CN-122017112-A - Method for evaluating quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum

CN122017112ACN 122017112 ACN122017112 ACN 122017112ACN-122017112-A

Abstract

The invention discloses a method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification with a characteristic spectrum, which comprises the following steps of constructing a constant temperature and constant humidity control area around a mobile phase system before continuously evaluating the quality of Tianyuan zhitong particles, integrally sealing a liquid storage bottle, a sample injection pipeline and a pump head in a temperature and humidity balance space, maintaining a detection environment steady state by dynamically adjusting a temperature difference and a humidity difference, arranging a charge neutralization device on a mobile phase input path in the constant temperature and humidity control area, and releasing static electricity accumulation energy through a high-impedance grounding guide path to keep the potential balance of the liquid storage bottle and the sample injection path. The invention controls the stability of a mobile phase through constant temperature and humidity, charge neutralization and ion capturing, avoids peak position drift caused by metal ion disturbance, maintains chromatographic balance through micro-flow speed pulsation and peak position dynamic compensation, realizes consistent peak position stability and component identification in continuous detection, and improves the accuracy and reliability of Tianyuan zhitong particle quality evaluation.

Inventors

WANG JINYU
LI XINJIAN
LIU YING
YI HONG
CHENG YI
LIU DEWEN
TONG YAN

Assignees

中国中医科学院中药研究所

Dates

Publication Date: 20260512
Application Date: 20260313

Claims (10)

1. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum is characterized by comprising the following steps of: before continuous quality evaluation of Tianyuan zhitong particles, a constant temperature and humidity control area is built around a mobile phase system, a liquid storage bottle, a sample injection pipeline and a pump head are integrally sealed in a temperature and humidity balance space, and a steady detection environment is maintained by dynamically adjusting a temperature difference and a humidity difference; setting a charge neutralization device on a mobile phase input path in a constant temperature and humidity control area, releasing static electricity accumulation energy through a high-impedance grounding guide path, and keeping the potential balance of a liquid storage bottle and a sample introduction path; setting a dynamic ion capturing device at the inlet of the mobile phase under the condition of potential balance, adopting a high specific surface inert adsorption matrix to adsorb transient free ions, and stabilizing ion adsorption behavior by depending on the potential balance environment; Step four, under the stable state of ion concentration, micro-flow speed pulsation control is implemented in the process of conveying the mobile phase, and the time balance of adsorption dynamics of the chromatographic stationary phase is maintained by periodically adjusting the micro-flow speed to act on the output liquid flow of the mobile phase; And fifthly, after the mobile phase conveying is stable, establishing a peak position dynamic tracking compensation mechanism, generating an offset reference interval based on the retention time distribution of the previous detection period, and executing synchronous fine adjustment on the retention time of the current detection period.
2. The method for evaluating the quality of the Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 1, wherein the step of constructing a constant temperature and humidity control region around a mobile phase system before performing continuous quality detection evaluation on the Tianyuan zhitong particles comprises the following steps: before continuous detection, the liquid storage bottle, the sample injection pipeline and the pump head are sealed in a sealed temperature-humidity balance space, the space is made of double-layer corrosion-resistant insulating materials, an annular airflow channel is arranged in the space, and air subjected to temperature-humidity adjustment is conveyed through an external air circulation device to form continuous flowing thin-layer airflow on the surfaces of the liquid storage bottle, the sample injection pipeline and the pump head; after the closed space is established, the dynamic balance regulation and control of the internal temperature and humidity of the space are carried out through an external constant temperature circulating device and a humidity regulating cavity, and the gas distribution is controlled to be uniform; Under the condition of temperature-humidity balance space stability, an isothermal connecting pipeline is arranged between an outlet of a liquid storage bottle and an inlet of a sample injection pipe, the pipeline comprises a polytetrafluoroethylene inner layer and a high-heat-conductivity metal outer layer, and the temperature of the outer layer and the temperature of air are kept balanced through a thermal convection effect; Under the condition of establishing a temperature-humidity balance environment, the steady state of a closed space is maintained through air flow rate adjustment and heat exchange rate regulation, and the liquid storage bottle, the sample injection pipeline and the pump head are controlled to be in the same temperature-humidity condition.
3. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification with characteristic patterns according to claim 2, wherein the step of disposing a charge neutralizing device in a mobile phase input path in a constant temperature and humidity control region comprises: A charge guide layer is arranged outside a mobile phase input path in the constant temperature and humidity control area, the charge guide layer is made of a composite conductive material with high dielectric strength and stable surface resistance, and the charge guide layer continuously covers along the outer wall of the mobile phase input path and penetrates through an outlet of a liquid storage bottle, a connection part of a sample injection pipe and an inlet of a pump head; a high-impedance grounding guide path is arranged on the extending path of the charge guide layer, the guide path is made of a high-molecular conductive composite material, conductive particles are contained in the guide path to control the resistance range, and two ends of the guide path are respectively connected with the tail end of the guide layer and an external ground potential layer; arranging a plurality of pressure equalizing contact points in a constant temperature and humidity control area, forming an equipotential surface between the pressure equalizing contact points and the charge guiding layer, and constructing a continuous potential conduction network among the liquid storage bottle, the sample injection pipeline and the pump head; Under the formation condition of the potential balance environment, charge diffusion is realized through the antistatic coating on the surface of the guide layer, retained charges move into a high-impedance guide passage along the surface of the guide layer, the static zero accumulation state in the constant temperature and humidity environment is maintained, and the concentration of metal ions in the mobile phase is stabilized.
4. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 3, wherein the step of arranging a dynamic ion capturing device at the inlet of the mobile phase under the condition of potential equalization comprises the following steps: Establishing a high specific surface inert adsorption matrix structure for ion adsorption at a mobile phase inlet in a constant temperature and humidity and potential balance environment, wherein the adsorption matrix is made of an inert inorganic material with a three-dimensional porous framework, and the surface is subjected to plasma treatment to remove active functional groups and is encapsulated in a shell with a fluid distribution channel; a temperature conducting layer is arranged outside the high specific surface inert adsorption matrix, the temperature of an adsorption area is kept constant through constant temperature liquid circulation, and a low-speed micro-circulation fluid channel is arranged around the adsorption matrix; The adsorption device is provided with a fluid guide layer consisting of porous flow dividing plates which are arranged at the upper end and the lower end of the adsorption matrix and are combined with the adsorption matrix in a flexible crimping manner; Under the condition of stable adsorption behavior, the flow velocity distribution is controlled by adjusting the inlet pressure and the outlet back pressure of the mobile phase, and the steady state of an adsorption area is maintained by matching with a constant temperature and humidity environment, so that the adsorption and release of metal ions by the adsorption matrix are dynamically balanced.
5. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 4, wherein the pore distribution density of a three-dimensional porous skeleton of a high specific surface inert adsorption matrix is controlled to be in a range from micron to nanometer, a heat conducting ring is arranged outside a temperature conducting layer for uniformly distributing heat of a constant temperature liquid circulation layer, the pore diameter of an upper-layer splitter plate of a fluid guiding layer is larger than that of a lower-layer splitter plate, and the adsorption matrix is connected with a potential balance network.
6. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 4, wherein the step of performing micro-flow pulsation control on the mobile phase delivery process in the steady state of ion concentration comprises: A liquid conveying structure capable of carrying out micro-amplitude flow speed adjustment is established under the condition of stable ion concentration, the liquid conveying structure consists of a high-precision driving device and a controllable elastic liquid storage cavity, and a temperature control layer is coated outside the elastic liquid storage cavity and keeps constant temperature through constant-temperature liquid circulation; A multistage pressure buffer unit is arranged in a mobile phase passage under the condition of establishing a micro-amplitude flow speed controllable structure, and the pressure buffer unit is composed of a fine spiral liquid channel so as to diffuse flow speed fluctuation and form uniform and coordinated micro-amplitude pulsation characteristics; Adjusting the shear rate of the stationary phase surface and controlling the thickness of the boundary layer through periodic flow fluctuation under the condition of stable flow velocity pulsation waveform so as to maintain time balance of adsorption and desorption processes and inhibit transient complex reaction; and under the condition of establishing equilibrium of adsorption dynamics, the pulsation stability is maintained by synchronously adjusting the pumping frequency of the mobile phase and the elastic recovery rate of the liquid storage cavity, and the flow rate period is kept consistent under the condition of constant temperature and constant humidity.
7. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 6, wherein in the micro-flow pulsation control process, a temperature control layer coated outside an elastic liquid storage cavity is made of a metal film with high heat conduction performance, and when an outlet of the liquid storage cavity is connected with a main conveying pipeline, fluid forms micro-flow fluctuation when passing through the liquid storage cavity and acts on mobile phase output liquid flow.
8. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 7, wherein in the micro-flow pulsation control process, a temperature control layer coated outside an elastic liquid storage cavity is made of a metal film with high heat conduction performance, and when an outlet of the liquid storage cavity is connected with a main conveying pipeline, fluid forms micro-flow fluctuation when passing through the liquid storage cavity and acts on mobile phase output liquid flow.
9. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 7, wherein the step of establishing a peak position dynamic tracking compensation mechanism after the mobile phase delivery is stable comprises the following steps: After the stable conveying of the mobile phase is completed, carrying out retention time distribution analysis on the chromatogram of the previous detection period to determine a peak position reference standard of the current period, and determining reference data according to a peak shape distribution range, a peak area and signal intensity; After the retention time reference distribution diagram is established, an offset reference interval is generated according to the time interval and peak shape characteristics of each chromatographic peak, the interval is generalized according to the relative change trend of the retention time of each peak in the previous period, and the stability of a mobile phase conveying path, the column temperature differential and the micro flow velocity pulsation waveform change are considered; After the offset reference interval is established, carrying out real-time synchronous fine adjustment on the chromatographic retention time of the current detection period, wherein the synchronous fine adjustment realizes peak position time correction by adjusting the micro-amplitude pulsation period of the mobile phase conveying rate; after the peak position synchronous fine tuning is finished, the peak position time data of the current period is automatically compared with the reference interval by continuously maintaining a peak position dynamic tracking compensation mechanism, and the boundary of the offset reference interval of the next detection period is updated.
10. The method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum according to claim 9, wherein when a peak position dynamic tracking compensation mechanism operates in a continuous detection period, an offset reference interval is updated based on the retention time distribution of a previous detection period, and synchronous fine tuning is performed on the retention time of a chromatographic peak of the current detection period on the premise that a constant temperature and humidity control area, potential balance conditions and micro-flow rate pulsation control states are kept unchanged.

