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CN109682776A - Multimode near infrared online monitors system and its application method - Google Patents

Multimode near infrared online monitors system and its application method Download PDF

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Publication number
CN109682776A
CN109682776A CN201811459678.0A CN201811459678A CN109682776A CN 109682776 A CN109682776 A CN 109682776A CN 201811459678 A CN201811459678 A CN 201811459678A CN 109682776 A CN109682776 A CN 109682776A
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valve
equipment
near infrared
medical fluid
measured
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金叶
吴永江
刘雪松
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Zhejiang University ZJU
Lishui University
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Zhejiang University ZJU
Lishui University
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Priority to CN201811459678.0A priority Critical patent/CN109682776A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

It include duplex strainer, frequency conversion impeller pump, optical fiber and detection components the invention discloses a kind of multimode near infrared online monitoring system and its application method, the system;The input terminal of duplex strainer pass through respectively the first liquid feed valve, the second liquid feed valve accordingly with fill the equipment A of medical fluid to be measured, equipment B is connect, output end is connect with the input terminal of frequency conversion impeller pump;The output end of frequency conversion impeller pump is connect with detection components;Detection components, for eliminating turbulent flow and bubble in medical fluid to be measured, the output end of detection components passes through the first liquid valve respectively, the second liquid valve is connect with accordingly equipment A, equipment B;Optical fiber is connected between the detection components and On-line NIR analyzer.The present invention automatically acquires spectrum including dynamic, static mode, and especially static acquisition mode is completely eliminated influence of the turbulent flow near infrared spectrum baseline, increases substantially near infrared online monitoring accuracy, promotes the promotion and application of near infrared online detection technology.

Description

Multimode near infrared online monitors system and its application method
Technical field
The present invention relates to online measuring technique fields, and in particular to a kind of multimode near infrared online monitoring system and its answers Use method.
Background technique
Near-infrared spectral analysis technology have spectra collection is convenient, analysis time is short, do not destroy sample, do not consume reagent, It the advantages that free from environmental pollution, can be completed by mathematical modeling to the multiple determination of complex system, be gradually widely used in Medicine produces the real-time analysis of each Key Quality link.
Have Patents documents about application of the near-infrared spectral analysis technology in Chinese medicine production Quality Control field at present, Such as patent " a kind of DANHONG ZHUSHEYE double effect concentration process online test method (CN201410135322.7) ", " honeysuckle concentration Process clearance detection method (CN201510177436.2) in real time online ", a kind of " DANHONG ZHUSHEYE alcohol precipitation process on-line checking side Method (CN201210070474.4) " etc..Above-mentioned each patent using industrial conventional on-line measuring device, including flow cell, Fibre-optical probe etc., there is no the measures such as the filtering de-bubble for taking the medical fluid of on-line checking profession and flow adjusting.Due in The particularity of medicine production object, such as insoluble solid particle is more in medical fluid, it is unstable to be also easy to produce a large amount of foams, flow velocity, directly Near infrared spectra collection is influenced, leads to exception, mistake spectrum and the frequent generation of baseline drift, not can guarantee the steady of spectra collection Qualitative and model built accuracy and reliability.In order to eliminate solid impurity, foam, temperature to the shadow of near infrared spectrum It rings, patent " a kind of near infrared online detection pretreatment system and its apply (CN201110093881.2) " design is to medical fluid to be measured De-bubble, temperature control, flow control, spectra collection, sample collection and clear are filtered to liquid automatically according to setup parameter Blowdown etc. is washed, although spectrum stability is substantially improved, but still can not eliminate influence of the turbulent flow to spectrum.
Near-infrared is individually equipped with a set of close red for Chinese Traditional Medicine quality control generally every production equipment at present Outer on-line measuring device (flow cell), testing cost is larger.In addition, by inquiry existing literature, existing near infrared online inspection Survey case be not implemented prediction result feedback control, can not really realize the online real-time monitoring of production process, with really it is right The quality monitoring of production process still has relatively large distance.
Summary of the invention
In order to solve the above-mentioned technical problem, the present invention proposes that a kind of multimode near infrared online monitors system and its application side Method, including dynamic, static mode automatically acquire spectrum, more production equipments share on-line monitoring system, on-line monitoring fructufy When feedback and regulation, integrated cleaning and the functions such as blowdown, can be used for the whole-course quality control of more production equipments, realization is closely red External spectrum data and automatic control system linkage, on-line monitoring result can directly feed back to automatic control system, really real The online real-time monitoring of existing production process.The problems such as to solve the repeatability of spectra collection, stability and poor reliability, the present invention Static and dynamic spectrum acquisition mode is designed simultaneously, and turbulent flow is completely eliminated near infrared spectrum in especially static acquisition mode The influence of baseline increases substantially near infrared online monitoring accuracy, promotes the promotion and application of near infrared online detection technology.
