near-infrared spectrum sampling device to determine the traditional Chinese medicine extraction end point.

According to the judgment results of the end point of medicinal material extraction and the end point of traditional Chinese medicine extraction, the running speed and direction of the motor and the opening and closing of each valve are controlled through the continuous countercurrent extraction integrated control system.

During the extraction process, the solvent and medicinal materials continuously enter the main body of the extraction tank, and the medicinal liquid and residue are continuously discharged from the main body of the extraction tank, ultimately achieving efficient, fast, and economical continuous extraction of traditional Chinese medicines.

The acquired spectrum of Tibetan Artemisia dregs is shown in Figure 12. After performing spectral preprocessing and band selection on the spectrum of the medicinal dregs, an appropriate window size is selected to determine the MBSD end point. The obtained MBSD change trend chart is shown in Figure 13 (b) shown.

The key quality parameters in the extraction process of traditional Chinese medicine were measured, and the results obtained are shown in Figure 13(a). The extraction endpoints determined by these two methods are both around 100 minutes, proving that the MBSD method can be used instead of the traditional method to determine the extraction endpoint of medicinal residues. .

This embodiment discloses a continuous counter-current extraction equipment for traditional Chinese medicine, which uses a single-screw device to transport medicinal materials and is equipped with heating, ultrasonic and stirring devices to achieve continuous counter-current extraction of traditional Chinese medicine, and can perform close-in extraction of medicinal residues and medicinal liquids. Infrared monitoring, online monitoring of the continuous countercurrent extraction process of traditional Chinese medicine based on near-infrared monitoring results, and judgment of the extraction endpoints of traditional Chinese medicine and medicinal residues. Compared with the commonly used unit, discontinuous, discrete extraction methods and control methods, this method The continuous countercurrent extraction tanks disclosed in the embodiments can be used in parallel, are more flexible in the extraction of multiple medicinal materials, and can accurately, quickly and non-destructively monitor the changes in the active ingredients during the extraction process, and accurately determine the extraction endpoint of the extracted medicinal materials and the extraction endpoint of the medicinal liquid, forming Continuous and uninterrupted extraction effectively saves energy and raw material consumption, improves the speed of liquid medicine content monitoring, better ensures the quality of traditional Chinese medicine, and meets the requirements of "improving quality and increasing efficiency" in the modernization of traditional Chinese medicine.

This embodiment discloses a continuous counter-current extraction equipment for traditional Chinese medicine, which uses a single-screw device to transport medicinal materials, and is equipped with an ultrasonic, heating and stirring device on the single-screw device, thereby realizing continuous counter-current extraction of traditional Chinese medicine. A first near-infrared spectrum sampling device is installed at the high end of the main body of the extraction tank to obtain the spectrum of the medicinal residue, and then the end point of medicinal material extraction can be determined based on the spectrum of the medicinal residue. Only when the end point of medicinal material extraction is reached can the medicinal residue be released, thus ensuring the accuracy of the extraction of traditional Chinese medicine. sufficiency, improve the quality of traditional Chinese medicine, and reduce the cost of traditional Chinese medicine extraction. A second near-infrared spectrum sampling device is set up at the low end of the main body of the extraction tank to obtain the liquid spectrum of traditional Chinese medicine, which can then perform component analysis of the medicinal liquid based on the spectrum of the medicinal liquid, thereby monitoring the process of extracting traditional Chinese medicine, and based on the component analysis The results determine the endpoint of traditional Chinese medicine extraction to ensure the quality of traditional Chinese medicine. Through the main body of the extraction tank that is tilted relative to the horizontal plane, the liquid inlet pipe and the slag discharge pipe are set at the high end of the main body of the extraction tank, and the liquid outlet pipe is set at the low end of the main body of the extraction tank. On the basis of realizing continuous countercurrent extraction of traditional Chinese medicine, The countercurrent flushing of the solvent achieves effective control of the solvent content in the medicinal residue, preventing the difference in solvent content in the medicinal residue from affecting the accuracy of judging the end point of medicinal extraction, thereby affecting the quality of traditional Chinese medicine extraction. Setting the pitch of the single-screw device to gradually decrease from the feeding pipe to the slag discharge pipe can squeeze the medicinal residue, further control the solvent content of the medicinal residue, and effectively ensure the accuracy of judging the end point of medicinal material extraction. The ultrasonic device, heating device and spiral conveying rod of this embodiment are detachable, and the ultrasonic device or the heating device can be selected according to the different processing techniques of different traditional Chinese medicines, thereby being able to adapt to the extraction of different traditional Chinese medicines and improve the adaptability of the equipment; The motor in this embodiment is a forward and reverse bidirectional rotating motor, which can realize repeated squeezing and extraction of medicinal residues through forward and reverse rotation of the motor, ensuring the adequacy of extraction of medicinal residues, ensuring the extraction quality of traditional Chinese medicines, and reducing the cost of extracting traditional Chinese medicines.

Example 2

In this embodiment, a continuous extraction method of traditional Chinese medicine is disclosed, including:

The medicinal liquid flows out from the outlet tube;

Further, obtain the spectrum of the medicinal residue through a second near-infrared spectrum sampling device;

The continuous countercurrent extraction integrated control system analyzes the spectrum of the medicinal liquid and determines the end point of the extraction of traditional Chinese medicine;

When the end point of Chinese medicine extraction is reached, the Chinese medicine extraction liquid is discharged from the outlet pipe.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that the present invention can still be modified. Modifications or equivalent substitutions may be made to the specific embodiments, and any modifications or equivalent substitutions that do not depart from the spirit and scope of the invention shall be covered by the scope of the claims of the invention.

