CN110879242B - Fixed electrochemical sensor for measuring dissolved carbon dioxide and special sensing film thereof - Google Patents
Fixed electrochemical sensor for measuring dissolved carbon dioxide and special sensing film thereof Download PDFInfo
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Abstract
The invention discloses a fixed electrochemical sensor for measuring dissolved carbon dioxide, a conductive substrate and a sensing film; the conductive substrate is a bottom layer, the sensing film is divided into an inner layer and an outer layer, the inner layer is a carbonate selective film, and the outer layer is a polymer film. The invention also discloses a preparation method and application of the sensor. The invention uses the potential signal measured by the sensor to directly calculate the partial pressure (P (CO) 2 )). The whole operation process is simple and convenient, and gas collection is not needed. And the potential signal measured by the sensor is correlated with the partial pressure of dissolved carbon dioxide (P (CO) 2 ) Linear correlation is good. Meanwhile, the accuracy of the electrode is still good under the existence of various interference factors.
Description
Technical Field
The application relates to the technical field of electrochemistry, in particular to an all-solid-state electrochemistry polymer sensor for measuring dissolved carbon dioxide.
Background
Blood gas analysis is an important matter in examining medicine, and is used for detecting the pH value (pH value) and partial pressure of carbon dioxide [ p (CO) 2 )]Partial pressure of oxygen [ p (O) 2 )]And (3) a quantitative measurement instrument for analyzing and evaluating the acid-base balance (disorder) state and respiratory condition of human blood. When the human body has diseases on any aspect of respiratory, metabolic and in-vivo regulation mechanisms, the blood gas acid-base disorder is caused, and the clinical blood gas analysis has important significance in rescuing critical patients, major operations, extracorporeal circulation, artificial kidney, cardiac catheter, organ transplantation and other diagnosis and treatment, and is one of the indispensable inspection items in hospitals.
Carbon dioxide (CO) 2 ) There are 3 forms of presence in blood: firstly, physical dissolution accounting for 7.3 percent of the total amount; secondly, it is combined with hemoglobin (Hb) to form carbamic hemoglobin (HbNH) 2 +CO 2 HbNHCOOH) accounting for 24.4% of the total amount; and thirdly, the water is combined with the water, and the total amount of the water is 68.3 percent. P (CO) measured in clinical blood gas analysis 2 ) In fact, CO physically dissolved in plasma 2 Tension, the reference range is 4.65-5.98 kPa. In clinical examination medicine, ion-selective electrodes (ion selective electrode, ISE) and electrochemical principles are mostly used for blood gas p (CO) 2 ) Is measured; the volume of the sensor can be further reduced and the power consumption can be reduced by utilizing a metal-oxide-semiconductor field effect transistor (MOSFET) and an ISE composite product, namely an ion-sensitive field effect transistor (ion sensitive field effect transistor, ISFET). The blood being transported by O inhaled from the atmosphere 2 To the tissue while simultaneously carrying CO emitted by the tissue 2 To the lungs for expulsion of the extra-corporeal vehicle. Thus, p (CO) in blood 2 ) The percutaneous partial pressure of carbon dioxide (CO) can also be carried out by applying a modified electrode to the skin surface 2 )，tcp(CO 2 )]The assay, which is a non-invasive detection method. In addition, the principle of selective absorption of gas molecules to light spectrum and the Larmbert-Beer law can be utilized to carry out injection type blood gas p (CO) on the micro-blood vessels 2 ) And (5) measuring.
