CN106290530B - It is a kind of can self-correction interference signal electrochemical analyte sensor-based system and method - Google Patents
It is a kind of can self-correction interference signal electrochemical analyte sensor-based system and method Download PDFInfo
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Abstract
The invention discloses it is a kind of can self-correction interference signal electrochemical analyte sensor-based system, including sensor body, DC-voltage supply component, current measuring members, ac impedance measurement component, circuit changing switch, controller, data processing and communication component, power supply.A blank electrode identical with working electrode size is added, interference signal is eliminated by way of signal subtraction.An ac impedance measurement component is added, its system impedance value exported is used in combination to judge the working condition of sensor.The influence generated to analyte signal by the presence of chaff interferent and measuring environment variation can be effectively eliminated, sensor is made to ensure the validity and accuracy of measuring signal during operation.
Description
Technical field
The present invention relates to analyte sensing system technical fields, and in particular to it is 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 basic functional principle is by sensor
Apply suitable voltage or electric current on working electrode, converting the chemical analyte measured in sample to by electrochemical reaction can
The electric signal of detection.There are all types of biosensors for multiple analytes, wherein most study, most on the market at present
Common biosensor is current mode (ampere-type) glucose sensor, for successfully controlling the glucose water of diabetes
It is very important for flat.
Traditional amperometric glucose sensor is using the glucose oxidase being fixed on sensor electrode in sample
The glycoxidative generation gluconic acid of grape and by-product hydrogen peroxide, then hydrogen peroxide is aoxidized on working sensor electrode from
And generate detectable current signal.Similar therewith, the reaction occurred in a variety of oxidoreducing enzyme being known in the art is
It is used for the amperometric sensor design based on same operation principle.
One common problem of electrochemical sensor is them not only (or can have the analyte with analyte to be measured
Enzymatic reaction by-product) be electrochemically reacted, but also can be not intended to other measured electroactive chemical species into
It goes and reacts, due to these " interference species ", this reaction for being not intended to be measured causes signal strength to increase, to influence to dividing
Analyse the accurate judgement of object concentration.For example, in traditional amperometric glucose sensor based on glucose oxidase, it is known that all
As the interference species of acetaminophen, ascorbate and lithate etc obscure real analyte signal.
In addition, the signal that traditional amperometric electrochemical sensor is obtained also can be by the measuring environment residing for sensor
Change is influenced, these situations include but not limited to that the electro-chemical activity of sensor electrode decorative layer weakens, and dehydration or decomposition are de-
It falls, sensor is combined the displacement etc. from detection environment of the impermeable stratum covering formed and sensor by nonspecific proteins.By
The signal source of its working electrode can not be told 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 to carry out self-test, differentiate and exclude non-analysis
The solution of the signal of object, wherein non-analyte signal includes chaff interferent signal and electrode perimeter environmental signal etc..Currently, needle
The exclusion of chaff interferent signal is mainly solved by increasing AF panel diaphragm in working sensor electrode surface, working machine
System is that the chaff interferent different from analyte is isolated using diaphragm physicochemical characteristics, makes it can not contact sensor electrode surface hair
Raw electrochemical reaction.Common scheme includes that the pore size of adjustment diaphragm is isolated by macromolecular chaff interference, and utilizes diaphragm material
Material and water contact generate repelling effect in the positive charge or negative electrical charge of strand institute band to the chaff interferent molecule with identical charges
Deng.And the judgement of environmental signal is usually generated by absolute figure to signal code and rate of change analysis, for example, when letter
It, can when number value is apparently higher than significantly lower than normal range (NR) or signal intensity rate because of normal analyte concentration rate of change
To think that sensor measurement data fails, need to recalibrate sensor or stop sensor work.Above two interference signal
It excludes and the solution of environmental signal exclusion also combines application often.
Both existing schemes have certain limitation.For the exclusion of interference signal, AF panel diaphragm is answered
High, the complex process with not only manufacturing cost, and can only be effective to specific a kind of chaff interferent.Such as by adjusting pore size
Chaff interferent than analyte molecule bigger can only be excluded, and cannot exclude and analyte molecule size is similar or smaller interference
Object;Equally, charge exclusive method can only also exclude with analyte electrically charged opposite chaff interferent, and cannot exclude neutrality or with
The chaff interferent of the same charge of analyte band.For the exclusion of measuring environment effect of signals, the absolute number of sensor electric signal is used
Value is analyzed and rate of change analysis is only capable of excluding extreme case, and cannot differentiate or exclude the smaller measuring environment variation of amplitude
It influences.In this case, the accuracy of sensor can still be affected, it is therefore desirable to periodically be calibrated to adjust electric current letter
Correlation number between analyte concentration ensures accuracy, and which increases the use difficulty of sensor, eases of use
It is deteriorated.
Invention content
It is an object of the present invention to provide it is a kind of can self-correction interference signal electrochemical analyte sensor-based system and method, with solution
Certainly the deficiencies in the prior art.