To achieve the goals above, one aspect of the present invention provides a kind of multimode near infrared online monitoring system, should System includes duplex strainer, frequency conversion impeller pump, optical fiber and detection components;
The input terminal of the duplex strainer pass through respectively the first liquid feed valve, the second liquid feed valve accordingly with fill medicine to be measured The equipment A of liquid, equipment B connection, output end are connect with the input terminal of frequency conversion impeller pump;
The output end of the frequency conversion impeller pump is connect with detection components, for by the medical fluid pumping to be measured in relevant device extremely In detection components;
The detection components, for eliminating turbulent flow and bubble in medical fluid to be measured, the output end difference of the detection components It is connect by the first liquid valve, the second liquid valve with accordingly equipment A, equipment B, medical fluid to be measured is transmitted back in original equipment;
The optical fiber is connected between the detection components and On-line NIR analyzer, and being used for will be to detection group The infrared spectroscopy testing result of medical fluid to be measured is transmitted to On-line NIR analyzer in part.
Preferably, the detection components include bubble filter, it is circulating valve, first switch valve, electromagnetic flowmeter, visual Flow cell, air valve and second switch valve;
The bubble filter is connect with one end of frequency conversion impeller pump, circulating pump and first switch valve respectively, and described first The other end of switch valve is connect with the electromagnetic flowmeter;
The electromagnetic flowmeter, the visual flow cell, the air valve and the second switch valve are sequentially connected with;
One end of the optical fiber is connect with the visual flow cell, and the other end connects the On-line NIR analysis Instrument.
Preferably, connecting sample tap by sampling valve between the first switch valve and the visual flow cell.
Preferably, stainless steel filtration core is detachably provided in the bubble filter, by filtered medicine to be measured Liquid is flowed out from the lower end of bubble filter, flows into electromagnetic flowmeter by first switch valve.
Preferably, first liquid feed valve, the second liquid feed valve, the first liquid valve, the second liquid valve, first switch valve, Second switch valve, circulating valve, air valve and sampling valve are all made of pneumatic diaphragm valve.
Preferably, first liquid feed valve, the second liquid feed valve, the first liquid valve, the second liquid valve, first switch valve, Second switch valve, circulating valve, air valve and sampling valve pass through gas source pipe and connect with air compressor.
Another aspect of the present invention provides and a kind of applies the more of multimode near infrared online as described above monitoring system Module near infrared online monitoring method is dynamic acquisition mode, includes the following steps:
The corresponding liquid feed valve of equipment where opening medical fluid to be measured and liquid valve;
First switch valve and second switch valve are opened, circulating valve, sampling valve and air valve is closed, is made by frequency conversion impeller pump Medical fluid to be measured is to stablize flow velocity by visual flow cell, the infrared spectroscopy of medical fluid to be measured in the visual flow cell of collecting fiber, and will Infrared spectroscopy information is transmitted to infrared spectrometric analyzer;
First switch valve, second switch valve, sampling valve and air valve are opened, circulating valve is closed, acquires sample from sample tap.
Another aspect of the invention provides and a kind of applies the more of multimode near infrared online as described above monitoring system Module near infrared online monitoring method includes the following steps: for static acquisition mode
The corresponding liquid feed valve of equipment where opening medical fluid to be measured and liquid valve;
First switch valve, second switch valve, circulating valve are opened, sampling valve, air valve is closed, makes flushing detection components to be measured Pipeline;
First switch valve, second switch valve are closed, circulating valve is opened, medical fluid to be measured in flow cell is made to remain static, Bubble floating simultaneously, acquires near infrared spectrum in medical fluid quiescing process to be measured, remaining medical fluid is returned by pipeline where circulating valve Return corresponding equipment;
Sampling valve and air valve are opened, receives medical fluid to be measured after sample tap outflow under atmospheric pressure and gravity Collection;
After completing infrared spectroscopy acquisition and sample acquisition, first switch valve and second switch valve are opened, circulating valve is closed, makes Medical fluid to be measured is flow back into original equipment.
Another aspect of the invention provides a kind of storage medium, and computer program is stored in the storage medium, described Computer program realizes multimode near infrared online monitoring method as described above in execution processed.