Currently common p (CO 2 ) The detection method comprises the following steps: 1. an assay based on ion selective electrode principle. p (CO) 2 ) The electrode is essentially a gas-sensitive electrode, and the use of a pH electrode to indirectly measure CO dissolved in blood 2 The content is as follows. The method comprises the steps of coating a water-gel layer on the surface of a pH electrode, sealing the electrode by using a layer of breathable film, wherein the breathable film only allows gas to pass through and prevents ions from passing through, the permeated CO2 is dissolved in an inner layer solution, the pH value of the solution is changed, and the signal change of the pH electrode is caused. 2. Based on ion-sensitive field effect transistor principle. The detection technique uses ISFETs as sensing elements for measuring ionic components and concentrations in blood. ISFET is a composite product of ISE and MOSFET, and has advantages of small size, low power consumption, easy integration, etc., compared to ISE, but it is difficult to perform long-time test. 3. The probe structure of the optical fiber carbon dioxide partial pressure sensor. Optical fiber p (CO) 2 ) When the sensor probe is placed in blood, CO in the blood 2 Will penetrate andthe light with the wavelength of lambda 1 and lambda 2 and the intensity of I01 and I02 emitted by the optical fiber passes through the cavity, is respectively absorbed by the corresponding gases, is reflected back to the optical fiber through the semi-permeable window with the inner wall plated with the reflecting film, and then the reflected light intensities If1 and If2 are respectively measured by the detector, and the size of the corresponding gas partial pressure can be determined according to the ratio of I01/If1 to I02/If 2. The weight and size of the detector determine the size of the wound surface, which is a difficulty. .
Disclosure of Invention
Aiming at the defects in the prior art, the patent uses the carbonate ion sensing membrane to prepare the consolidation sensor for directly measuring the partial pressure of carbon dioxide, thereby realizing the dissolution of CO in aqueous solution, serum and real human blood samples 2 Is a direct detection of (a). .
The invention comprises the following steps: the invention relates to a fixed electrochemical sensor for measuring dissolved carbon dioxide, which comprises a conductive substrate and a sensing film; the conductive substrate is a bottom layer, the sensing film is divided into an inner layer and an outer layer, the inner layer is a carbonate selective film, and the outer layer is a polymer film.
Specifically, the conductive substance of the conductive substrate is: gold, platinum, palladium, carbon, silver/silver chloride, metal-conductive polymers, and the like. Gold, carbon, silver/silver chloride are preferred.
Specifically, the polymer film is a cellulose film, a regenerated cellulose film, a nylon film and a polycarbonate film. Cellulose membranes and regenerated cellulose membranes are preferred.
Specifically, the carbonate selective membrane contains an ion exchanger, a carbonate ion carrier, a polymer material auxiliary agent and an auxiliary agent.
The carbonate selective membrane comprises the following components: the content of the ion exchanger is as follows: 1-5% (weight ratio); the content of carbonate carrier is: 10% -30% (weight ratio); the content of the polymer material auxiliary agent is as follows: 50-80% (weight ratio); the content of the auxiliary agent is as follows: 3 to 15 percent (weight ratio).
Specifically, the ion exchanger comprises: sodium tetraphenyl borate, potassium tetrakis (4-chlorophenyl) borate, ammonium tetrakis (4-chlorophenyl) borate, sodium tetrakis (3, 5-di (trifluoromethyl) phenyl) borate, tris (dodecyl) methyl ammonium chloride; ammonium tetrakis (4-chlorophenyl) borate, sodium tetrakis (3, 5-di (trifluoromethyl) phenyl) borate, tri (dodecyl) methyl ammonium chloride, tetra (dodecyl) ammonium tetrakis (4-chlorophenyl) borate are preferred.
Specifically, the carbonate carrier comprises: 4-butyl-alpha, alpha-trifluoroacetophenone, N-dioctyl-3 alpha, 12 alpha-di- (4-trifluoroacetyl-benzoic acid) -5 beta-deoxycholic acid-24-amide
Specifically, the polymer material auxiliary agent comprises a high boiling point solvent, a plastic auxiliary agent and a fiber auxiliary agent; plastic auxiliaries and fiber auxiliaries are preferred.
Specifically, the auxiliary agent comprises resin particles, quartz powder, silicon dioxide particles, silica gel powder and aluminum oxide; resin particles, silica gel powder are preferable.
Further, the invention also provides a preparation method of the all-solid-state electrochemical high polymer sensor, which comprises the steps of mixing a carbonate carrier, an ion exchanger, a plasticizer, ammonium tetra (4-chlorophenyl) borate and an auxiliary agent, fully oscillating and dissolving, then dripping the uniform solution on the surface of an electrode, standing overnight at room temperature, and tightly adhering a high polymer film above an inner layer film to obtain the solid-state electrochemical sensor for dissolving carbon dioxide.