The present invention uses following technical scheme:
It is a kind of can self-correction interference signal electrochemical analyte sensor-based system, including sensor body, DC voltage supply
Electrical components, current measuring members, ac impedance measurement component, circuit changing switch, controller, data processing and communication component,
Power supply,
Sensor body, including working electrode, reference electrode, to electrode and blank electrode;
DC-voltage supply component, including two independent parallel circuits apply to working electrode and blank electrode respectively
Relative to the identical voltage of reference electrode, to excite corresponding analyte electrochemical reaction current and chaff interferent kinetic current;
Current measuring members, including two independent current measuring members measure working electrode and blank electrode institute respectively
By electric current and the numerical value measured is sent to data processing and communication component;
Ac impedance measurement component, for applying one again while applying DC voltage to working electrode or blank electrode
Then the alternating voltage of a fixed frequency measures working electrode or the corresponding current response of blank electrode and calculates its corresponding friendship
Then output result is sent to data processing and communication component by galvanic electricity impedance;
Circuit changing switch is used for working electrode between corresponding current measuring members and ac impedance measurement component
Switching, the opportunity of switching and frequency are determined by the instruction of controller;Or it is used for blank electrode in corresponding current measuring members
Switch between ac impedance measurement component, the opportunity of switching and frequency are determined by the instruction of controller;
Controller is used for timing, controls sampling time and the frequency of current measuring members, ac impedance measurement component is adopted
The opportunity of sample time and frequency, the state of circuit changing switch and data processing and communication component processing and transmission data;
Data processing and communication component, by from the output result that current measuring members and ac impedance measurement component obtain into
Row operation, to obtain analyte concentration and send the result to reception terminal;
Power supply gives DC-voltage supply component, current measuring members, ac impedance measurement component, circuit changing switch, control
Device processed, data processing and communication component provide the electric energy needed for operation;
DC-voltage supply element outputs are connected with working electrode, blank electrode respectively;Blank electrode output end and its
Corresponding current measuring members connection, working electrode are connected with circuit changing switch, and circuit changing switch is electric with work respectively again
The corresponding current measuring members of grade, the connection of ac impedance measurement component or working electrode current measuring members corresponding with its connect
Connect, blank electrode is connected with circuit changing switch, circuit changing switch again respectively with blank electrode corresponding current measuring members,
Ac impedance measurement component connects;Controller output end switches with current measuring members, ac impedance measurement component, circuit respectively
Switch, data processing connected with communication component, current measuring members, ac impedance measurement component respectively with data processing and communication
Part input connects, and power output end is connected with DC-voltage supply component, controller respectively.
Further, working electrode surface is modified with oxidoreducing enzyme or redox couple medium just for analyte,
Blank electrode in addition to without for analyte oxidoreducing enzyme or redox couple medium modify other than, remaining attribute with
Blank electrode is identical;The position of working electrode and blank electrode on a sensor is adjacent, and the shortest distance 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 component alternating voltage is 100kHz-1kHz, ac impedance measurement component
The output of impedance measurement includes the impedance value and phase or the real and imaginary parts of impedance of impedance.
Further, the current measurement sample frequency of working electrode is higher by 10 times of ac impedance measurement sample frequency or more.
It is a kind of can self-correction interference signal electrochemical analyte method for sensing, include the following steps:
Step 1: applying respectively to working electrode and blank electrode relative to the identical voltage of reference electrode, to excite phase
The analyte electrochemical reaction current and chaff interferent kinetic current answered, are measured by corresponding current measuring members, and handle respectively
The numerical value measured is sent to data processing and communication component;AC impedance component is applying direct current to working electrode or blank electrode
Apply the alternating voltage of a fixed frequency while voltage again, then measures working electrode or the corresponding electric current of blank electrode is anti-
Its corresponding alternating current impedance should and be calculated, output result is then sent to data processing and communication component;
Step 2: data processing and communication component are defeated using being obtained from current measuring members and ac impedance measurement component
Go out result and carry out operation, to obtain analyte concentration and send the result to reception terminal.
Further, the operation in step 2 includes 1 input data point, 9 input message sequences and 2 output informations
Sequence, 1 input data point are:T0,9 input message sequence of system initial time be: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, when calibrating analyte
Between tc0,2 output information sequences are:Measure analyte concentration sequence C 1, time of measuring tc1;When sensor-based system is powered simultaneously for the first time
After startup, system records startup time t0, and start simultaneously at record working electrode and blank electrode sample rate current I1, I2 and
Sampling time t1, t2;The t2 sampling times are no more than 1 minute before and after t1;
Specifically comprise the following steps:
Step A, first determine whether current run time T=(t1-t0) alreadys exceed preset running life Tmax, such as
Fruit is determined as that then system prompt sensor is out of date needs replacing;If it is determined that no, then operating procedure B;
Step B, judge whether run time has been more than preset initialization time, if it is, operating procedure C;If
It is no, then it prompts in sensor initializing, waits for next current sample time, then repeatedly step A;
Step C, it is responsible for executing with current value calculating analyte concentration is measured, reads record working electrode and blank electricity first
Sample rate current I1, I2 and sampling time t1, t2 of pole start operation;
Step D and E, be filtered and reduce noise and interference, obtained after data processing processed electric current I1 ', I2 ' and when
Between t1 ', t2 ';
Step F, the signal in blank electrode is subtracted from working electrode currents, obtains analyte current I=I1 '-
I2 ', to eliminate the current signal of chaff interferent generation;Simultaneously by the information of comprehensive t1 ' and t2 ', analyte current is obtained
Corresponding time t=(t1'+t2')/2;
Step G, using analyte current I and newest conversion coefficient X, the concentration C 1 of surveyed analyte is calculated;It is used
Formula is C1=f (I, X), while retention analysis object concentration corresponds to time tc1=t, and analyte concentration is waited for after the completion of calculating and being obtained
It takes new current sample and repeats step A.
