CN106290530A - A kind of can the self-correction interference electrochemical analyte sensor-based system of signal and method - Google Patents
A kind of can the self-correction interference electrochemical analyte sensor-based system of signal and method Download PDFInfo
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Abstract
The invention discloses a kind of can self-correction interference signal electrochemical analyte sensor-based system, including sensor body, DC-voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, controller, data process and communication component, power supply.Add a blank electrode identical with working electrode size, by the way of signal subtraction, eliminate interference signal.Add ac impedance measurement parts, and the system impedance value exported with it judges the duty of sensor.Can effectively eliminate impact analyte signal produced because of the existence of chaff interference and measurement environmental change, make sensor ensure to measure effectiveness and the accuracy of signal during operation.
Description
Technical field
The present invention relates to analyte sensing system technical field, be specifically related to a kind of can self-correction interference signal electrochemistry
Analyte sensing system and method.
Background technology
Electrochemical sensor is a kind of widely used analyte sensor, and its basic functional principle is by sensor
Applying voltage or the electric current being suitable on working electrode, being converted into by electrochemical reaction by the chemical analyte measured in sample can
The signal of telecommunication of detection.There is at present all types of biosensor for multiple analytes the most on the market, wherein most study,
Common biosensor is current mode (ampere-type) glucose sensor, and it is for successfully controlling the G/W of diabetes
It is very important for Ping.
Traditional amperometric glucose sensor utilizes the glucoseoxidase being fixed on sensor electrode in sample
Glucose oxidation generates gluconic acid and by-product hydrogen peroxide, then hydrogen peroxide is aoxidized on working sensor electrode from
And generate detectable current signal.Being similar to therewith, the reaction occurred in the multiple oxidoreductase being known in the art is
It is used for amperometric sensor based on same operation principle design.
One common problem of electrochemical sensor is that they not only (or can have this analyte with analyte to be measured
The by-product of enzymatic reaction) be electrochemically reacted, but also measured electroactive chemical species can be not intended to other and enter
Row reaction, due to these " interference species ", the most measured this reaction causes signal intensity to increase, thus has influence on dividing
The accurate judgement of analysis substrate concentration.Such as, in traditional amperometric glucose sensor based on glucoseoxidase, it is known that all
Interference species such as acetaminophen, Ascorbate and urate etc obscure real analyte signal.
Additionally, the signal that traditional amperometric electrochemical sensor is obtained also can be by the measurement environment residing for sensor
Changing and affected, these situations include but not limited to that the electro-chemical activity of sensor electrode decorative layer weakens, and are dehydrated or decompose de-
Falling, sensor is combined, by nonspecific proteins, the impermeable stratum formed and covers, and sensor displacement etc. from detection environment.By
Cannot tell the signal source of its working electrode in conventional current type electrochemical sensor, therefore these environmental changes will be to dividing
The accuracy of analysis analyte detection causes tremendous influence.
Based on this reason, amperometric electrochemical sensor needs are a set of can carry out self-inspection, differentiates and gets rid of non-analysis
The solution of the signal of thing, the most non-analyte signal includes chaff interference signal and electrode perimeter ambient signal etc..At present, pin
The eliminating of chaff interference signal is mainly solved by increasing AF panel barrier film at working sensor electrode surface, its working machine
System is the chaff interference utilizing the isolation of barrier film physicochemical characteristics different from analyte so that it is cannot send out by touch sensor electrode surface
Raw electrochemical reaction.Common scheme includes that macromole chaff interference is isolated by the pore size adjusting barrier film, and utilizes barrier film material
Material contacts the positive charge or negative charge carried at strand to the chaff interference molecule generation repelling effect with identical charges with water
Deng.And judge ambient signal, generally by the absolute figure of signal code and rate of change analysis are produced, such as, to work as letter
Count value is significantly lower than normal range, or signal intensity speed is apparently higher than during because of normal analyte concentration rate of change, can
To think that sensor measurement data lost efficacy, need to recalibrate sensor or stop sensor work.Above two interference signal
Get rid of and the solution of ambient signal eliminating combines application the most often.
Existing both schemes have certain limitation.For the eliminating of interference signal, answering of AF panel barrier film
High by not only manufacturing cost, complex process, and can only be effective to a specific class chaff interference.Such as by adjusting pore size
The chaff interference bigger than analyte molecule can only be got rid of, and the interference similar or less with analyte molecule size cannot be got rid of
Thing；Equally, electric charge exclusive method also can only get rid of with analyte electrically charged contrary chaff interference, and cannot get rid of neutrality or with
The chaff interference of the same electric charge of analyte band.For the eliminating of measurement environment effect of signals, use the absolute number of the sensor signal of telecommunication
Value is analyzed and rate of change analysis is only capable of getting rid of extreme case, and can not differentiate or measurement environmental change that eliminating amplitude is less
Impact.In this case, the accuracy of sensor still can be affected, it is therefore desirable to periodically carries out calibration to adjust electric current letter
Number and analyte concentration between correlation ensure accuracy, which increases the use difficulty of sensor, ease of use
It is deteriorated.
Summary of the invention
It is an object of the present invention to provide a kind of can the self-correction interference electrochemical analyte sensor-based system of signal and method, to solve
Certainly the deficiencies in the prior art.
