CN105353018A - Multi-term ion biochemical analysis dry plate and preparation method thereof - Google Patents
Multi-term ion biochemical analysis dry plate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a multi-term ion biochemical analysis dry plate and a preparation method thereof, which belong to the technical field of a blood gas biochemical sensor, and the multi-term ion biochemical analysis dry plate is used for detecting sodion, potassium ions, calcium ions, chloride ions and carbon dioxide concentration in body fluid. The dry plate comprises a supporting layer, a sodion selective electrode, a potassium ions selective electrode, a calcium ions selective electrode, a chlorine ions selective electrode, a carbon dioxide selection electrode, a reference electrode, an interface layer, a salt bridge and a top. The salt bridge is sealed between the interface layer and the top, sodion, potassium ions, calcium ions, chloride ions, the carbon dioxide selection electrode and the reference electrode are respectively bounded to the supporting layer, the interface layer and the top for assembly to obtain the dry plate. When a test is carried out, a reference liquid and a test liquid are mutually conducted through osmosis of the salt bridge. The dry plate can simultaneously measure the sodion, the potassium ions, the calcium ions, the chloride ions and the carbon dioxide concentration in the liquid to-be-measured, has the advantages of simple operation, fast response speed and small volume, has the characteristics of simple preparation operation and low production cost, and is suitable for industrial production.
Description
Technical field
The present invention relates to vim and vigour biochemical sensor technologies field, particularly relate to a kind of multinomial ion biochemical analysis dry plate and preparation method thereof.
Background technology
Sodium in human body fluid, potassium, calcium, chlorion and carbon dioxide etc. participate in many important functions and metabolic activity in body, very important effect is played to maintenance normal activities, electrolyte and disturbance of acid-base balance can make the metabolism of each organ of whole body particularly cardiovascular system, neural physiological function and body that corresponding obstacle occurs, and even jeopardize patient vitals.
Detect the ion-selective electrode that in body fluid, the many employings of sodium, potassium, calcium, chlorion and gas concentration lwevel are traditional clinically at present.The interior reference solution of conventional ion electrodes selective generally adopts electrolyte solution, can only at lower temperature, pressure operation, ion-selective electrode traditional in addition once can only detect a kind of ion concentration, express-analysis can not judge electrolyte disturbance and the disturbance of acid-base balance situation of human body, extend the therapeutic time of patient, and operation and maintenance is complicated, cost is high, not portable, the demand of the occasions such as operation, emergency treatment, field rescue cannot be met, also cannot adapt to the trend of domestic medicine, modern medical service in-vitro diagnosis apparatus pattern.
Chinese patent CN202189033U discloses a kind of card-type electrolyte testing electrode supporting with dry electrolytic matter analyser, the patent provides one and measure sodium, potassium, chlorine, calcium and pH method simultaneously, but its sodium, potassium, chlorine, calcium and hydrogen ion electrode need match use, structure and preparation technology's relative complex.
Existing patent adopts screen printing technique to prepare electrode substantially, but the metal level purity that serigraphy obtains is inadequate, and surface is uneven, can affect stability and the response time of electromotive force; In existing solid ionic choice electrode, all select Polyvinylchloride as the non-conductive polymer cementing agent (patent CN101852761A, CN104330449A, CN102636532A, CN101871912A, CN102558724A) of ion-selective membrane, Polyvinylchloride has higher intensity and chemical stability, and low price, but it must add plastifier just can guarantee that ion-selective membrane responds, As time goes on, plastifier be dissolved in carrier wherein can together with leak out from ion-selective membrane, cause ion-selective membrane to respond lower limit to be deteriorated, lifetime.
Summary of the invention
For existing ion-selective electrode Problems existing, the invention provides a kind of multinomial ion biochemical analysis dry plate and preparation method thereof, sodium in body fluid, potassium, calcium, chlorion and gas concentration lwevel can be measured simultaneously, prepared dry plate measuring accuracy is high, long-time stability are good, and the response time is short, and structure is simple, volume is little, preparation technology is simple, production cost is low, is applicable to producing in enormous quantities.