Further, newest conversion coefficient X includes the following steps to obtain in step G:Check whether sensor-based system passes through
The conversion coefficient X ' and corresponding nearest prover time tc ' for calibrating and calculating non-compensating approach, by X ' and tc ' numerical value import phase
It closes algorithm and it is compensated and is corrected by the result of ac impedance measurement;
Specifically comprise the following steps:
Step H, it first checks whether there are recent calibration, if not provided, system will use preset conversion system
Number X '=X0, prover time are calculated as 0;If so, then calculating X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f
The inverse operation of (I, X);Tc ' is updated to tc0 simultaneously, wherein C0 is the analyte concentration value of calibration, and I (tc0) is range calibration
Time of origin is recent to measure analyte current, and the time that I (tc0) occurs differs with tc0 to be no more than 5 minutes;
Step I, by X ' and tc ' numerical value import related algorithm and it is compensated by the result of ac impedance measurement and
It corrects, and calibration next time is waited for occur, then repeatedly step H;
Wherein, by X ' and tc ' numerical value import related algorithm and it is compensated by the result of ac impedance measurement and
It corrects, specifically comprises the following steps:
Step J, first determine whether newest prover time is later than the newest primary ac impedance measurement time, if
It is then to complete step K, conversion coefficient X=X ' is directly exported without any compensating approach;If it is not, then completing step L, read
It takes away from the calibration recent ac impedance measurement value Zre_cal and Zim_cal of time of origin, enters step M;
Step M, current impedance measurements Zre and Zim are first determined whether within a preset range, if it is not, then
System is judged as operation irregularity, stop showing result of calculation and shows information warning;If it is, operating procedure N, calculating are worked as
Preceding impedance value Zre and Zim with calibration when numerical value Zre_cal and Zim_cal difference, obtain dZre=Zre-Zre_cal and
DZim=Zim-Zim_cal;
Step O, judge whether the absolute difference of impedance value has been more than preset drift threshold dZre_thres and dZim_
Thres does not compensate and correct conversion coefficient if it is not, then completing step K, if it is, carrying out subsequent step P;
Step P, four condition judgments are contained compare impedance measured value difference dZre and dZim directionality, it is then right
Conversion coefficient X ' make it is corresponding correct, these judgements will appear in total 5 kinds it is possible as a result, being respectively:
A) dZre and dZim is just and more than corresponding threshold value;Step Q is executed at this time, and conversion coefficient X ' increase and is repaiied
Just, concrete mode is is multiplied by one and impedance real part and relevant equation h (Zre/Zre_cal, the Zim/ of imaginary part institute measured value
Zim_cal), the result of this equation is naturally larger than 1;
B) dZre is just and more than dZre_thres threshold values but dZim to be not more than dZim_thres threshold values;Step is executed at this time
R carries out increase amendment to conversion coefficient X ', and concrete mode is to be multiplied by one and the different relevant equation of impedance real part numerical difference
J (Zre/Zre_cal), the result of this equation are naturally larger than 1;
C) dZre is negative and less than negative dZre_thres threshold value, executes step S at this time, to conversion coefficient X ' reduce and repair
Just, concrete mode is to be multiplied by one and the relevant equation k (Zre/Zre_cal) of impedance real part numerical value, the result of this equation
Certainly less than 1;
D) dZre is in positive and negative dZre_thres threshold ranges but dZim is just and to be more than dZim_thres threshold values, holds at this time
Row step T carries out increase amendment to conversion coefficient X ', and concrete mode is to be multiplied by one to close with imaginary impedance numerical difference out-phase
Equation m (Zim/Zim_cal), the result of this equation is naturally larger than 1;
E) dZre is in positive and negative dZre_thres threshold ranges but dZim is negative and is less than negative dZim_thres threshold values, at this time
Step U is executed, reduction amendment is carried out to conversion coefficient X ', concrete mode is to be multiplied by one and imaginary impedance numerical difference out-phase
The equation n (Zim/Zim_cal) of pass, the result of this equation is certainly less than 1;
It obtains correcting conversion coefficient X after X ' to be done to compensating approach or not corrected if executing step K, X conducts
The output of this some algorithm is given to step G to calculate analyte concentration value.
Further, impedance value is after step M judging results are to be when step L reads calibration, before executing step N
It carries out.
Further, after the completion of step P, while an information warning is sent to sensor user by system, prompted
Sensor is in non-optimal working condition, needs to re-start calibration.
Beneficial effects of the present invention:
1, the present invention propose it is a kind of can self-correction interference signal electrochemical analyte sensor-based system, can effectively disappear
Except the influence generated to analyte signal by the presence of chaff interferent and measuring environment variation, sensor is made to ensure during operation
The validity and accuracy of measuring signal.This scheme is suitable for all containing oxidoreducing enzyme or redox couple medium
The amperometric electrochemical sensor of (redox couple medium), typical case can be a kind of containing glucose oxidase
The subcutaneous matter interstitial fluid glucose sensor of implanted human body, but be not limited only to such application.
