CN-122018475-A - On-line detection method and quality control system for traditional Chinese medicine production

CN122018475ACN 122018475 ACN122018475 ACN 122018475ACN-122018475-A

Abstract

The invention relates to the technical field of detection and analysis control, and discloses a traditional Chinese medicine production online detection method and a quality control system, wherein the system respectively forms sampling circulation, constant temperature quantitative circulation and detection circulation through the switching of passages of a six-way valve group so as to realize the online acquisition, constant temperature quantitative treatment and near infrared spectrum detection of liquid medicine, a quality analysis module and a control strategy module are embedded in a control and data analysis unit, and the quality analysis module outputs a key quality attribute real-time value after preprocessing the acquired near infrared spectrum data; the control strategy module dynamically adjusts the technological parameters to realize the self-adaptive quality control of the production process. The invention realizes the low-consumption high-efficiency on-line detection and the dynamic control of quality driving in the traditional Chinese medicine production process, and effectively improves the quality stability and uniformity of the product.

Inventors

CHEN ZHONGXIN
LI ZHENYU
XU YANG
LI LIAN
WANG YANWEN
YANG TIANJIA

Assignees

中北大学

Dates

Publication Date: 20260512
Application Date: 20260414

Claims (9)

1. An on-line quality control system for Chinese medicine production, comprising: the six-way valve group (5) is used for switching different fluid passages under the action of a control signal; the sampling unit comprises a production container (1), and an outlet and a reflux inlet of the production container (1) are respectively connected with a fifth port (E) and a sixth port (F) of the six-way valve group (5) through a sampling pipeline and a circulating pipeline; The constant temperature quantitative unit is used for performing constant temperature quantitative treatment on the liquid medicine and comprises a constant temperature quantitative box (8) with an inner cavity with a fixed volume, an inlet and an outlet of the constant temperature quantitative box (8) are respectively connected with a first port (A) and a fourth port (D) of the six-way valve group (5), a flowmeter is arranged at an inlet of the constant temperature quantitative box (8), and a constant temperature controller (9) is arranged on the constant temperature quantitative box (8); the driving and cleaning unit is used for providing driving force and cleaning a system and comprises an elution solvent bottle (11), wherein an outlet of the elution solvent bottle (11) is connected into a third port (C) of the six-way valve group (5) through a distilled water pipe, and a detection quantitative pump (10) is arranged on the distilled water pipe; The detection circulation unit is used for leading out liquid medicine and collecting near infrared spectrum data of the liquid medicine and comprises a flow cell (12), a liquid inlet (1201) of the flow cell (12) is connected with a second port (B) of the six-way valve group (5), a liquid outlet of the flow cell (12) is connected with a waste liquid cell (13), an optical fiber probe (1401) of a near infrared spectrometer (14) is arranged in the flow cell (12), the optical fiber probe (1401) is immersed in the liquid medicine, and a temperature sensor (1202) is arranged at the upper part of the flow cell (12); The control and data analysis unit is used for controlling the system, receiving and processing near infrared spectrum data and outputting real-time data of key quality attributes, and is respectively and electrically connected with the six-way valve group (5), the sampling unit, the constant-temperature quantifying unit, the driving and cleaning unit and the detection circulating unit, and comprises an industrial personal computer (15), wherein the industrial personal computer (15) is integrated with a quality analysis module and a control strategy module, the quality analysis module is used for calculating the real-time value of the key quality attributes according to the near infrared spectrum data acquired by the near infrared spectrometer (14), and the control strategy module is used for outputting control signals according to the real-time value of the key quality attributes and controlling the traditional Chinese medicine production process parameter adjusting mechanism; The control and data analysis unit is configured to control the six-way valve group (5) to be switched to different passage states so as to respectively form a sampling cycle, a constant temperature quantitative cycle and a detection cycle.
2. The on-line quality control system for Chinese medicine production according to claim 1, wherein the sampling cycle is that the fifth port (E) and the sixth port (F) of the six-way valve group (5) are communicated; the constant temperature quantitative circulation is that a sixth port (F) and a first port (A) of the six-way valve group (5) are communicated, and a fourth port (D) is communicated with a fifth port (E); The detection cycle is that a third port (C) and a fourth port (D) of the six-way valve group (5) are communicated, and a first port (A) and a second port (B) are communicated.
3. The on-line quality control system for traditional Chinese medicine production according to claim 1, wherein the six-way valve group (5) comprises a six-way valve housing (506), a port valve seat (505) is installed at the front end in the six-way valve housing (506), six ports are sequentially arranged on the port valve seat (505) along the circumferential direction, and are respectively a first port (a), a second port (B), a third port (C), a fourth port (D), a fifth port (E) and a sixth port (F); A main shaft (507) is rotatably mounted in the six-way valve housing (506) through a bearing (508), three communication grooves (509) are formed in the front end of the main shaft (507), each communication groove (509) corresponds to two adjacent ports, and each communication groove (509) is configured to correspondingly communicate the two adjacent ports when the main shaft (507) rotates to a preset angle, so that the six ports form three groups of communication channels through the three communication grooves (509); The middle part of the main shaft (507) is positioned at the front part of the bearing (508) and is provided with a sealing ring (510) in a ring mode, and the sealing ring (510) is tightly attached between the main shaft (507) and the inner wall of the six-way valve housing (506) and is used for realizing dynamic sealing when the main shaft (507) rotates; A servo motor (501) and a speed reducer (502) are further arranged in the six-way valve housing (506), and the servo motor (501) is in driving connection with the tail end of the main shaft (507) through the speed reducer (502) and is used for driving the main shaft (507) to rotate so as to switch the communication state among ports; The six-way valve is characterized in that a six-way valve controller (503) is arranged outside the six-way valve housing (506) through a six-way valve bracket (504), and the six-way valve controller (503) is electrically connected with the servo motor (501) and is used for receiving control signals and driving the servo motor (501) to rotate to a preset angle.