The present invention's multinomial ion biochemical analysis dry plate comprises: supporting layer, sodium selective electrode, potassium ion-selective electrode, calcium ion-selective electrode, Chloride selective electrode, carbon dioxide choice electrode, contrast electrode, middle layer, top layer and salt bridge.Preparation technology is as follows: (1) prepares metal/metal salt electrode; (2) on electrode, be coated with prepare reference layer solution, ion-selective membrane solution and prepare sodium, potassium, calcium ion-selective electrode, electrode is coated with the polymeric membrane solution prepared and prepares chlorine ion electrode, contrast electrode, electrode is coated with reference layer solution, ion-selective membrane solution, cushion solution prepares carbon dioxide choice electrode; (3) establish inlet and gas port at top layer, liquid pool is established in middle layer, and salt bridge is sealed between middle layer and top layer; (4) dry plate is assembled into by bonding with supporting layer, middle layer and top layer to sodion, potassium ion, chlorion, calcium ion, carbon dioxide choice electrode and contrast electrode.
Supporting layer plays protection and support electrode effect, and top layer is provided with inlet and gas port, and middle layer is provided with liquid pool, and salt bridge is sealed between middle layer and top layer; Supporting layer, middle layer and top layer are selected from polypropylene, Polyvinylchloride, tygon, polyester non-conductive polymer material.Salt bridge is filter paper material.
Sodium, potassium, calcium ion-selective electrode comprise: electrode, reference layer, ion-selective membrane.Chloride selective electrode and contrast electrode comprise: electrode, polymeric membrane.Carbon dioxide choice electrode comprises: electrode, reference layer, carbanion selective membrane, cushion.
Electrode.Electrode of the present invention comprises metal level and metal salt.Metal salt and metal level form phase boundary potential, have stable electromotive force response.Metal level metal is selected from gold, silver, copper, mercury, platinum, nickel.Slaine is selected from the insoluble metallic salt of metal level metal.Slaine can use the oxide of metal level metal, such as metal halide.Preferred electrode is silver/silver chloride electrode.
Electrode metal layer is attached to non-conductive polymer surface, be improve electrode stability, shorten the response time, the present invention can adopt vacuum coating, the mode of electroless plating or plating prepares metal level, preferred electroless plating method.Use electroless plating method, layer on surface of metal is even, can set up the balance between phase boundary instantaneously, form stable response electromotive force, shortens the response time.Metal salt can adopt the method for chemical oxidation to obtain, and uses iron chloride or liquor potassic permanganate to be oxidized metal level.
Reference layer.Sodion of the present invention, potassium ion, calcium ion and carbon dioxide choice electrode reference layer comprise: cementing agent, surfactant, bactericidal agent, spreading agent, buffering agent, slaine.Slaine select sodium chloride and potassium chloride composite, when sodium chloride and potassium chloride proportioning are 5:1, ion-selective electrode has optimal response.The too high or too low meeting of reference layer water cut simultaneously all can affect the bond strength of reference layer and ion-selective membrane, thus reduces signal accuracy and long-time stability, and reference layer optimum moisture content is 30% ~ 40%.
Reference layer is attached directly on electrode metal salt deposit by the mode of lamination or coating.By controlling reference layer drying time, temperature, humidity fixes sodium chloride and potassium chloride proportioning and water cut in reference layer.Preferred drying condition: temperature 25 DEG C, relative humidity 50%, time 40min.
Ion-selective membrane comprises: non-conductive polymer cementing agent, ionophore, carrier solvent, ion interference agent and surfactant.
For reducing the consumption of plastifier, reduce carrier to run off, promote the long-time stability of ion-selective membrane, non-conductive polymer cementing agent used in the present invention is acrylate materials, its physical and mechanical property is controlled, can reduce the use of plastifier, the physical property of its excellence can promote the adhesion property of ion-selective membrane and solid electrolyte reference layer simultaneously, improves the stability of the response signal of ion-selective electrode.Acrylate has lower coefficient of diffusion, is conducive to obtaining wider sensing range, and less coefficient of diffusion be conducive to carrier dispersed and suppress carrier run off, eliminate carrier run off on response electromotive force impact, improve the accuracy of test.Esters of acrylic acid cementing agent is selected from one or more in ethyl acrylate, methyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, glycidyl methacrylate, methacrylic acid ester in the positive last of the ten Heavenly stems, preferred: methyl methacrylate, account for 15% ~ 35% of ion-selective membrane gross mass.
Polymeric membrane.Polymeric membrane comprises cementing agent, solvent, volatile solvent, plastifier, surfactant.Polymeric membrane is prepared by non-conductive polymer material, uniform cell structure, and 1 ~ 3 μm, aperture, has good longitudinal diffusion coefficient and perviousness, have protective effect simultaneously to electrode.
Polymeric membrane cementing agent is selected from one or more in polyamide, polyolefin, polystyrene, polycarbonate, polyacrylate, polyetheretherketone, polyvinyl alcohol (PVA), polyvinyl acetate (PVA), cellulose acetate, cellulose propionate, cellulose butyrate, accounts for 30% ~ 50% of polymeric membrane gross mass.