2, a blank electrode identical with working electrode size is added in the present invention in sensor systems, passes through signal phase
The mode subtracted eliminates interference signal.Compared with increasing on a sensor, the manufacture of AF panel diaphragm is easier, and to chaff interferent point
Son can effectively eliminate signal caused by any kind of chaff interferent without selectivity.
3, an ac impedance measurement component is added in the present invention in sensor systems, the system impedance value for being used in combination it to export
Judge the working condition of sensor.Ac impedance measurement is a kind of independent with analyte concentration within the scope of suitable a-c cycle
Electrochemical measuring method, whether can accurately measure has notable environmental change around sensor.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 do not change
Become, AC impedance real part numerical value can also decline because of the aqueous increase of sensor senses layer at this time, therefore can be from its impedance
Change to correct the analyte concentration measured.Similarly, it is covered if sensor is had the nonspecific protein of barriering effect to combine
Lid, analyte diffusion hindered make sensor current reduce;AC impedance real part numerical value can increase at this time, therefore can be according to resistance
Anti- increased degree increases electric current-analyte concentration conversion coefficient, the signal reduced to modifying factor analyte diffusion hindered.?
Under extreme case, sensor is damaged or is fallen off because of external force collision, is no longer in detection environment, at this time ac impedance measurement
It can show the huge numerical value of exception, be more than preset normal range (NR), therefore can determine that sensor loses according to AC impedance
Effect reminds user to pay attention to.So using ac impedance measurement can than merely use working electrode measure electric current numerical value and
Change rate analyzes the state for more effectively indicating working electrode, and can be modified as the case may be, reduces to calibration
Demand.
4, the present invention establishes output of a set of algorithm using the result point situation of ac impedance measurement to sensing system
As a result it compensates and corrects, improve the accuracy of output result and prompt letter is exported to sensor user in due course
Breath is so as to the necessary change of sensing system progress or calibration.
Description of the drawings
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 processing and communication component utilize the output obtained from current measuring members and ac impedance measurement component
As a result the flow diagram of operation is carried out.
Fig. 4 be check sensor-based system whether through calibration and calculate non-compensating approach conversion coefficient X ' and it is corresponding most
The flow diagram of nearly prover time tc '.
Fig. 5 be by the result of ac impedance measurement to conversion coefficient X ' and the corresponding nearest calibration of non-compensating approach when
Between tc ' compensate and modified flow diagram.
Specific implementation mode
The present invention is done with reference to embodiment and attached drawing and is further explained.The following example is merely to illustrate this hair
It is bright, but be not used to limit the practical range of the present invention.
It is a kind of can self-correction interference signal electrochemical analyte sensor-based system, as depicted in figs. 1 and 2, including sensor
Ontology, DC-voltage supply component, current measuring members, ac impedance measurement component, circuit changing switch, controller, data
Processing and communication component, power supply.
Sensor body, including working electrode, reference electrode, to electrode and blank electrode;Working electrode surface is modified with
Oxidoreducing enzyme just for analyte or redox couple medium can also cover one layer and protect the thin of decorative layer under normal conditions
Film layer;Blank electrode in addition to without for analyte oxidoreducing enzyme or redox couple medium modify other than, remaining category
Property (such as electrode material, surface area size, shape and thinfilm protective coating etc.) is identical as blank electrode;Working electrode and
The position of blank electrode on a sensor is adjacent, and the shortest distance between two electrodes is no more than 5 millimeters.As one kind containing glucose
The subcutaneous matter interstitial fluid glucose sensor of implanted human body of oxidizing ferment, there are one the working electrodes of 0.5mmx0.5mm for sensor strip
With the blank electrode of a 0.5mmx0.5mm, 10 microns of thick glucose oxidases and 50 micro- are wherein covered on working electrode
The thick non-biocompatible thin film's layer of rice, and blank electrode is just coated with 50 microns thick of non-biocompatible thin film's layer.Two electrodes
The shortest distance of border is 2mm.
DC-voltage supply component, including two independent parallel circuits apply to working electrode and blank electrode respectively
Relative to the identical voltage of reference electrode, to excite corresponding analyte electrochemical reaction current and chaff interferent kinetic current.
Current measuring members, including two independent current measuring members measure working electrode and blank electrode institute respectively
By electric current and the numerical value measured is sent to data processing and communication component.
Ac impedance measurement component, for applying one again while applying DC voltage to working electrode or blank electrode
Then the alternating voltage of a fixed frequency measures working electrode or the corresponding current response of blank electrode and calculates its corresponding friendship
Then output result is sent to data processing and communication component by galvanic electricity impedance.The frequency selection of alternating voltage can be according to electricity
The size of pole, shape, depending on the modification situation of electrode surface, it will usually in 100kHz between 1kHz.Contain glucose above-mentioned
In the subcutaneous matter interstitial fluid glucose sensor of implanted human body of oxidizing ferment, the frequency of alternating voltage is 1kHz.Impedance measurement it is defeated
Go out can be including both sides information impedance impedance value (Z) and phase (Φ), can also be the real part (Z of impedanceRe) and it is empty
Portion (ZIm).The transformational relation of impedance value/phase 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 component
Switching, the opportunity of switching and frequency are determined by the instruction of controller;Or it is used for blank electrode in corresponding current measuring members
Switch between ac impedance measurement component, the opportunity of switching and frequency are determined by the instruction of controller.