Compared with prior art, the invention has the benefit that
Technical effect of the invention: from the angle for saving cost, multiple production equipments is solved and share a set of on-line monitoring system The practical problem of system.Spectra collection mode has dynamic and static both of which it can be selected that especially static mode simulates colorimetric The characteristics of ware spectra collection, thoroughly solution near infrared online detection flow in process is unstable, is also easy to produce bubble, insoluble solid Detection difficult problem caused by particle is more makes collected near infrared spectrum stabilization, reliable, favorable reproducibility, improves near-infrared The accuracy and precision of the result of on-line checking.In addition, the present invention realizes near infrared spectrum data and automation control system System linkage, on-line monitoring result can directly feed back to automatic control system, really realize the online real-time monitoring of production process, Development and application of the near-infrared spectral analysis technology in drug production process are pushed, really realizes medical fluid line Quality Control.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows Meaning property embodiment and its explanation do not constitute the restriction to the application for explaining the application.
Fig. 1 is multimode near infrared online monitoring system structure diagram;
Fig. 2 is detection components structural schematic diagram;
Fig. 3 is multimode near infrared online monitoring system operatio interface.
Specific embodiment
The invention will be further described with embodiment with reference to the accompanying drawing.
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
In addition, in the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom" "inner", " up time The orientation or positional relationship of the instructions such as needle ", " counterclockwise " is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of The description present invention and simplified description, rather than the device or element of indication or suggestion meaning must have a particular orientation, with spy Fixed orientation construction and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or Implicitly include one or more of the features.In the description of the present invention, unless otherwise indicated, the meaning of " plurality " is two It is a or more than two, unless otherwise restricted clearly.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc. Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected;It can be machine Tool connection, is also possible to be electrically connected;It can be directly connected, two members can also be can be indirectly connected through an intermediary Connection inside part.For the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be Concrete meaning in bright.
In the present invention unless specifically defined or limited otherwise, fisrt feature second feature "upper" or "lower" It may include that the first and second features directly contact, also may include that the first and second features are not direct contacts but pass through it Between other characterisation contact.Moreover, fisrt feature includes the first spy above the second feature " above ", " above " and " above " Sign is right above second feature and oblique upper, or is merely representative of first feature horizontal height higher than second feature.Fisrt feature exists Second feature " under ", " lower section " and " following " include that fisrt feature is directly below and diagonally below the second feature, or is merely representative of First feature horizontal height is less than second feature.
It is mentioned in background technique, that there are heat transfer efficiencys is low for traditional smooth tube, be easy fouling, thermodynamic efficiency is not high not Foot.In order to solve these technical problems, wherein several implementations that following technical solutions according to the present invention illustrate the present invention Mode:
Embodiment one:
A kind of multimode near infrared online monitors system as shown in Figure 1, and wherein the hardware components of on-line monitoring system include: Equipment A liquid feed valve 1, duplex strainer 2, frequency conversion impeller pump 3, equipment A liquid valve 4, equipment B liquid feed valve 5, equipment B liquid valve 6, Optical fiber 16, gas source pipe 17 and detection components.The use of valve is pneumatic diaphragm valve, air pressure is connected to by gas source pipe 17 Contracting machine.Equipment B liquid feed valve 5 and equipment B liquid valve 6 are butted up against into production equipment B circulating line the corresponding interface respectively.By equipment A Liquid feed valve 1 and equipment A liquid valve 4 butt up against production equipment A circulating line the corresponding interface respectively.Equipment A liquid feed valve 1, equipment B into Liquid valve 5 is connected with 2 place pipeline of duplex strainer by threeway.Equipment A liquid valve 4, equipment B liquid valve 6 and detection components institute It is connected in pipeline by threeway.Duplex strainer 2, frequency conversion impeller pump 3 and detection components flow through sequential connection same according to medical fluid On one pipeline, and shared by equipment A and equipment B.When online detection instrument A Chinese medicine liquid quality, opens equipment A liquid feed valve 1 and set Standby A liquid valve 4, pass hull closure B liquid feed valve 5 and equipment B liquid valve 6, according to the natural flow direction of equipment A circulating line Chinese medicine liquid, Medical fluid enters equipment A liquid feed valve 1, filters through duplex strainer 2, detection components is forced by frequency conversion impeller pump 3, after detecting Medical fluid is back to equipment A from equipment A liquid valve 4.Similarly, when the quality of liquid medicine of online detection instrument B, equipment B liquid feed valve 5 is opened With equipment B liquid valve 6, pass hull closure A liquid feed valve 1 and equipment A liquid valve 4, according to the natural stream of equipment B circulating line Chinese medicine liquid To medical fluid enters equipment B liquid feed valve 5, filters through duplex strainer 2, detection components is forced by frequency conversion impeller pump 3, through examining Medical fluid is back to equipment B from equipment B liquid valve 6 after survey.