For guaranteeing the permeance property of polymeric membrane, need adopt solvent and volatile solvent with the use of mode prepare.Solvent because boiling point is different, can form uniform micropore after polymeric membrane drying from volatile solvent, makes polymeric membrane have good perviousness.Solvent is selected from methylene chloride, tetrachloroethane, dimethylformamide, dimethyl sulfoxide (DMSO).Volatile solvent is selected from methyl alcohol, ethanol, acetone, butanone, toluene, tetrahydrofuran, methyl acetate, ethyl acetate, phenixin.By using different boiling solvent, the proportioning regulating solvent and volatile solvent and optimizing drying technique, controlling polymeric membrane and forming constant aperture and uniform micropore.The preferred 3:1 of proportioning of solvent and volatile solvent, preferred solvent and volatile solvent are respectively: tetrahydrofuran and methylene chloride, and optimum drying technique is: temperature 25 DEG C, relative humidity 25%, time 60min.
Cushion.Cushion is alkalescence, and the carbon dioxide in liquid to be measured, bicarbonate ion are all converted into carbanion by cushion, and then obtains the total carbon dioxide capacity in liquid to be measured by the concentration measuring carbanion.Cushion pH scope is 7.5 ~ 10.
Cushion comprises: cementing agent, buffering agent, surfactant.Cushion cementing agent is selected from one or more in agar, gelatin, polyvinyl alcohol (PVA), polyvinyl pyrrolidone, poly-ethyl acetate-vinyl alcohol, Polyvinylchloride-ethyl acetate-vinyl alcohol and synthesis of vinyl high molecular weight hydrophilic material, accounts for 40 ~ 90% of cushion gross mass.Buffering agent is selected from tricarboxymethyl aminomethane, diethanolamine, AMPD acid and buffering agent, one or more in organic acid buffering agent, accounts for 0.1% ~ 10% of cushion gross mass.
Each multinomial ion biochemical analysis dry plate comprises a sodion, potassium ion, calcium ion, chlorion, carbon dioxide choice electrode and a contrast electrode, during test contrast electrode respectively with sodion, potassium ion, calcium ion, chlorion, the conducting of carbon dioxide choice electrode, formed loop test liquid sodion to be measured, potassium ion, calcium ion, chlorion, gas concentration lwevel respectively.
Be different from existing patent intermediate ion choice electrode, major advantage of the present invention has: (1) can measure sodion, potassium ion, calcium ion, chlorion and gas concentration lwevel in liquid to be measured simultaneously, simple to operate, greatly improves work efficiency; (2) the metal/metal salt thin electrode surface uniform prepared, shortens electrode response time greatly, can equilibrium establishment within 10s, forms stable response electromotive force; (3) by sodium chloride in adjustment reference layer and potassium chloride proportioning, control reference layer water cut, select acrylate to be the high polymer binder of sodium, potassium, calcium, carbanion selective membrane, promote measuring accuracy and the long-time stability of sodion, potassium ion, calcium ion, chlorion and carbon dioxide choice electrode; (4) Chloride selective electrode and contrast electrode polymeric membrane adopt solvent and volatile solvent with the use of, the proportioning of control solvent, volatile solvent and drying process, make generation constant aperture and uniform microporous membrane structure, promote the measuring accuracy of Chloride selective electrode and contrast electrode, stability and response speed, make the biochemical analysis dry plate measuring accuracy of multinomial ion high, good stability; (5) only need a contrast electrode to coordinate multiple ion-selective electrode to use, use without the need to ion-selective electrode pairing, volume is little, structure is simple, production process is few, and test result is stablized, and greatly reduces cost simultaneously, is suitable for large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is multinomial ion biochemical analysis dry plate schematic diagram;
Fig. 2 is sodion, potassium ion, calcium ion, chlorion and carbon dioxide choice electrode schematic diagram.
Embodiment
The present invention is described in detail with embodiment by reference to the accompanying drawings.
As shown in Figure 1, multinomial ion biochemical analysis dry plate comprises: supporting layer 1, sodium selective electrode 2, potassium ion-selective electrode 3, calcium ion-selective electrode 4, Chloride selective electrode 5, carbon dioxide choice electrode 6, contrast electrode 7, middle layer 8, salt bridge 9, top layer 10.