The present invention is by the following technical solutions:
A kind of can self-correction interference signal electrochemical analyte sensor-based system, including sensor body, DC voltage supply
Electricity parts, current measuring members, ac impedance measurement parts, circuit changing switch, controller, data process and communication component,
Power supply,
Sensor body, including working electrode, reference electrode, to electrode and blank electrode；
DC-voltage supply parts, including two independent parallel circuits, apply to working electrode and blank electrode respectively
The voltage identical relative to reference electrode, to excite corresponding analyte electrochemical reaction current and chaff interference kinetic current；
Current measuring members, including two independent current measuring members, measures working electrode and blank electrode institute respectively
The electric current that passes through also is sent to data the numerical value recorded and processes and communication component；
Ac impedance measurement parts, for applying one again while applying DC voltage to working electrode or blank electrode
The alternating voltage of individual fixed frequency, then measures working electrode or the corresponding current response of blank electrode and calculates it and hand over accordingly
Leakage resistance resists, and then output result is sent to data and processes and communication component；
Circuit changing switch, is used for working electrode between corresponding current measuring members and ac impedance measurement parts
Switching, opportunity and the frequency of switching are determined by the instruction of controller；Or be used for blank electrode at corresponding current measuring members
And switch between ac impedance measurement parts, opportunity and the frequency of switching are determined by the instruction of controller；
Controller, for timing, controls sampling time and frequency, the adopting of ac impedance measurement parts of current measuring members
Sample time and frequency, the state of circuit changing switch, and data process and communication component processes and the opportunity of transmission data；
Data process and communication component, the output result obtained from current measuring members and ac impedance measurement parts are entered
Row operation, thus draw analyte concentration and send the result to receive terminal；
Power supply, to DC-voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, control
Device processed, data process and communication component provides the electric energy needed for running；
DC-voltage supply element outputs connects with working electrode, blank electrode respectively；Blank electrode outfan and its
Corresponding current measuring members connects, and working electrode and circuit changing switch connect, and circuit changing switch is electric with work the most respectively
The current measuring members of level correspondence, ac impedance measurement parts connect, or the current measuring members of working electrode and its correspondence is even
Connecing, blank electrode and circuit changing switch connect, corresponding with the blank electrode the most respectively current measuring members of circuit changing switch,
Ac impedance measurement parts connect；Controller output end switches with current measuring members, ac impedance measurement parts, circuit respectively
Switch, data process and communication component connects, and current measuring members, ac impedance measurement parts process and communication with data respectively
Part input connects, and power output end connects with DC-voltage supply parts, controller respectively.
Further, working electrode surface is modified with the oxidoreductase just for analyte or redox couple medium,
Blank electrode in addition to without modifying for the oxidoreductase of analyte or redox couple medium, remaining attribute all with
Blank electrode is identical；Working electrode and blank electrode position on a sensor is adjacent, and the beeline between two electrodes is not
More than 5 millimeters.
Further, cover layer in working electrode and blank electrode.
Further, the frequency of ac impedance measurement parts alternating voltage is 100kHz-1kHz, ac impedance measurement parts
The output of impedance measurement includes the resistance value of impedance and phase place or the real part of impedance and imaginary part.
Further, the current measurement sample frequency of working electrode exceeds ac impedance measurement sample frequency more than 10 times.
A kind of can self-correction interference signal electrochemical analyte method for sensing, comprise the steps:
Step one, apply the voltage identical relative to reference electrode to working electrode and blank electrode respectively, to excite phase
The analyte electrochemical reaction current answered and chaff interference kinetic current, measured by corresponding current measuring members respectively, and handle
The numerical value recorded is sent to data and processes and communication component；AC impedance parts are applying direct current to working electrode or blank electrode
Apply the alternating voltage of a fixed frequency while voltage again, then measure working electrode or the corresponding electric current of blank electrode is anti-
Its corresponding alternating current impedance and should be calculated, then output result is sent to data and processes and communication component；
Step 2, data process and communication component utilize from current measuring members and ac impedance measurement parts obtain defeated
Go out result and carry out computing, thus draw analyte concentration and send the result to receive terminal.
Further, the computing in step 2 comprises 1 input data point, 9 input message sequences and 2 output information
Sequence, 1 input data point is: system initial time t0, and 9 input message sequences are: working electrode sample rate current sequence I1,
Working electrode sampling time sequence t1, blank electrode sample rate current sequence I2, blank electrode sampling time sequence t2, impedance real part
Sequence Zre, imaginary impedance sequence Zim, impedance sampling time sequence tZ, calibrate analyte concentration sequence C 0, during calibration analyte
Between tc0,2 output information sequences be: measure analyte concentration sequence C 1, measure time tc1；When sensor-based system is energized also first
After startup, system records startup time t0, and start simultaneously at writing task electrode and blank electrode sample rate current I1, I2 and
Sampling time t1, t2；The t2 sampling time is less than 1 minute before and after t1；
Specifically include following steps:
Step A, first determine whether whether current run time T=(t1 t0) alreadys more than default running life Tmax, as
Fruit is judged to, then out of date needs of system prompt sensor is changed；If it is determined that no, then operating procedure B；
Step B, judge whether the operation time has exceeded the initialization time preset, if it is, operating procedure C；If
No, then in prompting sensor initializing, wait the next current sample time, then repeat step A；
Step C, responsible execution, with measuring current value computational analysis substrate concentration, are first read writing task electrode and blank are electric
Sample rate current I1, I2 and sampling time t1, t2 of pole start computing；
Step D and E, Filtering Processing reduce noise and interference, data obtain after processing the electric current I1 ', the I2 ' that processed and time
Between t1 ', t2 '；
Step F, the signal in blank electrode is deducted from working electrode currents, obtains analyte current I=I1 '-
I2 ', thus eliminate the current signal that chaff interference produces；Simultaneously by the information of comprehensive t1 ' and t2 ', obtain analyte current
Corresponding time t=(t1'+t2')/2；
Step G, use analyte current I and up-to-date conversion coefficient X, calculate the concentration C 1 of institute's cls analysis thing；Used
Formula is C1=f (I, X), simultaneously retention analysis substrate concentration correspondence time tc1=t, and analyte concentration waits after having calculated and obtaining
Take new current sample and repeat step A.