Detection components are by circulating valve 7, bubble removing filter 8, first switch valve 9, sample tap 10, sampling valve 11, electromagnetic current Meter 12, visual flow cell 13, air valve 14 and second switch valve 15 form.Visual flow cell 13 is connected to position by optical fiber 16 Near-infrared spectrometers on site.Frequency conversion impeller pump 3, electromagnetic flowmeter 12, near-infrared spectrometers and all valves Door is connected to automatic control system by signal wire, and connects and be controlled by it.Medical fluid is detected to turn through duplex strainer 2, frequency conversion After son pump 3, enter bubble removing filter 8 from bottom to top.Bubble removing filter 8 has vertically and horizontally medicine liquid outlet, vertically goes out Mouth is connected with circulating valve 7, and Horizontal Exit is connected with first switch valve 9.It is sample tap 10, sampling valve 11, electromagnetic flowmeter 12, visual Flow cell 13 and second switch valve 15 are located on the same pipeline perpendicular to ground according to sequence from bottom to top.Horizontal direction First switch valve 9 is connect with the sampling valve 11 of vertical direction and 12 place pipeline of electromagnetic flowmeter by threeway.Air valve 14 with The visual flow cell 13 of vertical direction is connected with 15 place pipeline of second switch valve by threeway.Circulating valve 7 and second switch valve 15 place pipelines are connected to two interfaces of threeway, and medical fluid merges into later returns from the third interface of the threeway all the way Production equipment.
There are two types of spectra collection mode is available for on-line monitoring system tool: static mode and dynamical fashion.
Dynamic spectrum acquisition mode are as follows: after production starts, first switch valve 9 and second switch valve 15 are kept open, Circulating valve 7 remains off, and sampling valve 11 and air valve 14 are closed when not sampling, by frequency conversion impeller pump 3 guarantee medical fluid with Stablize flow velocity by visual flow cell 13, medical fluid acquires near infrared spectrum in flow process.11 He of sampling valve is opened when sampling Air valve 14 acquires sample from sample tap 10.
Static spectrum acquisition mode are as follows: after production starts, first switch valve 9, second switch valve 15 and circulating valve 7 are opened, Sampling valve 11 and air valve 14 are closed, medicine liquid washing detection components pipeline is made.When acquiring spectrum and medical fluid sample, closes first and open Valve 9 and second switch valve 15 are closed, circulating valve 7 is opened, so that medical fluid in flow cell is remained static, while bubble floating, medical fluid Near infrared spectrum is acquired in quiescing process, remaining medical fluid returns to production equipment by 7 place pipeline of circulating valve.After acquiring spectrum Start to sample, sampling valve 11 and air valve 14 is opened simultaneously before sampling, the medical fluid in vertical duct is in atmospheric pressure and gravity Under from sample tap 10 outflow after be collected.First switch valve 9 and second switch valve 15 are opened after completing spectrum and sample acquisition, is closed Closed loop valve 7 makes medical fluid flow through pipeline where flow cell again.
The software section of on-line monitoring system is automation control program and near infrared spectra collection software, for remotely controlling System is located at each valve, flowmeter, pump and spectrum and the sample acquisition of production scene.Operation circle of automation control program Face is divided into " index predicted value ", " equipment A: time setting ", " equipment B: time setting " three parts." index predicted value " is aobvious in real time Show the online measured value of Testing index.The Trendline interface of the index can be entered after click numerical value, the real-time display index is in life Situation of change during production.