Controller is used for timing, controls sampling time and the frequency of current measuring members, ac impedance measurement component is adopted
The opportunity of sample time and frequency, the state of circuit changing switch and data processing and communication component processing and transmission data;Its
Middle impedance measure sample frequency be much smaller than current sample frequency, preferred current sample frequency specific impedance measurement be higher by 10 times with
On, such as current sample frequency is 1 time per minute, every 15 minutes 1 time of impedance sampling.The measurement frequency of ac impedance measurement component
It is formulated by the presupposed solution of controller and less than the measurement frequency of working electrode or blank electrode electric current.A kind of alternative is to make
With working electrode or blank electrode measure electric current as a result, especially its rate of change decide whether active circuit switching switch and
Ac impedance measurement component ensures system normal operation to ensure timely to provide impedance information.
Data processing and communication component, by from the output result that current measuring members and ac impedance measurement component obtain into
Row operation, to obtain analyte concentration and send the result to reception terminal.
Power supply gives DC-voltage supply component, current measuring members, ac impedance measurement component, circuit changing switch, control
Device processed, data processing and communication component provide the electric energy needed for operation.
DC-voltage supply element outputs are connected with working electrode, blank electrode respectively;Blank electrode output end and its
Corresponding current measuring members connection, working electrode are connected with circuit changing switch, and circuit changing switch is electric with work respectively again
The corresponding current measuring members of grade, the connection of ac impedance measurement component or working electrode current measuring members corresponding with its connect
Connect, blank electrode is connected with circuit changing switch, circuit changing switch again respectively with blank electrode corresponding current measuring members,
Ac impedance measurement component connects.Controller output end switches with current measuring members, ac impedance measurement component, circuit respectively
Switch, data processing connected with communication component, current measuring members, ac impedance measurement component respectively with data processing and communication
Part input connects, and power output end is connected with DC-voltage supply component, controller respectively.
It is a kind of can self-correction interference signal electrochemical analyte method for sensing, include the following steps:
Step 1: applying respectively to working electrode and blank electrode relative to the identical voltage of reference electrode, to excite phase
The analyte electrochemical reaction current and chaff interferent kinetic current answered, are measured by corresponding current measuring members, and handle respectively
The numerical value measured is sent to data processing and communication component;AC impedance component is applying direct current to working electrode or blank electrode
Apply the alternating voltage of a fixed frequency while voltage again, then measures working electrode or the corresponding electric current of blank electrode is anti-
Its corresponding alternating current impedance should and be calculated, output result is then sent to data processing and communication component.
Step 2: data processing and communication component are defeated using being obtained from current measuring members and ac impedance measurement component
Go out result and carry out operation, to obtain analyte concentration and send the result to reception terminal;The operation includes 1 input data
Point, 9 input message sequences and 2 output information sequences, 1 input data point are:T0,9 input letter of system initial time
Ceasing 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,
Analyte concentration sequence C 0 is calibrated, analyte time tc0 is calibrated, 2 output information sequences are:Measure analyte concentration sequence
C1, time of measuring tc1;As shown in figure 3, after sensor-based system is powered and starts for the first time, system records startup time t0, and same
When start recording working electrode and blank electrode sample rate current I1, I2 and sampling time t1, t2;The t2 sampling times are before and after t1
It is specific such as t1=t2 no more than 1 minute.
Specifically comprise the following steps:
Step A, first determine whether current run time T=(t1-t0) alreadys exceed preset running life Tmax (examples
Such as 5 days), if it is decided that it is yes, then system prompt sensor is out of date needs replacing;If it is determined that no, then operating procedure B.
Step B, judge whether run time has been more than preset initialization time (such as 30 minutes), if it is, fortune
Row step C;If it is not, then in prompt sensor initializing, next current sample time is waited for, then repeatedly step A.
Step C, it is responsible for executing with current value calculating analyte concentration is measured, reads record working electrode and blank electricity first
Sample rate current I1, I2 and sampling time t1, t2 of pole start operation.
Step D and E, it is filtered reduction noise and interference, specific processing mode is the conventional means of this field, this hair
It is not specifically related in bright.Processed electric current I1 ', I2 ' and time t1 ', t2 ' are obtained after data processing.
Step F, the signal in blank electrode is subtracted from working electrode currents, obtains analyte current I=I1 '-
I2 ', to eliminate the current signal of chaff interferent generation;Simultaneously by the information of comprehensive t1 ' and t2 ', analyte current is obtained
When corresponding time t=(t1'+t2')/2, t1=t2, t=t1 '.
Step G, using analyte current I and newest conversion coefficient X, the concentration C 1 of surveyed analyte is calculated;It is used
Formula is C1=f (I, X);In common electrochemical sensor application, analyte response electric current and its concentration in the sample
General linear, the expression of f (I, X) is then (I-b) * X, and wherein b is preset background current value, is retained simultaneously
Analyte concentration corresponds to time tc1=t, new current sample to be obtained and the repetition step A such as after the completion of analyte concentration calculating.