Further, up-to-date in step G conversion coefficient X comprises the steps to obtain: check whether sensor-based system passes through
Calibrate and calculate the conversion coefficient X ' of non-compensating approach and corresponding nearest prover time tc ', X ' and tc ' numerical value are imported phase
Close algorithm and it compensated by the result of ac impedance measurement and revises；
Specifically include following steps:
Step H, first check whether to there is recent calibration, if it did not, system will use the conversion system preset
Number X '=X0, prover time is calculated as 0；If it has, then calculate X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f
The inverse operation of (I, X)；Tc ' being updated to tc0, wherein, C0 is the analyte concentration value of calibration, and I (tc0) is range calibration simultaneously
The recent analyte current that records of time of origin, the time that I (tc0) occurs differs less than 5 minutes with tc0；
Step I, X ' and tc ' numerical value are imported related algorithm and by the result of ac impedance measurement to its compensate with
Revise, and appearance is calibrated in wait, then repeats step H next time；
Wherein, X ' and tc ' numerical value are imported related algorithm and by the result of ac impedance measurement to its compensate with
Revise, specifically include following steps:
Step J, first determine whether whether up-to-date prover time is later than the up-to-date ac impedance measurement time once, if
It is then to complete step K, does not perform any compensation correction directly output conversion coefficient X=X '；If it is not, then complete step L, read
Take away from calibration time of origin recent ac impedance measurement value Zre_cal and Zim_cal, enter step M；
Step M, first determine whether current impedance measurements Zre and Zim the most all in preset range, if it is not, then
System is judged as operation irregularity, stops display result of calculation and show information warning；If it is, operating procedure N, calculate and work as
The difference of numerical value Zre_cal and Zim_cal when front resistance value Zre and Zim and calibration, draw dZre=Zre Zre_cal and
DZim=Zim Zim_cal；
Step O, judge the absolute difference of resistance value whether exceeded preset drift threshold dZre_thres and dZim_
Thres, if it is not, then complete step K, does not compensates and corrects conversion coefficient, if it is, carry out subsequent step P；
Step P, contain the directivity of four conditional judgments difference dZre and dZim to compare impedance measured value, the most right
Conversion coefficient X ' makees corresponding correction, and these judgements there will be 5 kinds of possible results, respectively altogether:
A) dZre and dZim is just being and more than corresponding threshold value；Now perform step Q, conversion coefficient X ' is carried out increase and repaiies
Just, concrete mode is to be multiplied by equation h (Zre/Zre_cal, a Zim/ relevant to impedance real part and imaginary part institute measured value
Zim_cal), the result of this equation is naturally larger than 1；
B) dZre for just and more than dZre_thres threshold value but dZim is not more than dZim_thres threshold value；Now perform step
R, carries out conversion coefficient X ' increasing and revises, and concrete mode is to be multiplied by an equation closed with impedance real part numerical difference out-phase
J (Zre/Zre_cal), the result of this equation is naturally larger than 1；
C) dZre is for bearing and less than negative dZre_thres threshold value, now performs step S, conversion coefficient X ' is carried out reduction and repaiies
Just, concrete mode is to be multiplied by an equation k (Zre/Zre_cal) relevant to impedance real part numerical value, the result of this equation
Certainly less than 1；
D) in positive and negative dZre_thres threshold range but dZim is just and to be more than dZim_thres threshold value to dZre, now holds
Row step T, carries out conversion coefficient X ' increasing and revises, and concrete mode is closed with imaginary impedance numerical difference out-phase for being multiplied by one
Equation m (Zim/Zim_cal), the result of this equation is naturally larger than 1；
E) in positive and negative dZre_thres threshold range but dZim is for bearing and less than negative dZim_thres threshold value, now for dZre
Performing step U, carry out conversion coefficient X ' reducing and revise, concrete mode is for being multiplied by one and imaginary impedance numerical difference out-phase
The equation n (Zim/Zim_cal) closed, the result of this equation is certainly less than 1；
Obtain revising conversion coefficient X or not revising as performed step K, X conduct after X ' is done compensating approach
The output of this some algorithm is given to step G in order to computational analysis concentration value.
Further, when step L reads calibration, resistance value is after step M judged result is for being, before performing step N
Carry out.
Further, after step P completes, send an information warning, prompting by system to sensor user simultaneously
Sensor is in non-optimal duty, needs to re-start calibration.
Beneficial effects of the present invention:
1, the present invention propose a kind of can self-correction interference signal electrochemical analyte sensor-based system, can effectively disappear
Except impact analyte signal produced because of the existence of chaff interference and measurement environmental change, sensor is made to ensure during operation
Measure effectiveness and the accuracy of signal.This scheme is applicable to all containing oxidoreductase or redox couple medium
The amperometric electrochemical sensor of (redox couple medium), its typical case's application can be a kind of containing glucoseoxidase
Implanted human body subcutaneous matter interstitial fluid glucose sensor, but be not limited only to this type of application.