4. The on-line quality control system for traditional Chinese medicine production according to claim 1, wherein a straight barrel filter (2), an inlet electromagnetic valve (3) and an inlet constant delivery pump (4) are sequentially installed on the sampling pipe, the straight barrel filter (2) comprises two layers of filter screens which are respectively 100 meshes and 200 meshes, a branch pipe for installing the sampling electromagnetic valve (6) is arranged on the circulating pipe, and a sampling beaker (7) is connected to an outlet of the branch pipe.
5. The on-line quality control system for Chinese medicine production according to claim 1, wherein the industrial personal computer (15) is further integrated with a database module for storing near infrared spectrum data, key quality attribute data, process parameter data and on-line detection control data.
6. An on-line detection method for producing Chinese medicine by using the on-line quality control system for producing Chinese medicine according to claim 5, comprising the steps of: S1, injecting liquid medicine into a constant temperature quantitative box (8), opening a sampling electromagnetic valve (6), after the injection of the constant temperature quantitative box (8) is completed, flowing the liquid medicine into a sampling beaker (7), completing off-line liquid medicine sampling, obtaining an off-line sample, synchronously collecting near infrared spectrum and high performance liquid chromatography data of the off-line sample, and establishing a corresponding relation model; s2, closing an inlet quantitative pump (4) and an inlet electromagnetic valve (3), and monitoring and regulating the temperature of the liquid medicine in a constant temperature quantitative box (8) through a constant temperature controller (9), and finishing the quantitative constant temperature process when the set temperature is reached; S3, starting a detection quantitative pump (10), injecting distilled water in an elution solvent bottle (11) into a constant temperature quantitative box (8), pushing liquid medicine in the constant temperature quantitative box (8) into a flow cell (12), starting a near infrared spectrometer (14), and collecting on-line near infrared spectrum data, wherein set parameters of the on-line near infrared spectrum data collecting process are completely the same as those of an off-line sample in collecting near infrared spectrum, so that on-line liquid medicine detection is completed; S4, a quality analysis module in the industrial personal computer (15) receives the online near infrared spectrum data, and outputs a key quality attribute real-time value after processing; s5, a control strategy module in the industrial personal computer (15) refers to data in a database module according to the real-time value of the key quality attribute and generates a control signal to control a traditional Chinese medicine production process parameter adjusting mechanism and dynamically adjust process parameters; S6, after data acquisition is completed, distilled water in the eluting solvent bottle (11) is injected into the constant-temperature quantitative box (8), the constant-temperature quantitative box (8) and the flow cell (12) are flushed by using the distilled water in the eluting solvent bottle (11), and the waste liquid is pushed into the waste liquid pool (13), so that the accuracy of next detection is guaranteed.
7. The method for on-line detection of Chinese medicine production according to claim 6, wherein in step S1, near infrared spectrum and high performance liquid chromatography data of an off-line sample are collected, and a corresponding relation model is established, and the method specifically comprises the following steps: dividing the off-line sample into two parts after filtering, respectively sealing, wherein the two parts of off-line sample are respectively used for collecting near infrared spectrum data and high performance liquid chromatography data; preparing a reference substance solution as a reference substance, setting concentration gradients, collecting high performance liquid chromatography data under different concentration gradients, recording a chromatogram according to chromatographic conditions, taking the peak area of the reference substance as an ordinate, taking the concentration of the reference substance solution as an abscissa, drawing a standard curve, determining a correlation coefficient, measuring key quality attributes, corresponding to near infrared spectrum data, and inputting the key quality attributes into a database module for calling by a control strategy module.
8. The on-line detection method for Chinese medicine production according to claim 7, wherein the concentration gradient of the standard solution is 0.0025mg/mL, 0.005mg/mL, 0.0125mg/mL, 0.025mg/mL, 0.05mg/mL, 0.125mg/mL, 0.25mg/mL, 0.375mg/mL.
9. The on-line detection method for Chinese medicine production according to claim 7, wherein in step S4, the processing of the near infrared spectrum data comprises the steps of: s41, performing three-time Hermite spline interpolation pretreatment on the online near infrared spectrum data, and taking the pretreated online sample spectrum data as a training input sample of the VAE; S42, near infrared spectrum data of an off-line sample corresponding to the on-line near infrared spectrum data is taken and input into a VAE for training together with the on-line sample spectrum data preprocessed in the step S41 and a preset loss function so as to obtain a trained VAE generation model; s43, inputting online near infrared spectrum data from a test data set into a trained VAE generation model to obtain generated near infrared spectrum data, and inputting the generated near infrared spectrum data into a PLS regression layer for predicting key quality attributes to obtain a key quality attribute predicted value; S44, preprocessing the offline near infrared spectrum data in the test data set through ridge regression, then inputting the data into a PLS regression layer, and determining optimal model parameters through the results to obtain a key quality attribute prediction result; S45, storing the key quality attribute prediction result obtained in the step S44 into a database module for being called by a control strategy module to adjust the production process parameters of the traditional Chinese medicine.