Newest conversion coefficient X includes the following steps to obtain in step G:Check sensor-based system whether by calibrating and calculating
The conversion coefficient X ' and corresponding nearest prover time tc ' for going out non-compensating approach, by X ' and tc ' numerical value import related algorithm and lead to
The result for crossing ac impedance measurement is compensated and is corrected to it;
As shown in figure 4, specifically comprising the following steps:
Step H, it first checks whether there are recent calibration, if not provided, system will use preset conversion system
Number X '=X0, prover time are calculated as 0;If so, then calculating X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f
The inverse operation of (I, X);Formula used is C1=(I-b) * X (t) in step G, then X '=C0/ (I (tc0)-b);Simultaneously more by tc '
It is newly tc0, wherein C0 be the analyte concentration value of calibration, and I (tc0) is measured point for range calibration time of origin is recent
Object electric current is analysed, the time that I (tc0) occurs differs with tc0 to be no more than 5 minutes.
Step I, by X ' and tc ' numerical value import related algorithm and it is compensated by the result of ac impedance measurement and
It corrects, and calibration next time is waited for occur, then repeatedly step H.Wherein, by X ' and tc ' numerical value imports and related algorithm and passes through
The result of ac impedance measurement is compensated and is corrected to it, as shown in figure 5, specifically comprising the following steps:
Step J, first determine whether newest prover time is later than the newest primary ac impedance measurement time, if
It is then to complete step K, conversion coefficient X=X ' is directly exported without any compensating approach;If it is not, then completing step L, read
It takes away from the calibration recent ac impedance measurement value Zre_cal and Zim_cal of time of origin, enters step M;Step L is read
Impedance value can also carry out after step M judging results are to be before executing step N when calibration.
Step M, current impedance measurements Zre and Zim are first determined whether within a preset range, if it is not, then
System is judged as operation irregularity, stop showing result of calculation and shows that information warning, shown information warning can also be
It prompts sensor user to carry out primary new calibration and whether sensor is determined according to calibration result and the difference of expected results
Still work in acceptable precision;If it is, operating procedure N, calculates present impedance value Zre and Zim and number when calibration
The difference of value Zre_cal and Zim_cal, obtain dZre=Zre-Zre_cal and dZim=Zim-Zim_cal.
Step O, judge whether the absolute difference of impedance value has been more than preset drift threshold dZre_thres and dZim_
Thres does not compensate and correct conversion coefficient if it is not, then completing step K, if it is, carrying out subsequent step P;Step
The maximum allowable positive and negative discrepancy threshold used in O is identical, therefore need to only compare dZre, the absolute value and dZre_thres of dZim,
dZim_thres.Its alternative solution can be that maximum allowable positive and negative discrepancy threshold is different, and dZre or dZim is positive value at this time, then needs
Judge whether to be more than its corresponding maximum allowable positive variance threshold value, then needs to judge whether to be less than if it is negative value maximum allowable
Negative variance threshold value.
Step P, four condition judgments are contained compare impedance measured value difference dZre and dZim directionality, it is then right
Conversion coefficient X ' make it is corresponding correct, these judgements will appear in total 5 kinds it is possible as a result, being respectively:
A) dZre and dZim is just and more than corresponding threshold value;Step Q is executed at this time, and conversion coefficient X ' increase and is repaiied
Just, concrete mode is is multiplied by one and impedance real part and relevant equation h (Zre/Zre_cal, the Zim/ of 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 is just and more than dZre_thres threshold values but dZim to be not more than dZim_thres threshold values;Step is executed at this time
R carries out increase amendment to conversion coefficient X ', and concrete mode is to be multiplied by one and the different relevant equation of impedance real part numerical difference
J (Zre/Zre_cal), the result of this equation are naturally larger than 1;One specific embodiment is j (Zre/Zre_cal)=Zre/
Zre_cal。
C) dZre is negative and less than negative dZre_thres threshold value, executes step S at this time, to conversion coefficient X ' reduce and repair
Just, concrete mode is to be multiplied by one and the relevant equation k (Zre/Zre_cal) of 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) dZre is in positive and negative dZre_thres threshold ranges but dZim is just and to be more than dZim_thres threshold values, holds at this time
Row step T carries out increase amendment to conversion coefficient X ', and concrete mode is to be multiplied by one to close with imaginary impedance numerical difference out-phase
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) dZre is in positive and negative dZre_thres threshold ranges but dZim is negative and is less than negative dZim_thres threshold values, at this time
Step U is executed, reduction amendment is carried out to conversion coefficient X ', concrete mode is to be multiplied by one and imaginary impedance numerical difference out-phase
The equation n (Zim/Zim_cal) of pass, the result of this equation is certainly less than 1;One specific embodiment is n (Zim/Zim_cal)
=Zim/Zim_cal.
It obtains correcting conversion coefficient X after X ' to be done to compensating approach or not corrected if executing step K, X conducts
The output of this some algorithm is given to step G to calculate analyte concentration value.After the completion of step P, system can be passed through simultaneously
An information warning is sent to sensor user, prompts sensor to be in non-optimal working condition, needs to re-start calibration.