2, the present invention adds a blank electrode identical with working electrode size in sensor systems, by signal phase
The mode subtracted eliminates interference signal.Manufacture easier compared with increasing AF panel barrier film on a sensor, and chaff interference is divided
Son does not has selectivity, can effectively eliminate the signal that any kind of chaff interference causes.
3, the present invention adds ac impedance measurement parts, and the system impedance value exported with it in sensor systems
Judge the duty of sensor.Ac impedance measurement is a kind of independent with analyte concentration in the range of suitable a-c cycle
Electrochemical measuring method, can accurately record and around sensor, whether have notable environmental change.Such as sensor electrode is attached
The current signal that nearly tissue water content increase can cause sensor to obtain increases therewith, but the actual concentrations of analyte does not change
Becoming, now AC impedance real part numerical value also can decline because of the aqueous increase of sensor senses layer, therefore can be from its impedance
The analyte concentration recorded is revised in change.In like manner, cover if sensor is combined by the nonspecific protein having barriering effect
Lid, analyte diffusion hindered makes sensor current reduce；Now AC impedance real part numerical value can increase, therefore can be according to resistance
The degree increase electric current-analyte concentration conversion coefficient of anti-increase, thus the signal that modifying factor analyte diffusion hindered reduces.?
Under extreme case, sensor damages because of external force collision or comes off, and is no longer on detecting in environment, now ac impedance measurement
An abnormal googol value can be shown, exceed default normal range, therefore can determine that sensor loses according to AC impedance
Effect, reminds user to note.So, use ac impedance measurement can than the simple numerical value using working electrode to measure electric current and
Rate of change analysis more effectively indicates the state of working electrode, and can be modified as the case may be, reduces calibration
Demand.
4, the present invention establishes a set of algorithm and uses the output to sensing system of the result point situation of ac impedance measurement
Result compensates and revises, and improves the degree of accuracy of output result and in due course to sensor user output prompting letter
Breath to carry out change or the calibration of necessity to sensing system.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of sensor-based system of the present invention.
Fig. 2 is another schematic diagram of sensor-based system of the present invention.
Fig. 3 is that data process and communication component utilizes the output obtained from current measuring members and ac impedance measurement parts
Result carries out the schematic flow sheet of computing.
Fig. 4 is to check that whether through calibration the conversion coefficient X ' that calculates non-compensating approach and correspondence sensor-based system
Nearly prover time tc ' schematic flow sheet.
Fig. 5 is to the conversion coefficient X ' of non-compensating approach and when calibrating recently of correspondence by the result of ac impedance measurement
Between the tc ' schematic flow sheet that compensates and revise.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example is merely to illustrate this
Bright, but it is not used to limit the practical range of the present invention.
A kind of can self-correction interference signal electrochemical analyte sensor-based system, as depicted in figs. 1 and 2, including sensor
Body, DC-voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, controller, data
Process and communication component, power supply.
Sensor body, including working electrode, reference electrode, to electrode and blank electrode；Working electrode surface is modified with
Just for oxidoreductase or the redox couple medium of analyte, the thin of one layer of protection decorative layer the most also can be covered
Film layer；Blank electrode is in addition to without modifying for the oxidoreductase of analyte or redox couple medium, and remaining belongs to
Property (such as electrode material, surface area size, shape, with thinfilm protective coating etc.) is all identical with blank electrode；Working electrode and
Blank electrode position on a sensor is adjacent, and the beeline between two electrodes is less than 5 millimeters.If one is containing glucose
Oxidasic implanted human body subcutaneous matter interstitial fluid glucose sensor, sensor is with the working electrode of a 0.5mmx0.5mm
With the blank electrode of a 0.5mmx0.5mm, wherein on working electrode, it is coated with 10 microns of thick glucoseoxidases and 50 micro-
Non-biocompatible thin film's layer that rice is thick, and blank electrode is just coated with 50 microns of thick non-biocompatible thin film's layers.Two electrodes
The beeline of border is 2mm.
DC-voltage supply parts, including two independent parallel circuits, apply to working electrode and blank electrode respectively
The voltage identical relative to reference electrode, to excite corresponding analyte electrochemical reaction current and chaff interference kinetic current.
Current measuring members, including two independent current measuring members, measures working electrode and blank electrode institute respectively
The electric current that passes through also is sent to data the numerical value recorded and processes and communication component.
Ac impedance measurement parts, for applying one again while applying DC voltage to working electrode or blank electrode
The alternating voltage of individual fixed frequency, then measures working electrode or the corresponding current response of blank electrode and calculates it and hand over accordingly
Leakage resistance resists, and then output result is sent to data and processes and communication component.The frequency of alternating voltage selects can be according to electricity
The size of pole, shape, depending on the modification situation of electrode surface, it will usually between 100kHz to 1kHz.Above-mentioned containing glucose
In oxidasic implanted human body subcutaneous matter interstitial fluid glucose sensor, the frequency of alternating voltage is 1kHz.Impedance measurement defeated
Information of both going out to include, can be resistance value (Z) and the phase place (Φ) of impedance, it is also possible to be the real part (Z of impedanceRe) and empty
Portion (ZIm).The transformational relation of resistance value/phase place and real part/imaginary part is as follows:
ZRe=Z*cos (Φ)；
ZIm=-Z*sin (Φ)；
Z=√ (ZRe 2+ZIm 2)；
Φ=-tan-1(ZIm/ZRe)。
Circuit changing switch, is used for working electrode between corresponding current measuring members and ac impedance measurement parts
Switching, opportunity and the frequency of switching are determined by the instruction of controller；Or be used for blank electrode at corresponding current measuring members
And switch between ac impedance measurement parts, opportunity and the frequency of switching are determined by the instruction of controller.