Each keypress function in " equipment A: time setting " are as follows:
1) after clicking " equipment A preparation ", equipment A liquid feed valve 1, equipment A liquid valve 4, circulating valve 7, first switch valve 9, the Two switch valves 15 and frequency conversion impeller pump 3 automatically open, other valves are in close state;
2) after clicking " stopping " key, all valves and pump are automatically closed;
3) setting " Spectral acquisition times ", " sample time " and " circulation time " is needed to join before clicking " static state acquisition (modeling) " Number, three time parameters can self-settinies according to the actual situation.With " Spectral acquisition times " 10 seconds, " sample time " 10 seconds, " follow After for 10 seconds ring time ", clicking " static state acquisition (modeling) ", automatic trigger spectra collection program, meanwhile, equipment A liquid feed valve 1, equipment A liquid valve 4, circulating valve 7 automatically open, valve first switch valve 9, second switch valve 15, sampling valve 11, air valve 14 It is automatically closed, after 10 seconds (spectra collection finishes), into sample program, sampling valve 11, air valve 14 are automatically opened, other valves Ortho states is maintained, after 5 seconds (medical fluid acquisition finishes), into cyclic program, equipment A liquid feed valve 1, equipment A liquid valve 4, first switch Valve 9, second switch valve 15 automatically open, and valve cycles valve 7, sampling valve 11, air valve 14 are automatically closed, and 10 seconds (circulation finishes) Afterwards, spectra collection program is reentered, so on circulate.After " static state acquisition (modeling) " right-click, stop above-mentioned movement;
4) setting " Spectral acquisition times " and " circulation time " parameter are needed before starting " static state acquisition (production) " function, " taken The sample time ", parameter was without corresponding function.By taking " Spectral acquisition times " 10 seconds, " circulation time " 10 seconds as an example, " static state acquisition is clicked After (production) ", automatic trigger spectra collection program, meanwhile, equipment A liquid feed valve 1, equipment A liquid valve 4, circulating valve 7 are beaten automatically It opens, valve first switch valve 9, second switch valve 15, sampling valve 11, air valve 14 are automatically closed, and 10 seconds (spectra collection finishes) Afterwards, into cyclic program, equipment A liquid feed valve 1, equipment A liquid valve 4, first switch valve 9, second switch valve 15 are automatically opened, are followed Ring valve 7, sampling valve 11, air valve 14 are automatically closed, and after 10 seconds (circulation finishes), reenter spectra collection program, so past Multiple circulation.After clicking " static state acquisition (production) " by right key, stop above-mentioned movement;
5) after clicking " dynamic acquisition preparation " key, equipment A liquid feed valve 1, equipment A liquid valve 4, first switch valve 9, second Switch valve 15 automatically opens, and circulating valve 7, sampling valve 11, air valve 14 are automatically closed;
6) after clicking " sampling starts ", sampling valve 11, air valve 14 are automatically opened, other valve states are constant;
After clicking " sampling stops ", sampling valve 11, air valve 14 are automatically closed, other valve states are constant.
Each keypress function in " equipment B: time setting " are as follows:
1) after clicking " equipment B preparation ", equipment B liquid feed valve 5, equipment B liquid valve 6, circulating valve 7, first switch valve 9, the Two switch valves 15 and frequency conversion impeller pump 3 automatically open, other valves are in close state;
2) after clicking " stopping " key, all valves and pump are automatically closed;
3) setting " Spectral acquisition times ", " sample time " and " circulation time " is needed before clicking " static state acquisition (modeling) " Time parameter.By taking " Spectral acquisition times " 10 seconds, " sample time " 10 seconds, " circulation time " 10 seconds as an example, " static state acquisition is clicked After (modeling) ", automatic trigger spectra collection program, meanwhile, equipment B liquid feed valve 5, equipment B liquid valve 6, circulating valve 7 are beaten automatically It opens, first switch valve 9, second switch valve 15, sampling valve 11, air valve 14 are automatically closed, after 10 seconds (spectra collection finishes), into Entering sample program, sampling valve 11, air valve 14 automatically open, other valves maintain ortho states, after 10 seconds (medical fluid acquisition finishes), into Enter cyclic program, equipment B liquid feed valve 5, equipment B liquid valve 6, first switch valve 9, second switch valve 15 automatically open, and valve follows Ring valve 7, sampling valve 11, air valve 14 are automatically closed, and after 10 seconds (circulation finishes), reenter spectra collection program, past with this Multiple circulation.After " static state acquisition (modeling) " right-click, stop above-mentioned movement;
4) setting " Spectral acquisition times " and " circulation time " parameter are needed before starting " static state acquisition (production) " function, " taken No setting is required for sample time " parameter.By taking " Spectral acquisition times " 10 seconds, " circulation time " 10 seconds as an example, click that " static state acquisition is (raw Produce) " after, spectra collection program is triggered first, meanwhile, equipment B liquid feed valve 5, equipment B liquid valve 6, circulating valve 7 automatically open, the One switch valve 9, second switch valve 15, sampling valve 11, air valve 14 are automatically closed, after 10 seconds (spectra collection finishes), into following Round trip sequence, equipment B liquid feed valve 5, equipment B liquid valve 6, first switch valve 9, second switch valve 15 automatically open, valve cycles valve 7, sampling valve 11, air valve 14 are automatically closed, and after 10 seconds (circulation finishes), reenter spectra collection program, and so on follow Ring.After clicking " static state acquisition (production) " by right key, stop above-mentioned movement;
5) after clicking " dynamic acquisition preparation " key, equipment B liquid feed valve 5, equipment B liquid valve 6, first switch valve 9, second Switch valve 15 automatically opens, and circulating valve 7, sampling valve 11, air valve 14 are automatically closed;
6) after clicking " sampling starts ", sampling valve 11, air valve 14 are automatically opened, other valve states are constant;Click " takes Sample stops " after, sampling valve 11, air valve 14 are automatically closed, other valve states are constant.