As shown in Figure 2, sodium, potassium, calcium ion-selective electrode comprise: silver layer 21, silver chloride layer 22, reference layer 23, ion-selective membrane 24; Carbon dioxide choice electrode comprises: silver layer 31, silver chloride layer 32, reference layer 33, ion-selective membrane 34, cushion 35; Chloride selective electrode, contrast electrode comprise: silver layer 41, silver chloride layer 42, polymeric membrane 43.
Concrete implementation step is as follows:
By the method for electroless plating at polyethylene terephthalate plated surface silver layer, prepare silver layer 21,31,41.
The front 2/3 section of employing chemical method of dried silver layer 21,31,41 is oxidized.The contact electrode being oxidized position will be needed to be immersed in 0.1mol/L ferric chloride solution after 60s, and taking-up pure water cleans up and drying, has both obtained silver chloride layer 22,32,42.
Reference layer is coated with.By 6g polyvinyl alcohol (PVA), 1g glycerine, 5g sodium chloride, 1g potassium chloride, 0.02g citric acid, 0.02g germifuge, 0.004g surfactant H212 is dissolved in 100g water, coated on silver chloride layer 22,32, drying condition: 25 DEG C, relative humidity 50%, dry 40min.
Ion-selective membrane is coated with.By 0.1g methyl methacrylate, 0.1g ortho-nitrophenyl octyl ether, 0.004g ionophore, 0.003g tetraphenylboron sodium, 0.005g surfactant H212 is dissolved in acetone, is coated on reference layer 23,33, and drying at room temperature.
Polymeric membrane is coated with.By 0.1g polyamide, 0.2g triphenyl phosphate, 0.005g surfactant H212 is dissolved in 1mL methylene chloride and 3mL tetrahydrofuran, is coated on silver chloride layer 42, and at 25 DEG C, dry 60min under relative humidity 25% environment.
Cushion is coated with.5g is gathered ethyl acetate-vinyl alcohol, Tris-HCl buffering agent 0.25g, 0.02g germifuge, 0.01g surfactant H212 is dissolved in 50g water, is coated on carbanion selective membrane 34, and dry.
Salt bridge 9 to be sealed and between middle layer 8 and top layer 10.
Get sodion, potassium ion, calcium ion, chlorion and carbon dioxide choice electrode, contrast electrode to align with middle layer 8 according to position of opening and bonding, bondingly with supporting layer 1 again after solidification be assembled into dry plate.
Multinomial ion biochemical analysis dry plate long-term storage conditions is :-10 ~-18 DEG C.
Multinomial ion biochemical analysis dry plate using method, uses after needing to place 1h at normal temperatures when taking out from low temperature environment, keeps probe temperature 37 ± 0.1 DEG C during test.Insert in test trough by dry plate during test, two lateral opening dropping reference liquid and test fluid respectively, required sample 10 ~ 20 μ L, the test duration is less than 10s.
In order to advantage of the present invention is better described, the invention provides 1 group of experimental data, specific as follows.
Embodiment 1, with the response electromotive force of multinomial ion biochemical analysis dry plate test known ion strength solution (Na ion concentration 220mmol/L, potassium concentration 2mmol/L, calcium ion concentration 0.49mmol/L, chlorine ion concentration 65mmol/L, concentration of total carbon dioxide 35.27mmol/L), measure 5 times, test result is as shown in the table.
Dry plate | Sodion response electromotive force/mV | Potassium ion response electromotive force/mV | Calcium ion response electromotive force/mV | Chlorion response electromotive force/mV | Photosynthesis-carbon dioxide response electromotive force/mV |
1 | 13.8 | -61.6 | -96.5 | 69.9 | 53.4 |
2 | 13.6 | -61.6 | -96.3 | 70.1 | 53.4 |
3 | 13.6 | -61.4 | -96.6 | 70.1 | 53.5 |
4 | 13.9 | -61.8 | -96.3 | 69.6 | 53.6 |
5 | 13.7 | -61.8 | -96.4 | 69.8 | 53.4 |
Coefficient of variation % | 0.95 | 0.27 | 0.14 | 0.30 | 0.17 |
The foregoing is only implementation method of the present invention; not thereby the scope of the claims of the present invention is limited; every utilize present disclosure and accompanying drawing content to do equivalent structure or equivalent flow process exchange; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. multinomial ion biochemical analysis dry plate and preparation method thereof, is characterized in that: described multinomial ion biochemical analysis dry plate comprises supporting layer, sodium selective electrode, potassium ion-selective electrode, calcium ion-selective electrode, Chloride selective electrode, carbon dioxide choice electrode, contrast electrode, middle layer, salt bridge, top layer; The main preparation process of described multinomial ion biochemical analysis dry plate comprises, and (1) prepares metal/metal salt thin electrode; (2) on electrode, be coated with prepare reference layer solution, ion-selective membrane solution and prepare sodium, potassium, calcium ion-selective electrode, electrode is coated with the polymeric membrane solution prepared and prepares Chloride selective electrode, contrast electrode, electrode is coated with reference layer solution, ion-selective membrane solution, cushion solution prepares carbon dioxide choice electrode; (3) establish inlet and gas port at top layer, liquid pool is established in middle layer, and salt bridge is sealed between middle layer and top layer; (4) dry plate is assembled into by bonding with supporting layer, middle layer and top layer to sodion, potassium ion, chlorion, calcium ion, carbon dioxide choice electrode and contrast electrode.