Controller, for timing, controls sampling time and frequency, the adopting of ac impedance measurement parts of current measuring members
Sample time and frequency, the state of circuit changing switch, and data process and communication component processes and the opportunity of transmission data；Its
The sample frequency that middle impedance is measured much smaller than current sample frequency, preferred current sample frequency ratio impedance measurement exceed 10 times with
On, such as current sample frequency is 1 time per minute, and impedance is sampled every 15 minutes 1 time.The measurement frequency of ac impedance measurement parts
Formulated by the presupposed solution of controller and less than working electrode or the measurement frequency of blank electrode electric current.A kind of alternative method is to make
Measure by working electrode or blank electrode the result of electric current, particularly its rate of change decide whether active circuit switching switch and
Ac impedance measurement parts, to ensure to provide impedance information timely, it is ensured that system is properly functioning.
Data process and communication component, the output result obtained from current measuring members and ac impedance measurement parts are entered
Row operation, thus draw analyte concentration and send the result to receive terminal.
Power supply, to DC-voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, control
Device processed, data process and communication component provides the electric energy needed for running.
DC-voltage supply element outputs connects with working electrode, blank electrode respectively；Blank electrode outfan and its
Corresponding current measuring members connects, and working electrode and circuit changing switch connect, and circuit changing switch is electric with work the most respectively
The current measuring members of level correspondence, ac impedance measurement parts connect, or the current measuring members of working electrode and its correspondence is even
Connecing, blank electrode and circuit changing switch connect, corresponding with the blank electrode the most respectively current measuring members of circuit changing switch,
Ac impedance measurement parts connect.Controller output end switches with current measuring members, ac impedance measurement parts, circuit respectively
Switch, data process and communication component connects, and current measuring members, ac impedance measurement parts process and communication with data respectively
Part input connects, and power output end connects with DC-voltage supply parts, controller respectively.
A kind of can self-correction interference signal electrochemical analyte method for sensing, comprise the steps:
Step one, apply the voltage identical relative to reference electrode to working electrode and blank electrode respectively, to excite phase
The analyte electrochemical reaction current answered and chaff interference kinetic current, measured by corresponding current measuring members respectively, and handle
The numerical value recorded is sent to data and processes and communication component；AC impedance parts are applying direct current to working electrode or blank electrode
Apply the alternating voltage of a fixed frequency while voltage again, then measure working electrode or the corresponding electric current of blank electrode is anti-
Its corresponding alternating current impedance and should be calculated, then output result is sent to data and processes and communication component.
Step 2, data process and communication component utilize from current measuring members and ac impedance measurement parts obtain defeated
Go out result and carry out computing, thus draw analyte concentration and send the result to receive terminal；This computing comprises 1 input data
Point, 9 input message sequences and 2 output information sequences, 1 input data point is: system initial time t0,9 input letters
Breath sequence is: working electrode sample rate current sequence I1, working electrode sampling time sequence t1, blank electrode sample rate current sequence
I2, blank electrode sampling time sequence t2, impedance real part sequence Zre, imaginary impedance sequence Zim, impedance sampling time sequence tZ,
Calibration analyte concentration sequence C 0, calibrates analyte time tc0, and 2 output information sequences are: measure analyte concentration sequence
C1, measures time tc1；As it is shown on figure 3, after sensor-based system is energized first and starts, system records startup time t0, and same
Time start sample rate current I1, I2 and sampling time t1, t2 of writing task electrode and blank electrode；The t2 sampling time is before and after t1
Less than 1 minute, concrete such as t1=t2.
Specifically include following steps:
Step A, first determine whether whether current run time T=(t1 t0) alreadys more than default running life Tmax (example
Such as 5 days), if it is decided that be yes, then out of date needs of system prompt sensor is changed；If it is determined that no, then operating procedure B.
Step B, judge the operation time whether exceeded preset initialization time (such as 30 minutes), if it is, fortune
Row step C；If it is not, then in prompting sensor initializing, wait the next current sample time, then repeat step A.
Step C, responsible execution, with measuring current value computational analysis substrate concentration, are first read writing task electrode and blank are electric
Sample rate current I1, I2 and sampling time t1, t2 of pole start computing.
Step D and E, Filtering Processing reduce noise and interference, and its concrete processing mode is the conventional means of this area, this
It is not specifically related in bright.Data obtain electric current I1 ', I2 ' and time t1 ', the t2 ' processed after processing.
Step F, the signal in blank electrode is deducted from working electrode currents, obtains analyte current I=I1 '-
I2 ', thus eliminate the current signal that chaff interference produces；Simultaneously by the information of comprehensive t1 ' and t2 ', obtain analyte current
During corresponding time t=(t1'+t2')/2, t1=t2, t=t1 '.
Step G, use analyte current I and up-to-date conversion coefficient X, calculate the concentration C 1 of institute's cls analysis thing；Used
Formula is C1=f (I, X)；In common electrochemical sensor application, analyte response electric current and its concentration in the sample
The most linear, the expression of f (I, X) is then (I-b) * X, and wherein b is default background current value, retains simultaneously
Analyte concentration correspondence time tc1=t, analyte concentration calculated after etc. new current sample to be obtained repeat step A.