It when equipment is cleaned, clicks " equipment A preparation " or " equipment B preparation ", cleaning solution is made to monitor system near infrared online It is recycled between system and equipment A or equipment B.When cleaning terminates that near infrared online is stopped using to monitor system, " stopping " key is clicked.
By multimode near infrared online Application of Monitoring System in traditional Chinese medicine extraction production process.It is total that medicinal material is weighed in proportion 100kg is packed into the extractor of 1 ton of hot reflux extracting-concentration machine group, is extracted 2 times, every time 2 hours.The primary amount of water that extracts is medicine 3.5 times of material amount, second extraction amount of water are 3 times of medicinal material amount.Temperature, solvent volume, heating-up time, soaking time, drug Slag etc. is by automatic control system whole process real-time control.
Near infrared spectra collection parameter is as follows: absorbance data format is Absorbance, scanning times 32, resolution ratio For 8cm-1, optical fiber transmission-type probe light path 2mm, scanning optical spectrum range is 4000~12000cm-1, using air as reference.
" static state acquisition (modeling) " mode in modeling process, is used, clicks " equipment B preparation " after extracting production and starting, Make medicine liquid washing detection components pipeline." static state acquisition (modeling) " is clicked after suitable time, into spectra collection, sampling, circulation Repeated pattern.Wherein " Spectral acquisition times ", " sample time " and " circulation time " parameter are respectively set are as follows: 180 seconds, 30 seconds and 90 seconds.Each sample collection spectrum about 13 chooses wherein 3, calculates averaged spectrum, is used for model foundation.Extracting solution sample About 100 milliliters of sampling amount.
Stop detection at the end of extracting production, clicks " static state acquisition (modeling) " by right key.When equipment is cleaned, " equipment B is clicked Prepare ", it monitors cleaning solution near infrared online and is recycled between system and extract equipment.Cleaning terminates that near-infrared is stopped using to exist When line monitoring system, click " stopping ".
Using each in the standard method of analyses such as high performance liquid chromatography, oven drying method, gravimeter measurement extracting solution sample Model index.
The near-infrared model of each index is established using near-infrared data processing software (Bruker, OPUS).It compares various pre- The influence of processing method and different modeling wave bands to each index quantification model.The results show that original spectrum is by first derivative The R value and RSEP value of each model are larger after reason, and RMSECV value is smaller.By abnormal point judgement, Pretreated spectra and modeling After the selection of wave band, 213 extracting solution samples are finally obtained for modeling.Each index of extraction process is established with Partial Least Squares Near-infrared quantitative calibration models, and with model built predict it is new extract batch, model prediction parameter, which summarizes, is shown in Table 3.It extracted The RSEP value of each index model of journey can control within 10%, and the related coefficient of true value and predicted value reaches 0.97 or more, Comply fully with the required precision that Chinese Traditional Medicine is analyzed in real time.
The predictive ability parameter of each index model of 1 extraction process of table
When being used to monitor on-line traditional Chinese medicine extraction production process for model built, " Spectral acquisition times " are set and " when circulation Between " parameter, it is respectively as follows: 180 seconds and 90 seconds.Spectra collection program, gained light are triggered after clicking " static state acquisition (production) " key Modal data directly exports each index prediction result after model calculates, and is shown in " index after being read by automatic control system Predicted value " interface.
It is tested by multiple batches of repetition, threshold value of each index in concentration process can be obtained, and its threshold value is set as " alarm value ".When production process is abnormal situation or reaches production terminal, near infrared online monitoring system monitors to refer to Data are marked more than after set threshold value, automatic control system can issue red warning, and plant personnel is reminded to be located accordingly Reason.