Further improvement, conductive materials such as conductive polymers, carbon nanotubes and the like can be used between the polymer film and the electrode so as to increase the stability of the system.
The invention also provides application of the electrochemical sensor, and the electrochemical sensor can directly measure partial pressure of gaseous carbon dioxide in solution by fixedly connecting the electrochemical sensor with dissolved carbon dioxide.
Specifically, the partial pressure of dissolved carbon dioxide (P (CO) 2 ))。
The invention also provides a special polymer sensing film applied to the fixedly connected electrochemical sensor, wherein the sensing film is divided into an inner layer and an outer layer, the inner layer is a carbonate selective film, and the outer layer is a polymer film.
The carbonate selective membrane contains: carbonate carrier, ion exchanger, plasticizer, tetra (dodecyl) ammonium tetra (4-chlorophenyl) borate.
Further, the carbonate selective membrane comprises the following components in percentage by weight: carbonate carrier (20-25 wt.%), ion exchanger (1-3 wt.%), plasticizer (50-70 wt.%) and tetra (dodecyl) ammonium tetra (4-chlorophenyl) borate (1-3 wt.%).
In a further improvement, the carbonate selective membrane can be added with auxiliary agents, the auxiliary agents are convenient to prepare and operate, and the proper content of the auxiliary agents is (5-10%wt).
The polymer film is regenerated cellulose film, nylon film, polycarbonate film, preferably regenerated cellulose film.
The beneficial effects are that: the invention uses the potential signal measured by the sensor to directly calculate the partial pressure (P (CO) 2 )). The whole operation process is simple and convenient, no gas is required to be collected, and the potential signal measured by the sensor is compared with the partial pressure (P (CO) 2 ) Linear correlation is good. Meanwhile, when the electrode is used for measuring serum or whole blood samples, the interference of substances such as Yang Suangen ions and heparin in the samples can be effectively inhibited, and the accuracy of measuring aqueous solution, serum and whole blood samples by the electrode is good.
The high molecular sensing membrane can efficiently inhibit the interference of substances such as Yang Suangen ions, heparin and the like in the sample. So that the sensor can accurately measure PCO in blood samples 2 Partial pressure.
Drawings
FIG. 1 is a graph of the operation of a stationary sensor for dissolving carbon dioxide
FIG. 2 is a graph of selectivity of a stationary sensor for dissolving carbon dioxide
FIG. 3 is a graph showing the working curve and Time trace of a polymer sensor film
Detailed Description
In order to make the present application solution better understood by those skilled in the art, the following description will be made in detail and with reference to the accompanying drawings in the embodiments of the present application, it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments.
Example 1 solid-state electrochemical sensor
The bottom layer is: gold;
the outer layer is: a cellulose film;
the inner layer is: 5% of sodium tetraphenyl borate, 10% of 4-butyl-alpha, alpha-trifluoro acetophenone, 70% of plastic auxiliary agent and 15% of quartz powder.
Example 2 solid-state electrochemical sensor
The bottom layer is: gold;
the outer layer is: regenerating the cellulose membrane;
the inner layer is: 5% of sodium (3, 5-bis (trifluoromethyl) phenyl) borate, 10% of 4-butyl-alpha, alpha-trifluoroacetophenone, 70% of plastic auxiliary agent and 15% of quartz powder.
Example 3 solid-state electrochemical sensor
The bottom layer is: carbon;
the outer layer is: regenerating the cellulose membrane;
the inner layer is: 5% of sodium (3, 5-bis (trifluoromethyl) phenyl) borate, 10% of 4-butyl-alpha, alpha-trifluoroacetophenone, 70% of plastic auxiliary agent and 15% of quartz powder.