Conversion coefficient X up-to-date in step G comprises the steps to obtain: check that whether sensor-based system is through calibrating and calculating
Go out the conversion coefficient X ' of non-compensating approach and corresponding nearest prover time tc ', X ' and tc ' numerical value are imported related algorithm and lead to
It is compensated and revises by the result crossing ac impedance measurement；
As shown in Figure 4, following steps are specifically included:
Step H, first check whether to there is recent calibration, if it did not, system will use the conversion system preset
Number X '=X0, prover time is calculated as 0；If it has, then calculate X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f
The inverse operation of (I, X)；In step G, formula used is C1=(I b) * X (t), then X '=C0/ (I (tc0)-b)；More by tc ' simultaneously
New be tc0, and wherein, C0 is the analyte concentration value calibrated, and I (tc0) is that range calibration time of origin is recent to be recorded point
Analysing thing electric current, the time that I (tc0) occurs differed with tc0 less than 5 minutes.
Step I, X ' and tc ' numerical value are imported related algorithm and by the result of ac impedance measurement to its compensate with
Revise, and appearance is calibrated in wait, then repeats step H next time.Wherein, X ' and tc ' numerical value are imported related algorithm and pass through
It is compensated and revises by the result of ac impedance measurement, as it is shown in figure 5, specifically include following steps:
Step J, first determine whether whether up-to-date prover time is later than the up-to-date ac impedance measurement time once, if
It is then to complete step K, does not perform any compensation correction directly output conversion coefficient X=X '；If it is not, then complete step L, read
Take away from calibration time of origin recent ac impedance measurement value Zre_cal and Zim_cal, enter step M；Step L reads
During calibration, resistance value can also be carried out after step M judged result is for being before performing step N.
Step M, first determine whether current impedance measurements Zre and Zim the most all in preset range, if it is not, then
System being judged as operation irregularity, stops display result of calculation and show information warning, shown information warning can also be
Prompting sensor user carries out the newest calibration and whether the difference according to calibration result with expected results determines sensor
Still work in acceptable precision；If it is, operating procedure N, calculate present impedance value Zre and Zim and number during calibration
The difference of value Zre_cal and Zim_cal, draws dZre=Zre Zre_cal and dZim=Zim Zim_cal.
Step O, judge the absolute difference of resistance value whether exceeded preset drift threshold dZre_thres and dZim_
Thres, if it is not, then complete step K, does not compensates and corrects conversion coefficient, if it is, carry out subsequent step P；Step
The maximum allowable positive and negative discrepancy threshold used in O is identical, the most only need to compare absolute value and the dZre_thres of dZre, dZim,
dZim_thres.Its replacement scheme can be that maximum allowable positive and negative discrepancy threshold is different, now dZre or dZim be on the occasion of, then need
Judge whether, more than its corresponding maximum allowable positive variance threshold value, then to need if negative value to judge whether less than maximum allowable
Negative variance threshold value.
Step P, contain the directivity of four conditional judgments difference dZre and dZim to compare impedance measured value, the most right
Conversion coefficient X ' makees corresponding correction, and these judgements there will be 5 kinds of possible results, respectively altogether:
A) dZre and dZim is just being and more than corresponding threshold value；Now perform step Q, conversion coefficient X ' is carried out increase and repaiies
Just, concrete mode is to be multiplied by equation h (Zre/Zre_cal, a Zim/ relevant to impedance real part and imaginary part institute measured value
Zim_cal), the result of this equation is naturally larger than 1；One specific embodiment be h (Zre/Zre_cal, Zim/Zim_cal)=
Zre/Zre_cal+Zim/Zim_cal–1。
B) dZre for just and more than dZre_thres threshold value but dZim is not more than dZim_thres threshold value；Now perform step
R, carries out conversion coefficient X ' increasing and revises, and concrete mode is to be multiplied by an equation closed with impedance real part numerical difference out-phase
J (Zre/Zre_cal), the result of this equation is naturally larger than 1；One specific embodiment is j (Zre/Zre_cal)=Zre/
Zre_cal。
C) dZre is for bearing and less than negative dZre_thres threshold value, now performs step S, conversion coefficient X ' is carried out reduction and repaiies
Just, concrete mode is to be multiplied by an equation k (Zre/Zre_cal) relevant to impedance real part numerical value, the result of this equation
Certainly less than 1；One specific embodiment is k (Zre/Zre_cal)=Zre/Zre_cal.
D) in positive and negative dZre_thres threshold range but dZim is just and to be more than dZim_thres threshold value to dZre, now holds
Row step T, carries out conversion coefficient X ' increasing and revises, and concrete mode is closed with imaginary impedance numerical difference out-phase for being multiplied by one
Equation m (Zim/Zim_cal), the result of this equation is naturally larger than 1；One specific embodiment be m (Zim/Zim_cal)=
Zim/Zim_cal。
E) in positive and negative dZre_thres threshold range but dZim is for bearing and less than negative dZim_thres threshold value, now for dZre
Performing step U, carry out conversion coefficient X ' reducing and revise, concrete mode is for being multiplied by one and imaginary impedance numerical difference out-phase
The equation n (Zim/Zim_cal) closed, the result of this equation is certainly less than 1；One specific embodiment is n (Zim/Zim_cal)
=Zim/Zim_cal.
Obtain revising conversion coefficient X or not revising as performed step K, X conduct after X ' is done compensating approach
The output of this some algorithm is given to step G in order to computational analysis concentration value.After step P completes, system can be passed through simultaneously
Sending an information warning to sensor user, prompting sensor is in non-optimal duty, needs to re-start calibration.