Embodiment two:
The present embodiment and the difference of embodiment one are: by multimode near infrared online Application of Monitoring System in traditional Chinese drug inspissation Production process.
The Aqueous extracts that embodiment one obtains are introduced to the concentration of 1 ton of hot reflux extracting-concentration machine group by way of vacuumizing In tank, vacuum degree is set as -0.04~-0.08MPa in concentration process, and temperature is 75~85 DEG C, is concentrated to a relative density of Think that concentration process reaches terminal when 1.1.
Near infrared spectra collection parameter is the same as example 1." static state acquisition (modeling) " mode is used, is produced in concentration " equipment A preparation " is clicked after beginning, makes medicine liquid washing detection components pipeline." static state acquisition (modeling) " is clicked after suitable time, Into spectra collection, sampling, circulation repeated pattern.Wherein " Spectral acquisition times ", " sample time " and " circulation time " parameter It is respectively set are as follows: 180 seconds, 30 seconds and 90 seconds.Each sample collection spectrum about 13 chooses wherein 3, saves averaged spectrum, For model foundation.About 100 milliliters of concentrate sample volume.
Stop detection at the end of concentration production, clicks " static state acquisition (modeling) " by right key.When equipment is cleaned, " equipment A is clicked Prepare ", it monitors cleaning solution near infrared online and is recycled between system and concentration tank.At the end of cleaning, click " stopping ".
It is measured in concentrate sample according to one method of embodiment and respectively models index.
The near-infrared quantitative calibration models of each index of concentration process are established using Partial Least Squares.Pass through near-infrared data Processing software carries out permutation and combination modeling, comparative study influences of the various preprocess methods to each index model.Pass through comparison Model performance parameter, near-infrared model after optimization.
Each index model predictive ability parameter is concentrated and is shown in Table 2.Since present case uses static spectrum acquisition mode, when close red When outer on-line monitoring system enters spectra collection program, two valves are automatically closed flow cell up and down, and bubble rises rapidly, medical fluid In static and stable state, therefore collected spectrum can match in excellence or beauty the stability of cuvette spectra collection mode and accurate Property.According to 2 data of table, the RSEP value of each index partial least square model is below 4.8%, the phase relation of true value and predicted value Number is 0.999, and the result for showing that near-infrared prediction result and standard method obtain is very close, and precision of prediction is high, prediction knot Fruit has very high confidence level.
The predictive ability parameter of each index model of 2 concentration process of table
After starting near infrared online monitoring system, by clicking corresponding near-infrared operation interface, method with embodiment 1, Model built can be used to monitor traditional Chinese drug inspissation production process on-line.It is tested by multiple batches of repetition, each index can be obtained and exist Threshold value in concentration process, and its threshold value is set as " alarm value ".When production process is abnormal situation or reaches production Terminal, near infrared online monitor the monitored achievement data of system more than after set threshold value, and automatic control system can issue Red warning, reminds plant personnel to perform corresponding processing.
From the angle for saving cost, the practical problem that multiple production equipments share a set of on-line monitoring system is solved.Spectrum Acquisition mode have dynamic and static both of which it can be selected that especially static mode simulation cuvette spectra collection the characteristics of, It thoroughly solves to examine caused by near infrared online detection flow in process is unstable, to be also easy to produce bubble, insoluble solid particle more Difficult problem is surveyed, makes collected near infrared spectrum stabilization, reliable, favorable reproducibility, improves the result of near infrared online detection Accuracy and precision.In addition, the present invention realizes near infrared spectrum data and automatic control system linkage, on-line monitoring knot Fruit can directly feed back to automatic control system, really realize the online real-time monitoring of production process, push near infrared spectrum point Medical fluid line Quality Control is really realized in development and application of the analysis technology in drug production process.
It above are only several embodiments of the invention, it should be understood by those skilled in the art that, reality of the invention Applying example can provide as method, system or computer program product.Therefore, the present invention can be used complete hardware embodiment, completely it is soft The form of part embodiment or embodiment combining software and hardware aspects.
In addition, it should be noted that:
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any One or more embodiment or examples in can be combined in any suitable manner.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention, it is all according to this hair Bright technical spirit any simple modification, equivalent change and modification to the above embodiments, still fall within the technology of the present invention In the range of scheme.