Example 4 solid-state electrochemical sensor
The bottom layer is: silver/silver chloride;
the outer layer is: a cellulose film;
the inner layer is: 2.5% of tri (dodecyl) methyl ammonium chloride, 20% of 4-butyl-alpha, alpha-trifluoroacetophenone, 60% of plastic auxiliary, 15% of silicon dioxide particles and 2.5% of tetra (dodecyl) ammonium tetra (4-chlorophenyl) borate
Example 5 solid-state electrochemical sensor
The bottom layer is: carbon;
the outer layer is: a cellulose film;
the inner layer is: 7.5% of tri (dodecyl) methyl ammonium chloride, 20% of 4-butyl-alpha, alpha-trifluoroacetophenone, 55% of plastic auxiliary agent, 15% of silicon dioxide particles and 2.5% of tetra (dodecyl) ammonium tetra (4-chlorophenyl) borate
Among the above examples, example 5 performed best in terms of detection range, accuracy and voltage stability.
Example 6 preparation of solid-state electrochemical sensor with dissolved carbon dioxide and characterization of sensor properties
4-butyl-alpha, alpha-trifluoroacetophenone (188 mg) and tri (dodecyl) methyl ammonium chloride (18 mg) were mixed and then dissolved in the plastic auxiliary agent by sufficient shaking, the uniform solution was applied to the electrode surface by dropping, and the mixture was allowed to stand at room temperature overnight. And then the polymer layer is tightly adhered on the upper part of the inner layer film to form the carbonate electrode. Conductive materials such as conductive polymer and carbon nanotube can be used between the polymer film and the electrode to increase system stability
The method for measuring the potential value comprises the following steps: the electrode was immersed in 20mL of deionized water at room temperature, sodium bicarbonate mother solution was added dropwise, and after stirring was stopped, carbonate ion solutions of different concentrations were obtained, and potential values were measured using a 6-channel EMF device. A double liquid-connected Ag/AgCl reference electrode (3M KCl is filled in, and 1M lithium acetate is used as an external solution) is used. The ion activity coefficients used in the experimental data were calculated with reference to the debye-shock equation, all potential values were corrected by the hendersen equation, and all data were averages of the data obtained for 5 parallel electrodes. As can be taken from fig. 1, the electrode pairs are different from P (CO 2 ) Partial pressure Log (P (CO) 2 ) P has good linear response (R) in the range of-1.67 to 0.4 2 ＝0.9996)，P(CO 2 ) The lower detection limit was 10mmHg.
Under the same experimental conditions, the fixed electrochemical sensor for dissolving carbon dioxide and the reference electrode are placed in 20mL of a salt solution containing interfering metal ions (100 mM NaCl, 1mM NaSCN, 1mM Sal-, 0.128mg/mL Heparin, 10mM NaClO 4) together, sodium bicarbonate mother solution is added dropwise, carbonate ion solutions with different concentrations are obtained after stirring is stopped, and potential measurement is carried out, so that the result shown in FIG. 2 is obtained. FIG. 2 is a selectivity curve of a solid state sensor for dissolved carbon dioxide, wherein (a) 100mM Cl - ；(b)1mM SCN - ；(c)10mM ClO4 - ；(d)1mM Sal - ；(e)0.128mg/ml Heparin
The detection lower limit of the stationary electrochemical sensor for dissolved carbon dioxide and the concentration selectivity coefficient of the interfering ions in the background solution were calculated according to equation 1, as shown in table 1.
TABLE 1 summary of Selectivity coefficients for solid-state electrochemical sensors for dissolving carbon dioxide under various disturbances
| Interfering ions | Selectivity coefficient |
| Cl - | -3.08±0.014 |
| SCN - | 0.69±0.007 |
| ClO4 - | -1.23±0.007 |
| Sal - | 0.52±0.048 |
| Heparin | -3.83±0.028 |
Example 7 accuracy of carbon dioxide dissolved fixed sensor in aqueous solution, serum and real human blood samples
Respectively placing a fixed electrochemical sensor for dissolving carbon dioxide and a reference electrode in a container containing carbon with a certain concentrationThe potential value obtained in the sodium hydrogen carbonate standard solution and the sample to be measured (aqueous solution, serum and real human blood sample) is measured by using the potential signal measured by the sensor and the partial pressure (P (CO) 2 ) Linear correlation, calculating P (CO) in a sample to be measured 2 ) And calculating the recovery rate with a theoretical value (a Libang instrument). The assay was repeated for each sample and precision (CV%) was calculated from standard deviation and average, and the results are shown in Table 2.