2. ion-selective electrode according to claim 1, it is characterized in that: described sodium, potassium, calcium ion-selective electrode comprise electrode, reference layer, ion-selective membrane, described Chloride selective electrode, contrast electrode comprise electrode, polymeric membrane, and described carbon dioxide choice electrode comprises electrode, reference layer, carbanion selective membrane, cushion.
3. electrode according to claim 2, is characterized in that: described electrode is metal/metal salt thin electrode, comprises metal level and metal salt; Metal level metal is selected from gold, silver, copper, mercury, platinum, nickel; Slaine is selected from the insoluble metallic salt of metal level metal.
4. electrode according to claim 2, is characterized in that: described electrode adopts electroless plating, the mode of Vacuum Deposition or plating is attached on substrate, metal level and metal salt thickness 0.1 ~ 10 μm on substrate.
5. reference layer according to claim 2, is characterized in that: described reference layer comprises cementing agent, surfactant, bactericidal agent, spreading agent, buffering agent, slaine; Slaine is selected from sodium chloride and potassium chloride is composite, and proportioning is 1:1 ~ 8:1, accounts for 20% ~ 50% of reference layer gross mass.
6. reference layer according to claim 2, is characterized in that: described reference layer is attached on electrode, baking temperature 20 ~ 50 DEG C, dry environment relative humidity 20% ~ 50%, drying time 30 ~ 100min, reference layer water cut 30% ~ 40%.
7. ion-selective membrane according to claim 2, is characterized in that: described ion-selective membrane comprises non-conductive polymer cementing agent, ion interference agent, carrier, carrier solvent, surfactant; Non-conductive polymer cementing agent is selected from one or more in ethyl acrylate, methyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, glycidyl methacrylate, methacrylic acid ester in the positive last of the ten Heavenly stems, accounts for 15% ~ 35% of ion-selective membrane gross mass.
8. polymeric membrane according to claim 2, is characterized in that: described polymeric membrane comprises cementing agent, solvent, volatile solvent, plastifier, surfactant; Polymeric membrane cementing agent is selected from one or more in polyamide, polyolefin, polystyrene, polycarbonate, polyacrylate, polyetheretherketone, polyvinyl alcohol (PVA), polyvinyl acetate (PVA), cellulose acetate, cellulose propionate, cellulose butyrate, accounts for 30% ~ 50% of polymeric membrane gross mass; Polymeric membrane solvent is selected from one or more in methylene chloride, tetrachloroethane, dimethylformamide, dimethyl sulfoxide (DMSO); Volatile solvent is selected from one or more in methyl alcohol, ethanol, acetone, butanone, toluene, tetrahydrofuran, methyl acetate, ethyl acetate, phenixin; Polymeric membrane solvent and volatile solvent proportioning 1:1 ~ 10:1.
9. carbon dioxide choice electrode cushion according to claim 2, is characterized in that: described cushion comprises cementing agent, buffering agent, surfactant; Buffering agent is selected from one or more in tricarboxymethyl aminomethane, diethanolamine, AMPD acid and buffering agent or organic acid buffering agent, accounts for 0.1% ~ 10% of cushion gross mass.
10. carbon dioxide choice electrode cushion according to claim 2, is characterized in that: described cushion is attached on carbanion selective membrane, and cushion is alkalescence, and pH scope is 7.5 ~ 10.
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CN111610239A (en) * | 2020-03-02 | 2020-09-01 | 湖南工业大学 | Electrochemical test strip for detecting electrolyte concentration and detection method thereof |
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CN113588759A (en) * | 2021-07-12 | 2021-11-02 | 成都云芯医联科技有限公司 | Siphon type ion selective electrode electrolyte detection test paper |
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