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CN-122006292-A - Flow real-time monitoring method and system for At-211 column separation process

CN122006292ACN 122006292 ACN122006292 ACN 122006292ACN-122006292-A

Abstract

The invention relates to the technical field of flow monitoring and discloses a flow real-time monitoring method and a flow real-time monitoring system for an At-211 column separation process, wherein the method comprises the steps of collecting the conductivity of eluent in an outlet pipeline of an At-211 chromatographic column in real time, and continuously analyzing the conductivity to generate a state mark; wherein, when detecting that the eluent is switched to the absolute ethanol phase, the state mark is valid; and the method and the device accurately judge the switching time of the absolute ethyl alcohol phase by collecting the conductivity and generating the state mark, analyze the collected pressure time sequence data to generate a steady-state pressure value, then analyze the pressure time sequence data for the second time to obtain a pressure memory value, comprehensively capture the continuous influence of the pressure steady state and the flow, finally generate a flow stability index, and evaluate the flow state of the whole elution process of the alcohol phase.

Inventors

  • GU LONG
  • Su Xingkang
  • WANG GUAN
  • HUANG HUA

Assignees

  • 福建睿斯科医疗技术有限公司

Dates

Publication Date
20260512
Application Date
20260413

Claims (10)

  1. The real-time flow monitoring method for the separation process of the at-211 column is characterized by comprising the following steps: Step S1, collecting the conductivity of eluent in an outlet pipeline of an At-211 chromatographic column in real time, and continuously analyzing the conductivity to generate a state mark; when detecting that the eluent is switched into the absolute ethyl alcohol phase, the state mark is valid, otherwise, the state mark is invalid; Step S2, when the state mark is valid, continuously acquiring the pressure of the eluent in the outlet pipeline in real time to obtain pressure time sequence data, and performing steady-state analysis on the pressure time sequence data to generate a steady-state pressure value representing the pressure level in the current steady flow state; Step S3, when the state mark is valid, performing secondary analysis on the pressure time sequence data to obtain a pressure memory value representing the continuous influence of the flow on the current pressure; And S4, analyzing the steady-state pressure value and the pressure memory value to generate a flow stability index for evaluating the flow state in the whole ethanol phase elution process.
  2. 2. The method for monitoring flow rate in real time in an At-211 column separation process according to claim 1, wherein the continuous analysis of conductivity to generate a status flag comprises: analyzing the conductivity to generate a reference conductivity and a control upper limit value; and calculating the deviation degree of the conductivity relative to the reference conductivity, calculating the first derivative of the deviation degree changing along with time, and fusing the deviation degree and the first derivative to generate a phase change response factor reflecting the deviation amplitude and the rapid change.
  3. 3. The method for monitoring flow rate in real time during an At-211 column separation process according to claim 2, wherein the conductivity is continuously analyzed to generate a status flag, further comprising: Analyzing the phase change response factor, and calculating the concentration degree of the phase change response factor to obtain a drift stability index; performing cooperative calculation on the reference conductivity and the control upper limit value to generate a dynamic phase change threshold; If the drift stability index is continuously lower than the dynamic phase change threshold, judging that the eluent is switched into the absolute ethanol phase, and generating a state mark as valid, otherwise, judging as invalid.
  4. 4. The method for monitoring flow rate in real time during an At-211 column separation process of claim 1, wherein performing steady state analysis on the pressure timing data to generate a steady state pressure value indicative of a pressure level At a current steady flow state comprises: arranging the continuously collected pressures according to the collection time to form pressure time sequence data; carrying out phase space reconstruction on the pressure time sequence data, identifying attractor structures in the phase space, and calculating pressure micelle distribution entropy of the volume evolution of each attractor structure along with time; And analyzing gradient change of pressure micelle distribution entropy, dividing pressure segments, calculating similarity of all attractor structures in each pressure segment, and generating evolution consistency factors.
  5. 5. The method for monitoring flow rate in real time during an At-211 column separation process of claim 4, wherein steady state analysis of pressure timing data generates a steady state pressure value indicative of a pressure level At a current steady flow state, further comprising: screening out a convergence pressure section based on the evolution consistency factor, and analyzing to generate a pressure backbone sequence; And calculating the convergence degree according to the pressure base stem sequence, and calibrating the pressure base stem sequence according to the convergence degree to generate a steady-state pressure value representing the pressure level in the current steady-state flow state.
  6. 6. The method for monitoring flow rate in real time in an At-211 column separation process according to claim 5, wherein when the status flag is valid, performing a secondary analysis on the pressure timing data to obtain a pressure memory value indicating a continuous influence of the flow rate on the current pressure, comprising: analyzing pressure fluctuation in the pressure time sequence data in the condition that the state mark is effective time, and generating a pressure mark vector representing the pressure dynamic fluctuation; And analyzing the pressure imprinting vector to find out the difference between different pressure values and generate a residual image attenuation value of the pressure residual intensity.
  7. 7. The method for monitoring flow rate in real time in an At-211 column separation process according to claim 6, wherein when the status flag is valid, performing a secondary analysis on the pressure time series data to obtain a pressure memory value indicating a continuous influence of the flow rate on the current pressure, further comprising: and fusing the pressure imprinting vector and the ghost attenuation value to generate a pressure memory value representing the continuous influence of the flow on the current pressure.
  8. 8. The method for monitoring flow rate in real time during an At-211 column separation process according to claim 7, wherein analyzing based on steady-state pressure values and pressure memory values generates a flow rate stability index that evaluates flow rate conditions during an entire ethanol phase elution process, comprising: and analyzing the adaptation degree of the steady-state pressure value and the pressure memory value, and generating a memory adaptation factor which represents the synergy degree of the steady pressure and the continuous influence of the flow.
  9. 9. The method for monitoring flow rate in real time during an At-211 column separation process according to claim 8, wherein analyzing based on steady-state pressure values and pressure memory values generates a flow rate stability index that evaluates flow rate conditions during an entire ethanol phase elution process, further comprising: based on the pressure memory adaptation factor, calculating the dynamic influence weight of the flow on the pressure state to obtain the flow pressure association weight; And performing cooperative calculation on the steady-state pressure value, the pressure memory value, the flow pressure association weight and the pressure memory adaptation factor to generate a flow stability index for evaluating the flow state in the whole ethanol phase elution process.
  10. A real-time flow monitoring system for at-211 column separation process, applied to the monitoring method as claimed in any one of claims 1-9, comprising: The state analysis unit is used for collecting the conductivity of the eluent in the outlet pipeline of the At-211 chromatographic column in real time, and continuously analyzing the conductivity to generate a state mark; when detecting that the eluent is switched into the absolute ethyl alcohol phase, the state mark is valid, otherwise, the state mark is invalid; The pressure analysis unit is used for continuously collecting the pressure of the eluent in the outlet pipeline in real time when the state mark is valid to obtain pressure time sequence data, and performing steady-state analysis on the pressure time sequence data to generate a steady-state pressure value representing the pressure level in the current steady flow state; the influence analysis unit is used for carrying out secondary analysis on the pressure time sequence data when the state mark is valid to obtain a pressure memory value which indicates the continuous influence of the flow on the current pressure; And the flow judgment unit is used for analyzing the steady-state pressure value and the pressure memory value and generating a flow stability index for evaluating the flow state in the whole ethanol phase elution process.