Claims (10)
1. one kind can the electrochemical analyte sensor-based system of self-correction interference signal, it is characterised in that include sensor body, straight
Stream power voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, controller, data process and logical
News parts, power supply,
Sensor body, including working electrode, reference electrode, to electrode and blank electrode；
DC-voltage supply parts, including two independent parallel circuits, apply relative to working electrode with blank electrode respectively
In the voltage that reference electrode is identical, to excite corresponding analyte electrochemical reaction current and chaff interference kinetic current；
Current measuring members, including two independent current measuring members, measures working electrode respectively and blank electrode is passed through
Electric current and the numerical value recorded be sent to data process and communication component；
Ac impedance measurement parts, solid for applying one while applying DC voltage to working electrode or blank electrode again
Determine the alternating voltage of frequency, then measure working electrode or the corresponding current response of blank electrode and calculate its corresponding alternating current
Impedance, is then sent to output result data and processes and communication component；
Circuit changing switch, for cutting working electrode between corresponding current measuring members and ac impedance measurement parts
Changing, opportunity and the frequency of switching are determined by the instruction of controller；Or for blank electrode at corresponding current measuring members and
Switching between ac impedance measurement parts, opportunity and the frequency of switching are determined by the instruction of controller；
Controller, for timing, controls sampling time and the frequency of current measuring members, during the sampling of ac impedance measurement parts
Between and frequency, the state of circuit changing switch, and data process and communication component process and transmission data opportunity；
Data process and communication component, the output result obtained from current measuring members and ac impedance measurement parts are transported
Calculate, thus draw analyte concentration and send the result to receive terminal；
Power supply, to DC-voltage supply parts, current measuring members, ac impedance measurement parts, circuit changing switch, controls
Device, data process and communication component provides the electric energy needed for running；
DC-voltage supply element outputs connects with working electrode, blank electrode respectively；Blank electrode outfan and its correspondence
Current measuring members connect, working electrode and circuit changing switch connect, and circuit changing switch is right with work electricity level the most respectively
Current measuring members, the ac impedance measurement parts answered connect, or the current measuring members of working electrode and its correspondence connects, empty
White appliances pole and circuit changing switch connect, and corresponding with the blank electrode the most respectively current measuring members of circuit changing switch, exchange
Impedance measurement parts connect；Controller output end is opened with current measuring members, ac impedance measurement parts, circuit switching respectively
Close, data process and communication component connects, and current measuring members, ac impedance measurement parts process and communication section with data respectively
Part input connects, and power output end connects with DC-voltage supply parts, controller respectively.
The most according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, it is characterised in that work
Having the oxidoreductase just for analyte or redox couple medium as electrode face finish, blank electrode is except without pin
Outside modifying the oxidoreductase of analyte or redox couple medium, remaining attribute is all identical with blank electrode；Work electricity
Pole and blank electrode position on a sensor is adjacent, and the beeline between two electrodes is less than 5 millimeters.
The most according to claim 2 can self-correction interference signal electrochemical analyte sensor-based system, it is characterised in that work
Make cover layer in electrode and blank electrode.
The most according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, it is characterised in that hand over
It is 100kHz-1kHz that flow impedance measures the frequency of parts alternating voltage, and the output of ac impedance measurement parts impedance measurement includes
The resistance value of impedance and phase place or the real part of impedance and imaginary part.
The most according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, it is characterised in that work
The current measurement sample frequency making electrode exceeds ac impedance measurement sample frequency more than 10 times.
6. one kind can self-correction interference signal electrochemical analyte method for sensing, it is characterised in that comprise the steps:
Step one, apply the voltage identical relative to reference electrode to working electrode and blank electrode respectively, corresponding to excite
Analyte electrochemical reaction current and chaff interference kinetic current, measured by corresponding current measuring members respectively, and recording
Numerical value be sent to data process and communication component；AC impedance parts are applying DC voltage to working electrode or blank electrode
While apply the alternating voltage of a fixed frequency again, then measure working electrode or the corresponding current response of blank electrode also
Calculate its corresponding alternating current impedance, then output result is sent to data and processes and communication component；
Step 2, data process and communication component utilizes the output knot obtained from current measuring members and ac impedance measurement parts
Fruit carries out computing, thus draws analyte concentration and send the result to receive terminal.
The most according to claim 6 can self-correction interference signal electrochemical analyte method for sensing, it is characterised in that step
Computing in rapid two comprises 1 input data point, 9 input message sequences and 2 output information sequences, 1 input data point
For: system initial time t0,9 input message sequences are: working electrode sample rate current sequence I1, working electrode sampling time sequence
Row t1, blank electrode sample rate current sequence I2, blank electrode sampling time sequence t2, impedance real part sequence Zre, imaginary impedance sequence
Row Zim, impedance sampling time sequence tZ, calibrate analyte concentration sequence C 0, calibrate analyte time tc0,2 output information sequences
It is classified as: measure analyte concentration sequence C 1, measures time tc1；After sensor-based system is energized first and starts, system is recorded and is opened
Dynamic time t0, and start simultaneously at sample rate current I1, I2 and sampling time t1, t2 of writing task electrode and blank electrode；T2 adopts
The sample time is less than 1 minute before and after t1；
Specifically include following steps:
Step A, first determine whether whether current run time T=(t1 t0) alreadys more than default running life Tmax, if sentenced
Be set to and be, then out of date needs of system prompt sensor is changed；If it is determined that no, then operating procedure B；
Step B, judge whether the operation time has exceeded the initialization time preset, if it is, operating procedure C；If it is not, then
In prompting sensor initializing, wait the next current sample time, then repeat step A；
Step C, responsible execution use measurement current value computational analysis substrate concentration, first reading writing task electrode and blank electrode
Sample rate current I1, I2 and sampling time t1, t2 start computing；
Step D and E, Filtering Processing reduce noise and interference, and data obtain electric current I1 ', I2 ' and the time processed after processing
t1’、t2’；
Step F, the signal in blank electrode is deducted from working electrode currents, obtains analyte current I=I1 '-I2 ', from
And eliminate the current signal that chaff interference produces；Simultaneously by the information of comprehensive t1 ' and t2 ', obtain corresponding to analyte current
Time t=(t1'+t2')/2；
Step G, use analyte current I and up-to-date conversion coefficient X, calculate the concentration C 1 of institute's cls analysis thing；Formula used
For C1=f (I, X), simultaneously retention analysis substrate concentration correspondence time tc1=t, analyte concentration calculated after etc. to be obtained newly
Current sample and repeat step A.