TABLE 2 accuracy of all-solid-state sensor for dissolving carbon dioxide in sample to be measured
| Type of sample to be tested | Recovery/% | CV/％ |
| Aqueous solution | 114.5 | 6.5 |
| Serum | 85.3 | 5.1 |
| Whole blood | 47.0 | 7.0 |
Example 8 Polymer sensor Membrane
N, N-dioctyl-3 alpha, 12 alpha-di- (4-trifluoroacetyl-benzoic acid group) -5 beta-deoxycholic acid-24-amide (188 mg) and tri (dodecyl) methyl ammonium chloride (18 mg) were mixed and dissolved, then dropped into a fixing device of a regenerated cellulose membrane, inserted with a conductive wire, and allowed to stand at room temperature overnight.
The detection method is the same as in example 6. As shown in FIG. 3, FIG. 3 shows a graph (A) and a graph (B) of the operation of the stationary sensor for dissolving carbon dioxide with the storage Time
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the present application.
Claims (4)
1. A fixed electrochemical sensor for measuring dissolved carbon dioxide, which is characterized by comprising a conductive substrate and a sensing film; the conductive substrate is a bottom layer, the sensing film is divided into an inner layer and an outer layer, the inner layer is a carbonate selective film, and the outer layer is a polymer film; the conductive substance of the conductive substrate is as follows: gold, platinum, palladium, carbon, silver/silver chloride, metal-conductive polymers; the polymer film is a cellulose film, a regenerated cellulose film, a nylon film and a polycarbonate film;
the carbonate selective membrane consists of an ion exchanger, a carbonate carrier, a high polymer material auxiliary agent and an auxiliary agent;
the ion exchanger is as follows: at least comprises tetra (dodecyl) ammonium tetra (4-chlorophenyl) borate, and further comprises one of sodium tetraphenyl borate, potassium tetra (4-chlorophenyl) borate, ammonium tetra (4-chlorophenyl) borate, sodium tetra (3, 5-di (trifluoromethyl) phenyl) borate or tri (dodecyl) methyl ammonium chloride;
the carbonate carrier is as follows: 4-butyl- α, α, α -trifluoroacetophenone or N, N-dioctyl-3 α,12 α -bis- (4-trifluoroacetyl-benzoyl) -5 β -deoxycholic acid-24-amide;
the polymer material auxiliary agent is a high boiling point solvent, a plastic auxiliary agent or a fiber auxiliary agent;
the auxiliary agent is quartz powder or silicon dioxide particles;
the carbonate selective membrane comprises the following components:
the content of the ion exchanger is as follows: 1-5% (weight ratio);
the content of carbonate carrier is: 10% -30% (weight ratio);
the content of the polymer material auxiliary agent is as follows: 50-80% (weight ratio);
the content of the auxiliary agent is as follows: 3% -15% (weight ratio);
the preparation method of the electrochemical sensor comprises the following steps: mixing a carbonate carrier, an ion exchanger and a polymer material auxiliary agent, adding an auxiliary agent, mixing, fully oscillating for dissolution, dripping the uniform solution onto the surface of an electrode, standing overnight at room temperature, and tightly adhering a polymer film above an inner layer film to obtain the solid-state electrochemical sensor for dissolving carbon dioxide.
2. The method for manufacturing an electrochemical sensor according to claim 1, comprising the steps of: mixing a carbonate carrier, an ion exchanger and a polymer material auxiliary agent, adding an auxiliary agent, mixing, fully oscillating for dissolution, dripping the uniform solution onto the surface of an electrode, standing overnight at room temperature, and tightly adhering a polymer film above an inner layer film to obtain the solid-state electrochemical sensor for dissolving carbon dioxide.
3. The method according to claim 2, wherein a conductive polymer or carbon nanotube conductive material is used between the polymer film and the electrode to increase the system stability.
4. The use of an electrochemical sensor according to claim 1, wherein the partial pressure of gaseous carbon dioxide in the solution is directly measured by a stationary electrochemical sensor that dissolves carbon dioxide; the partial pressure P (CO 2) of dissolved carbon dioxide in the sample is directly calculated from the potential signal measured by the sensor.
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