Description

Method for evaluating quality of Tianyuan zhitong particles by combining thin-layer chromatography identification and characteristic spectrum Technical Field The invention relates to the technical field of mineral screening, in particular to a method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification with characteristic patterns. Background The Tianyuan zhitong is a compound prescription composed of ten traditional Chinese medicines of gastrodia tuber, szechuan lovage rhizome, dahurian angelica root, vinegar-processed corydalis tuber, paniculate swallowwort root, wild jujube seed, chinese angelica, fructus viticis, processed morinda root, purified pinellia tuber and the like, has the effects of dispelling wind and relieving pain, calming liver and suppressing yang, tranquillizing and improving intelligence, and is mainly used for treating tension headache, anxiety, insomnia and other accompanying symptoms. The quality evaluation of the granule is characterized in that the thin layer chromatography is used for qualitatively identifying main medicinal herbs in a prescription, such as ligusticum wallichii, angelica sinensis, rhizoma corydalis with vinegar, paniculate swallowwort root and semen zizyphi spinosae, the authenticity and the integrity of medicinal material components are confirmed through the definition and the specificity of characteristic spots, the characteristic chromatography is used for carrying out integral chemical component analysis on a sample through high performance liquid chromatography, 9 common peaks are extracted, key components such as ferulic acid, paeonol, ligustilide and the like are identified, and the consistency between batches is reflected by the chemical composition characteristics of the preparation. The two components are combined to form a quality control system of the system, so that the sources of medicinal materials are verified, the stability and the repeatability of the Tianyuan zhitong granule preparation are ensured, and scientific basis is provided for the industrial production and clinical application of the Tianyuan zhitong granule preparation. The prior art has the following defects: In the continuous quality evaluation and evaluation process of Tianyuan zhitong particles, a mobile phase system is easily influenced by temperature and humidity changes of an experimental environment or static accumulation of a liquid storage bottle under long-term operation, so that trace metal ions are suddenly increased in a short time. When the concentration of metal ions is accumulated to a critical threshold in a detection passage, transient complex reaction is generated with a chromatographic column stationary phase, so that the integral retention time of a chromatographic peak is synchronously shifted, and the phenomenon of uneven peak position drift or integral dislocation is caused. Such drift is generally difficult to identify in real time through conventional baseline correction, is very easy to be misjudged by a system as all main components of the medicinal materials are subjected to 'failure detection' or content abnormal reduction, so that serious deviation occurs in a batch quality assessment result, and even misjudgment on preparation stability and process consistency is caused. The above information disclosed in the background section is only for enhancement of understanding of the background of the disclosure and therefore it may include information that does not form the prior art that is already known to a person of ordinary skill in the art. Disclosure of Invention The invention aims to provide a method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification with characteristic patterns, so as to solve the problems in the prior art. In order to achieve the above purpose, the invention provides a method for evaluating the quality of Tianyuan zhitong particles by combining thin-layer chromatography identification with characteristic patterns, which comprises the following steps: Before continuous quality evaluation of Tianyuan zhitong particles, a constant temperature and humidity control area is built around a mobile phase system, a liquid storage bottle, a sample injection pipeline and a pump head are integrally sealed in a temperature and humidity balance space, and a detection environment is maintained to be stable by dynamically adjusting a temperature difference and a humidity difference so as to stabilize the concentration of metal ions in the mobile phase; setting a charge neutralization device on a mobile phase input path in a constant temperature and humidity control area, releasing static electricity accumulation energy through a high-impedance grounding guide path, keeping the potential balance of a liquid storage bottle and a sample introduction path, and inhibiting the transient increase of the concentration of metal ions caused by p