Claims

A continuous countercurrent extraction equipment for traditional Chinese medicine, which is characterized in that it includes an extraction tank main body that is tilted relative to the horizontal plane. The extraction tank main body includes a high end and a low end. The high end of the extraction tank main body is equipped with an extraction liquid inlet pipe and a slag discharge pipe. The extraction tank main body The low end of the extraction tank is equipped with a feed pipe and a liquid outlet pipe, and a single screw device is installed in the main body of the extraction tank. The single screw device includes a motor and a screw conveyor rod. The screw conveyor rod is connected to the output shaft of the motor. The screw conveyor rod is used to transfer the medicinal residue in the The feed pipe and the slag discharge pipe are transported back and forth. The first near-infrared spectrum sampling device for obtaining the spectrum of the slag is set at the high end of the extraction tank body. The first near-infrared spectrum sampling device is connected to the continuous countercurrent extraction integrated control system. The counter-current extraction integrated control system is connected to the motor. The continuous counter-current extraction integrated control system can judge whether the medicinal material extraction end point has been reached based on the medicinal residue spectrum. When the medicinal material extraction end point is reached, the medicinal material residue is discharged from the slag discharge pipe. When the medicinal material extraction end is not reached, the medicinal material extraction is not reached. At the end point, the motor is controlled to perform repeated reverse and forward rotation until it reaches the end point of medicinal material extraction; a second near-infrared spectrum sampling device for obtaining the spectrum of the medicinal liquid is set at the low end of the main body of the extraction tank. The second near-infrared spectrum sampling device and The continuous counter-current extraction integrated control system is connected. The continuous counter-current extraction integrated control system is also used to judge the end point of Chinese medicine extraction based on the spectrum of the medicinal liquid. When the end point of Chinese medicine extraction is reached, the Chinese medicine extraction liquid is discharged from the outlet tube; the moving window standard is adopted The deviation method constructs an end-point judgment model. This method uses n consecutive medicinal residue spectra as a window, calculates the SD value of the window, and then calculates the average SD as the MBSD value of the window. The time point when the MBSD value tends to be stable is considered to be the arrival of the medicinal material. Extract end point.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 1, characterized in that an interface is provided on the spiral conveying rod, and the interface is used to connect with an ultrasonic device or a heating device.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 1, characterized in that the spiral conveyor rod includes a rotating rod body, an external thread is provided on the rotating rod body, and the pitch of the external thread gradually changes from the feeding pipe to the slag discharge pipe. Small.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 3, characterized in that a stirring device is connected to the external thread.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 1, characterized in that a fourth valve is provided on the cleaning liquid inlet pipe, and the fourth valve is connected to the continuous countercurrent extraction integrated control system.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 1, characterized in that a filter screen is connected to one end of the screw conveyor rod close to the slag discharge pipe.
A continuous countercurrent extraction equipment for traditional Chinese medicine as claimed in claim 1, characterized in that a first valve is provided on the feed pipe, a second valve is provided on the slag discharge pipe, and a third valve is provided on the extraction liquid inlet pipe. A fifth valve is provided on the liquid outlet pipe, and the first valve, the second valve, the third valve, and the fifth valve are all connected to the continuous countercurrent extraction integrated control system.
A continuous countercurrent extraction equipment for traditional Chinese medicine according to claim 1, characterized in that the liquid outlet pipe is connected to a three-way valve, and the other two ends of the three-way valve are connected to the concentration device and the sewage pipe respectively.
A continuous extraction method of traditional Chinese medicine, which is characterized by including:

The solvent is transported to the main body of the extraction tank through the extraction liquid inlet pipe, and the medicinal materials are transported to the main body of the extraction tank through the feed pipe;

The medicinal materials and solvent are mixed in the main body of the extraction tank;

The medicinal liquid flows out from the outlet tube;

The chemical slag is transported to the direction of the slag discharge pipe through a single screw device;

Obtain the medicinal residue spectrum through the first near-infrared spectrum sampling device;

The continuous countercurrent extraction integrated control system analyzes the spectrum of the medicinal residue to determine whether the end point of medicinal material extraction has been reached;

When the end point of medicinal material extraction is reached, the medicinal residue is discharged from the slag discharge pipe;

When the end point of medicinal material extraction is not reached, the motor is controlled to perform repeated reverse and forward rotation until the end point of medicinal material extraction is reached;

a second near-infrared spectrum sampling device that acquires the spectrum of the medicinal liquid through the second near-infrared spectrum sampling device;

The continuous countercurrent extraction integrated control system determines the end point of Chinese medicine extraction based on the spectrum of the medicinal liquid. When the end point of Chinese medicine extraction is reached, the Chinese medicine extraction liquid is discharged from the outlet pipe;

The moving window standard deviation method is used to construct the end-point judgment model. This method uses n continuous medicinal residue spectra as windows, calculates the SD value of the window, and then calculates the average SD as the MBSD value of the window. The time point when the MBSD value tends to be stable is It is considered that the end point of medicinal material extraction has been reached.