Claims (8)
1. it is a kind of can self-correction interference signal electrochemical analyte sensor-based system, which is characterized in that including sensor body, straight
Galvanic electricity is pressed power supply part, current measuring members, ac impedance measurement component, circuit changing switch, controller, data processing and is led to
Component, power supply are interrogated,
Sensor body, including working electrode, reference electrode, to electrode and blank electrode;
DC-voltage supply component, including two independent parallel circuits apply to working electrode and blank electrode opposite respectively
In the identical voltage of reference electrode, to excite corresponding analyte electrochemical reaction current and chaff interferent kinetic current;
Current measuring members, including two independent current measuring members measure working electrode respectively and blank electrode are passed through
Electric current and the numerical value measured is sent to data processing and communication component;
Ac impedance measurement component, it is solid for applying one again while applying DC voltage to working electrode or blank electrode
Determine the alternating voltage of frequency, then measure working electrode or the corresponding current response of blank electrode and calculates its corresponding alternating current
Then output result is sent to data processing and communication component by impedance;
Circuit changing switch, for working electrode to be cut between corresponding current measuring members and ac impedance measurement component
It changes, the opportunity of switching and frequency are determined by the instruction of controller;Or for blank electrode in corresponding current measuring members and
Switch between ac impedance measurement component, the opportunity of switching and frequency are determined by the instruction of controller;
Controller is used for timing, controls sampling time and the frequency of current measuring members, when the sampling of ac impedance measurement component
Between and frequency, the state of circuit changing switch and data processing and communication component processing and transmission data opportunity;
Data processing and communication component transport the output result obtained from current measuring members and ac impedance measurement component
It calculates, to obtain analyte concentration and send the result to reception terminal;
Power supply gives DC-voltage supply component, current measuring members, ac impedance measurement component, circuit changing switch, control
Device, data processing and communication component provide the electric energy needed for operation;
DC-voltage supply element outputs are connected with working electrode, blank electrode respectively;Blank electrode output end and its correspondence
Current measuring members connection, working electrode connect with circuit changing switch, and circuit changing switch is right with work electricity grade respectively again
Current measuring members, the connection of ac impedance measurement component or the working electrode current measuring members corresponding with its answered connect, empty
White appliances pole is connected with circuit changing switch, circuit changing switch again respectively current measuring members corresponding with blank electrode, exchange
Impedance measurement component connects;Controller output end is opened with current measuring members, ac impedance measurement component, circuit switching respectively
Close, data processing connected with communication component, current measuring members, ac impedance measurement component respectively with data processing and communication section
Part input terminal connects, and power output end is connected with DC-voltage supply component, controller respectively.
2. it is according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, which is characterized in that work
There are the oxidoreducing enzyme or redox couple medium just for analyte as electrode face finish, blank electrode is in addition to without needle
Except oxidoreducing enzyme or the modification of redox couple medium to analyte, remaining attribute is identical as working electrode;Work electricity
The position of pole and blank electrode on a sensor is adjacent, and the shortest distance between two electrodes is no more than 5 millimeters.
3. it is according to claim 2 can self-correction interference signal electrochemical analyte sensor-based system, which is characterized in that work
Make cover layer in electrode and blank electrode.
4. it is according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, which is characterized in that hand over
The frequency of flow impedance measuring part alternating voltage is 100kHz-1kHz, and the output of ac impedance measurement component impedance measurement includes
The impedance value and phase of impedance or the real and imaginary parts of impedance.
5. it is according to claim 1 can self-correction interference signal electrochemical analyte sensor-based system, which is characterized in that work
The current measurement sample frequency for making electrode is higher by 10 times of ac impedance measurement sample frequency or more.
6. it is a kind of can self-correction interference signal electrochemical analyte method for sensing, which is characterized in that include the following steps:
Step 1: apply respectively to working electrode and blank electrode relative to the identical voltage of reference electrode, it is corresponding to excite
Analyte electrochemical reaction current and chaff interferent kinetic current, are measured by corresponding current measuring members respectively, and handle measures
Numerical value be sent to data processing and communication component;AC impedance component is 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 simultaneously
Its corresponding alternating current impedance is calculated, output result is then sent to data processing and communication component;
Step 2: data processing and communication component utilize the output knot obtained from current measuring members and ac impedance measurement component
Fruit carries out operation, to obtain analyte concentration and send the result to reception terminal;Wherein, the operation includes 1 input
Data point, 9 input message sequences and 2 output information sequences, 1 input data point are:System initial time t0,9 is defeated
Entering information sequence is:Working electrode sample rate current sequence I1, working electrode sampling time sequence t1, blank electrode sample rate current sequence
Arrange 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
Arrange C1, time of measuring tc1;After sensor-based system is powered and starts for the first time, system records startup time t0, and starts simultaneously at note
Record sample rate current I1, I2 and sampling time t1, t2 of working electrode and blank electrode;The t2 sampling times are no more than 1 before and after t1
Minute;
Specifically comprise the following steps:
Step A, first determine whether current run time T=(t1-t0) alreadys exceed preset running life Tmax, if sentenced
Being set to is, then system prompt sensor is out of date needs replacing;If it is determined that no, then operating procedure B;
Step B, judge whether run time has been more than preset initialization time, if it is, operating procedure C;If it is not, then
It prompts in sensor initializing, waits for next current sample time, then repeatedly step A;
Step C, it is responsible for executing and calculates analyte concentration with measuring current value, reads record working electrode and blank electrode first
Sample rate current I1, I2 and sampling time t1, t2 start operation;
Step D and E, it is filtered reduction noise and interference, processed electric current I1 ', I2 ' and time is obtained after data processing
t1',t2';
Step F, the signal in blank electrode is subtracted from working electrode currents, obtains analyte current I=I1 '-I2 ', from
And eliminate the current signal of chaff interferent generation;Simultaneously by the information of comprehensive t1 ' and t2 ', obtain corresponding to analyte current
Time t=(t1'+t2')/2;
Step G, using analyte current I and newest conversion coefficient X, the concentration C 1 of surveyed analyte is calculated;Formula used
For C1=f (I, X), while retention analysis object concentration corresponds to time tc1=t, analyte concentration calculate after the completion of etc. it is to be obtained new
Current sample and repeat step A;
Wherein, newest conversion coefficient X includes the following steps to obtain:Check whether sensor-based system is not mended by calibrating and calculating
Modified conversion coefficient X ' and corresponding nearest prover time tc ' are repaid, by X ' and tc ' numerical value imports related algorithm and passing through and exchanges
The result of impedance measurement is compensated and is corrected to it;
Specifically comprise the following steps:
Step H, it first checks whether there are recent calibration, if not provided, system will use preset conversion coefficient X '
=X0, prover time are calculated as 0;If so, then calculating X '=f-1(I (tc0), C0), wherein f-1(I (tc0), C0) is f (I, X)
Inverse operation;Tc ' is updated to tc0 simultaneously, wherein C0 is the analyte concentration value of calibration, and I (tc0) is range calibration
Time is recent to measure analyte current, and the time that I (tc0) occurs was differed with tc0 no more than 5 minutes;
Step I, by X ' and tc ' numerical value imports and related algorithm and it compensated and is repaiied by the result of ac impedance measurement
Just, and calibration next time is waited for occur, then repeatedly step H;
Wherein, by X ' and tc ' numerical value imports and related algorithm and it compensated and is corrected by the result of ac impedance measurement,
Specifically comprise the following steps:
Step J, first determine whether newest prover time is later than the newest primary ac impedance measurement time, if it is,
Step K is completed, conversion coefficient X=X ' is directly exported without any compensating approach;If it is not, then completing step L, read away from school
The quasi- recent ac impedance measurement value Zre_cal and Zim_cal of time of origin, enters step M;
Step M, current impedance measurements Zre and Zim are first determined whether within a preset range, if it is not, then will be
System is judged as operation irregularity, stops showing result of calculation and shows information warning;If it is, operating procedure N, calculates current resistance
The difference of anti-value Zre and Zim and numerical value Zre_cal and Zim_cal when calibration, obtain dZre=Zre-Zre_cal and dZim
=Zim-Zim_cal;
Step O, judge whether the absolute difference of impedance value has been more than preset drift threshold dZre_thres and dZim_
Thres does not compensate and correct conversion coefficient if it is not, then completing step K, if it is, carrying out subsequent step P;
Step P, four condition judgments are contained compare impedance measured value difference dZre and dZim directionality, then to conversion
Coefficient X ' make it is corresponding correct, these judgements will appear in total 5 kinds it is possible as a result, being respectively:
A) dZre and dZim is just and more than corresponding threshold value;Step Q is executed at this time, and increase amendment is carried out to conversion coefficient X ',
Concrete mode is is multiplied by one and impedance real part and relevant equation h (Zre/Zre_cal, the Zim/Zim_ of imaginary part institute measured value
Cal), the result of this equation is naturally larger than 1;
B) dZre is just and more than dZre_thres threshold values but dZim to be not more than dZim_thres threshold values;Execution step R at this time is right
Conversion coefficient X ' carries out increase amendment, and concrete mode is to be multiplied by one and the different relevant equation j of impedance real part numerical difference
(Zre/Zre_cal), the result of this equation is naturally larger than 1;
C) dZre is negative and less than negative dZre_thres threshold value, executes step S at this time, reduction amendment is carried out to conversion coefficient X ',
Concrete mode is to be multiplied by one and the relevant equation k (Zre/Zre_cal) of impedance real part numerical value, and the result of this equation is inevitable
Less than 1;
D) dZre is in positive and negative dZre_thres threshold ranges but dZim is just and to be more than dZim_thres threshold values, executes step at this time
Rapid T carries out increase amendment to conversion coefficient X ', and concrete mode is to be multiplied by one and the different relevant side of imaginary impedance numerical difference
Journey m (Zim/Zim_cal), the result of this equation are naturally larger than 1;
E) dZre is in positive and negative dZre_thres threshold ranges but dZim is negative and is less than negative dZim_thres threshold values, executes at this time
Step U carries out reduction amendment to conversion coefficient X ', and concrete mode is different relevant with imaginary impedance numerical difference to be multiplied by one
Equation n (Zim/Zim_cal), the result of this equation is certainly less than 1;
It obtains correcting conversion coefficient X after X ' to be done to compensating approach or not corrected if executing step K, X is as this portion
The output of algorithm is divided to be given to step G to calculate analyte concentration value.
7. it is according to claim 6 can self-correction interference signal electrochemical analyte method for sensing, which is characterized in that step
Impedance value carries out after step M judging results are to be before executing step N when rapid L reads calibration.
8. it is according to claim 6 can self-correction interference signal electrochemical analyte method for sensing, which is characterized in that step
After the completion of rapid P, while an information warning is sent to sensor user by system, sensor is prompted to be in non-optimal work
State needs to re-start calibration.
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