Description

Flow real-time monitoring method and system for At-211 column separation process Technical Field The invention relates to the technical field of flow monitoring, in particular to a flow real-time monitoring method and system for an At-211 column separation process. Background In the separation process of an At-211 extraction chromatographic column, particularly in the absolute ethyl alcohol elution stage, a conductivity monitoring mode is generally adopted At present, a conductivity monitoring threshold is set based on an aqueous phase acid system, the real-time monitoring of the flow of eluent is realized through the continuity of a conductivity signal, and the stability of the flow of the eluent is further indirectly judged. However, the monitoring mode has the following defects that the core eluent separated from the At-211 extraction chromatographic column is absolute ethyl alcohol, the conductivity of the core eluent is far lower than that of an aqueous-phase acid solution, the conductivity signal suddenly drops below a monitoring threshold value after an alcohol phase enters a detection flow path, an effective conductivity signal cannot be captured, the instantaneous flow calculation is invalid, the state of the flow of the eluent is difficult to evaluate through the signal continuity of the conductivity, and the accuracy of flow monitoring in the elution process is influenced. Disclosure of Invention Aiming At the defects of the prior art, the invention provides a method and a system for monitoring the flow of an At-211 column separation process in real time, which solve the problems. The technical aim of the invention is realized by the following technical scheme: the real-time flow monitoring method for the separation process of the At-211 column comprises the following steps: Step S1, collecting the conductivity of eluent in an outlet pipeline of an At-211 chromatographic column in real time, and continuously analyzing the conductivity to generate a state mark; when detecting that the eluent is switched into the absolute ethyl alcohol phase, the state mark is valid, otherwise, the state mark is invalid; Step S2, when the state mark is valid, continuously acquiring the pressure of the eluent in the outlet pipeline in real time to obtain pressure time sequence data, and performing steady-state analysis on the pressure time sequence data to generate a steady-state pressure value representing the pressure level in the current steady flow state; Step S3, when the state mark is valid, performing secondary analysis on the pressure time sequence data to obtain a pressure memory value representing the continuous influence of the flow on the current pressure; And S4, analyzing the steady-state pressure value and the pressure memory value to generate a flow stability index for evaluating the flow state in the whole ethanol phase elution process. Further, the conductivity is continuously analyzed to generate a status flag, including: analyzing the conductivity to generate a reference conductivity and a control upper limit value; and calculating the deviation degree of the conductivity relative to the reference conductivity, calculating the first derivative of the deviation degree changing along with time, and fusing the deviation degree and the first derivative to generate a phase change response factor reflecting the deviation amplitude and the rapid change. Further, the continuous analysis of the conductivity generates a status flag, further comprising: Analyzing the phase change response factor, and calculating the concentration degree of the phase change response factor to obtain a drift stability index; performing cooperative calculation on the reference conductivity and the control upper limit value to generate a dynamic phase change threshold; If the drift stability index is continuously lower than the dynamic phase change threshold, judging that the eluent is switched into the absolute ethanol phase, and generating a state mark as valid, otherwise, judging as invalid. Further, performing a steady state analysis on the pressure timing data to generate a steady state pressure value indicative of a pressure level at a current steady flow state, comprising: arranging the continuously collected pressures according to the collection time to form pressure time sequence data; carrying out phase space reconstruction on the pressure time sequence data, identifying attractor structures in the phase space, and calculating pressure micelle distribution entropy of the volume evolution of each attractor structure along with time; And analyzing gradient change of pressure micelle distribution entropy, dividing pressure segments, calculating similarity of all attractor structures in each pressure segment, and generating evolution consistency factors. Further, performing a steady state analysis on the pressure timing data to generate a steady state pressure value indicative of a pressure level at a current steady flow