Claims (9)

1. a kind of multimode near infrared online monitors system, which is characterized in that including duplex strainer, frequency conversion impeller pump, optical fiber And detection components;
The input terminal of the duplex strainer pass through respectively the first liquid feed valve, the second liquid feed valve accordingly with fill medical fluid to be measured Equipment A, equipment B connection, output end are connect with the input terminal of frequency conversion impeller pump;
The output end of the frequency conversion impeller pump is connect with detection components, for extremely detecting the medical fluid pumping to be measured in relevant device In component;
The detection components, for eliminating turbulent flow and bubble in medical fluid to be measured, the output end of the detection components passes through respectively First liquid valve, the second liquid valve are connect with accordingly equipment A, equipment B, and medical fluid to be measured is transmitted back in original equipment;
The optical fiber is connected between the detection components and On-line NIR analyzer, and being used for will be in detection components The infrared spectroscopy testing result of medical fluid to be measured is transmitted to On-line NIR analyzer.
2. a kind of multimode near infrared online according to claim 1 monitors system, which is characterized in that the detection components Including bubble filter, circulating valve, first switch valve, electromagnetic flowmeter, visual flow cell, air valve and second switch valve;
The bubble filter is connect with one end of frequency conversion impeller pump, circulating pump and first switch valve respectively, the first switch The other end of valve is connect with the electromagnetic flowmeter;
The electromagnetic flowmeter, the visual flow cell, the air valve and the second switch valve are sequentially connected with;
One end of the optical fiber is connect with the visual flow cell, and the other end connects the On-line NIR analyzer.
3. a kind of multimode near infrared online according to claim 2 monitors system, which is characterized in that the first switch Sample tap is connected by sampling valve between valve and the visual flow cell.
4. a kind of multimode near infrared online according to claim 3 monitors system, which is characterized in that the bubble filtering It is detachably provided with stainless steel filtration core in device, is flowed out, passes through from the lower end of bubble filter by filtered medical fluid to be measured First switch valve flows into electromagnetic flowmeter.
5. a kind of multimode near infrared online according to claim 3 monitors system, which is characterized in that first feed liquor Valve, the second liquid feed valve, the first liquid valve, the second liquid valve, first switch valve, second switch valve, circulating valve, air valve and sampling Valve is all made of pneumatic diaphragm valve.
6. a kind of multimode near infrared online monitoring system according to any one of claim 5, which is characterized in that described First liquid feed valve, the second liquid feed valve, the first liquid valve, the second liquid valve, first switch valve, second switch valve, circulating valve, broken sky Valve and sampling valve pass through gas source pipe and connect with air compressor.
7. the multimode near infrared online monitoring method of application multimode near infrared online as claimed in claim 3 monitoring system, It is characterized by comprising the following steps:
The corresponding liquid feed valve of equipment where opening medical fluid to be measured and liquid valve;
First switch valve and second switch valve are opened, circulating valve, sampling valve and air valve is closed, is made by frequency conversion impeller pump to be measured Medical fluid is to stablize flow velocity by visual flow cell, the infrared spectroscopy of medical fluid to be measured in the visual flow cell of collecting fiber, and will be infrared Transfer spectral information is to infrared spectrometric analyzer;
First switch valve, second switch valve, sampling valve and air valve are opened, circulating valve is closed, acquires sample from sample tap.
8. the multimode near infrared online monitoring method of application multimode near infrared online as claimed in claim 3 monitoring system, It is characterized by comprising the following steps:
The corresponding liquid feed valve of equipment where opening medical fluid to be measured and liquid valve;
First switch valve, second switch valve, circulating valve are opened, sampling valve, air valve are closed, makes the pipe to be measured for rinsing detection components Road;
First switch valve, second switch valve are closed, circulating valve is opened, so that medical fluid to be measured in flow cell is remained static, simultaneously Bubble floating acquires near infrared spectrum in medical fluid quiescing process to be measured, remaining medical fluid returns to phase by pipeline where circulating valve The equipment answered;
Sampling valve and air valve are opened, is collected medical fluid to be measured after sample tap outflow under atmospheric pressure and gravity;
After completing infrared spectroscopy acquisition and sample acquisition, first switch valve and second switch valve are opened, circulating valve is closed, makes to be measured Medical fluid is flow back into original equipment.
9. a kind of storage medium, is stored with computer program, which is characterized in that the computer program in execution processed, Realize the multimode near infrared online monitoring method as described in any one of claim 7 or 8.
CN201811459678.0A 2018-11-30 2018-11-30 Multimode near infrared online monitors system and its application method Pending CN109682776A (en)

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