Description

On-line detection method and quality control system for traditional Chinese medicine production Technical Field The invention belongs to the technical field of detection and analysis control and regulation, in particular relates to a detection and regulation system in the production process of traditional Chinese medicines, and specifically relates to an online detection method and a quality control system for traditional Chinese medicine production. Background The key quality attribute is an important parameter of the production quality of the traditional Chinese medicine, and most of detection modes are sampling detection or terminal detection. In the prior art, the traditional Chinese medicine production is mostly carried out by adopting a mode of fixing technological parameters, and the problems of poor quality stability and uniformity of traditional Chinese medicine products still exist although the production efficiency is improved to a certain extent. At present, a small amount of online detection systems are applied to the traditional Chinese medicine production link, but the online detection systems mainly depend on large-flow external circulation, the collected detection sample quantity is large, the detection stability is poor, the efficiency is low, the waste of products is easily caused, and the real-time detection and control of key quality attributes in the traditional Chinese medicine production process are not facilitated. In the actual production process, the traditional Chinese medicine production process involves more and more complex links, and the traditional detection method is difficult to meet the technical requirements on online monitoring in the current production process. The non-contact analysis technology represented by near infrared spectrum, raman spectrum, mid-infrared spectrum and the like gradually becomes a widely adopted technical method in the current online monitoring, and also gradually becomes an important development direction of the online monitoring. In practical application, the most suitable spectrum method is selected according to the specific state of the materials, so that the quality of the obtained data is ensured. The near infrared spectrum technology has the advantages of non-invasiveness and quick response, can perform qualitative and quantitative analysis on key quality attributes of the traditional Chinese medicine, has good application potential, and improves the applicability in the production link of the traditional Chinese medicine by diversified sampling modes. However, the existing near infrared spectrum technology still faces a plurality of technical bottlenecks in on-line detection of traditional Chinese medicine production, and is mainly embodied in the following four aspects: 1. the near infrared spectrum technology is extremely sensitive to an online detection environment, and factors such as temperature and humidity fluctuation, vibration, ambient light interference and the like can obviously influence the stability and the signal to noise ratio of a spectrum signal; 2. In order to ensure stable detection conditions, the liquid medicine to be detected is always required to be maintained in a relatively static state for a long time, so that the efficiency of real-time detection is severely restricted; 3. Because the components of the traditional Chinese medicine system are complex, the spectrum overlap among the components is serious, and a steady and movable quantitative model is difficult to build, so that the prediction precision of key quality attributes is difficult to guarantee; 4. how to realize closed-loop control and self-adaptive optimization of process parameters based on near infrared spectrum data, no mature and reliable solution is formed in the aspects of algorithm integration and engineering implementation at present. Therefore, developing a traditional Chinese medicine production process online detection system which is low in consumption, high in efficiency, high in adaptability and capable of realizing real-time detection and self-adaptive quality control has become a technical problem to be solved in the field. Disclosure of Invention The invention provides an online detection method and a quality control system for traditional Chinese medicine production, which are used for solving the problems that the detection mode of key quality attributes in the traditional Chinese medicine production process is lagged and uncontrollable, the detection system is low in efficiency and is easy to cause waste, the near infrared online detection technology with prospect is easy to interfere in practical application, has high environmental requirements, is difficult to face the spectrum overlapping of a complex traditional Chinese medicine system, is difficult to establish a steady and movable quantitative model, and the closed-loop control technology is not mature. The invention is realized by adopting the following technical scheme: th