The most according to claim 7 can self-correction interference signal electrochemical analyte method for sensing, it is characterised in that step
In rapid G, up-to-date conversion coefficient X comprises the steps to obtain: checks whether sensor-based system passes through to calibrate and calculate not compensate and repaiies
Positive conversion coefficient X ' and corresponding nearest prover time tc ', X ' and tc ' numerical value are imported related algorithm and pass through AC impedance
It is compensated and revises by the result measured；
Specifically include following steps:
Step H, first check whether to there is recent calibration, if it did not, system will use the conversion coefficient X ' preset
=X0, prover time is calculated as 0；If it has, then calculate X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f (I, X)
Inverse operation；Tc ' being updated to tc0, wherein, C0 is the analyte concentration value of calibration simultaneously, and I (tc0) is that range calibration occurs
The time recent analyte current that records, the time that I (tc0) occurs differs less than 5 minutes with tc0；
Step I, X ' and tc ' numerical value are imported related algorithm and passes through the result of ac impedance measurement and it is compensated and repaiies
Just, and wait and calibrate appearance next time, then repeat step H；
Wherein, X ' and tc ' numerical value are imported related algorithm and pass through the result of ac impedance measurement and it is compensated and revises,
Specifically include following steps:
Step J, first determine whether whether up-to-date prover time is later than the up-to-date ac impedance measurement time once, if it is,
Complete step K, do not perform any compensation correction directly output conversion coefficient X=X '；If it is not, then complete step L, read away from school
Quasi-time of origin recent ac impedance measurement value Zre_cal and Zim_cal, enter step M；
Step M, first determine whether current impedance measurements Zre and Zim the most all in preset range, if it is not, then will system
System is judged as operation irregularity, stops display result of calculation and shows information warning；If it is, operating procedure N, calculate current resistance
The difference of numerical value Zre_cal and Zim_cal when anti-value Zre and Zim and calibration, draws dZre=Zre Zre_cal and dZim
=Zim Zim_cal；
Step O, judge the absolute difference of resistance value whether exceeded preset drift threshold dZre_thres and dZim_
Thres, if it is not, then complete step K, does not compensates and corrects conversion coefficient, if it is, carry out subsequent step P；
Step P, contain the directivity of four conditional judgments difference dZre and dZim to compare impedance measured value, then to conversion
Coefficient X ' makees corresponding correction, and these judgements there will be 5 kinds of possible results, respectively altogether:
A) dZre and dZim is just being and more than corresponding threshold value；Now perform step Q, carry out conversion coefficient X ' increasing and revise,
Concrete mode is to be multiplied by equation h (Zre/Zre_cal, a Zim/Zim_ relevant to impedance real part and imaginary part institute measured value
Cal), the result of this equation is naturally larger than 1；
B) dZre for just and more than dZre_thres threshold value but dZim is not more than dZim_thres threshold value；Now perform step R, right
Conversion coefficient X ' carries out increasing correction, and concrete mode is to be multiplied by an equation j closed with impedance real part numerical difference out-phase
(Zre/Zre_cal), the result of this equation is naturally larger than 1；
C) dZre is for bearing and less than negative dZre_thres threshold value, now performs step S, carries out conversion coefficient X ' reducing correction,
Concrete mode is to be multiplied by an equation k (Zre/Zre_cal) relevant to impedance real part numerical value, and the result of this equation is inevitable
Less than 1；
D) in positive and negative dZre_thres threshold range but dZim is just and to be more than dZim_thres threshold value to dZre, now performs step
Rapid T, carries out conversion coefficient X ' increasing and revises, and concrete mode is to be multiplied by a side closed with imaginary impedance numerical difference out-phase
Journey m (Zim/Zim_cal), the result of this equation is naturally larger than 1；
E) in positive and negative dZre_thres threshold range but dZim is for bearing and less than negative dZim_thres threshold value, now performing for dZre
Step U, carries out conversion coefficient X ' reducing and revises, and concrete mode is to be multiplied by one to close with imaginary impedance numerical difference out-phase
Equation n (Zim/Zim_cal), the result of this equation is certainly less than 1；
Obtaining revising conversion coefficient X or not revising as performed step K after X ' is done compensating approach, X is as this portion
The output dividing algorithm is given to step G in order to computational analysis concentration value.
The most according to claim 8 can self-correction interference signal electrochemical analyte method for sensing, it is characterised in that step
When rapid L reads calibration, resistance value is after step M judged result is for being, carries out before performing step N.
The most according to claim 8 can self-correction interference signal electrochemical analyte method for sensing, it is characterised in that
After step P completes, sending an information warning by system to sensor user, prompting sensor is in non-optimal work simultaneously
Make state, need to re-start calibration.
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