Electrode for electrochemical biosensor for selectively detecting trifluoperazine, electrochemical biosensor comprising same, and manufacturing method therefor
The electrode with lanthanum nickelate nanoparticles on an electrochemical biosensor enables sensitive and selective detection of trifluoperazine in biological samples without pretreatment, addressing the limitations of current biosensors.
Patent Information
- Application Number
- PCT/KR2024/001341
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-12-04
- Filing Date
- 2024-01-29
- Publication Date
- 2025-06-12
AI Technical Summary
Current electrochemical biosensors lack the sensitivity and selectivity required for rapid and efficient detection of trifluoperazine (TFP) in biological samples without sample pretreatment.
An electrode for an electrochemical biosensor is developed, featuring lanthanum nickelate nanoparticles with a perovskite structure formed on its surface. This electrode is designed to selectively detect trifluoperazine by enhancing electrochemical reactions.
The biosensor achieves sensitive and selective detection of trifluoperazine, allowing for quick analysis without sample pretreatment, and demonstrates excellent economic feasibility and selectivity even with small biological samples.
Smart Images

Figure KR2024001341_12062025_PF_FP_ABST
Abstract
Description
Electrode for an electrochemical biosensor for selectively detecting trifluoperazine, an electrochemical biosensor comprising the same, and a method for manufacturing the same
[0001] The present invention relates to an electrode for an electrochemical biosensor for selectively detecting trifluoperazine, an electrochemical biosensor including the same, and a method for manufacturing the same. The present invention relates to an electrode for an electrochemical biosensor for selectively detecting trifluoperazine, which not only enables measurement without pretreatment of a sample to be measured (urine, serum, etc.), but also detects trifluoperazine quickly, sensitively, and simply, an electrochemical biosensor including the same, and a method for manufacturing the same.
[0002]
[0003] Trifluoperazine (TFP), a phenothiazine derivative, possesses a variety of biological activities, including antipsychotic and antihypertensive effects. However, excessive use or overdosage can cause serious side effects. Therefore, regular monitoring of trifluoperazine (TFP) concentrations in the body is considered important as part of clinical treatment.
[0004] Meanwhile, the physical properties of nanomaterials are crucial for the development of high-performance electrochemical sensors. In particular, transition metal oxides such as nickel oxide (NiO) are considered promising electrode materials for various electrochemical applications due to their low cost, wide band gap, multiple reduction reaction characteristics, high surface-to-volume ratio, non-toxicity, environmental friendliness, and excellent catalytic activity. Furthermore, perovskites (NMs) have attracted considerable attention due to their potential in electrochemical energy storage and conversion and electrochemical catalysis.
[0005] Perovskite oxides have an AB03 structure, where A represents a large-radius rare-earth metal cation and B represents a small-radius transition metal cation. Due to these characteristics, perovskite oxides have higher structural, thermal, and chemical stability than single-metal oxides. Therefore, they are used in various fields, and among them, lanthanum nickel oxide (LaNi0, LNO) perovskite has excellent conductivity, chemical stability, and electrochemical activity, and is being utilized in various applications.
[0006]
[0007] The present invention has been devised to solve the above problems, and its purpose is to provide an electrode for an electrochemical biosensor capable of sensitively and selectively detecting trifluoperazine (TFP), an antipsychotic drug, and an electrochemical biosensor including the same, and a method for manufacturing the same.
[0008]
[0009] In order to solve the above-described problem, the electrode for an electrochemical biosensor for selectively detecting trifluoroperazine of the present invention may include an electrode and lanthanum nickelate nanoparticles having a perovskite structure formed on one surface of the electrode.
[0010] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticles may have a rhombus-shaped structure.
[0011] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticles may have a thickness of 5 to 11 μm.
[0012] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticles may have a crystalline size of 11 to 16 nm.
[0013] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticles may have an average particle size of 15 to 25 nm.
[0014] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticles may contain 58.2 to 60.2 wt% of lanthanum element, 22.4 to 24.4 wt% of nickel element, and 16.4 to 18.4 wt% of oxygen element based on the total wt%.
[0015] Meanwhile, the electrochemical biosensor for selectively detecting the trifluoperazine of the present invention may include an electrode for an electrochemical biosensor for selectively detecting the trifluoperazine of the present invention.
[0016] Furthermore, the method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoroperazine of the present invention may include a first step of preparing an electrode and an aqueous solution of lanthanum nickel oxide nanoparticles, respectively, and a second step of applying the aqueous solution of lanthanum nickel oxide nanoparticles to one surface of the electrode and then drying it to form lanthanum nickel oxide nanoparticles having a perosite structure with a thickness of 5 to 11 μm on one surface of the electrode.
[0017] In a preferred embodiment of the present invention, the lanthanum nickel oxide nanoparticle aqueous solution can be prepared by including the steps of: a 1-1 step of mixing a lanthanum precursor and a nickel precursor to prepare a metal mixture; a 1-2 step of adding and stirring sodium hydroxide (NaOH) and calcium carbonate (K2CO3) to the metal mixture to prepare a mixed metal composition; a 1-3 step of drying the mixed metal composition to obtain a dried mixed metal; a 1-4 step of calcining the dried mixed metal to prepare lanthanum nickel oxide nanoparticles having a perosite structure; and a 1-5 step of dissolving the lanthanum nickel oxide nanoparticles in ultrapure water and then ultrasonically treating the same to prepare a lanthanum nickel oxide nanoparticle aqueous solution.
[0018] In a preferred embodiment of the present invention, step 1-1 may produce a metal mixture by mixing a lanthanum precursor and a nickel precursor in a molar ratio of 1:0.8 to 1.2.
[0019] In a preferred embodiment of the present invention, the drying of steps 1-3 can be performed at a temperature of 40 to 60°C for 8 to 16 hours.
[0020] In a preferred embodiment of the present invention, the firing of steps 1 to 4 can be performed at a temperature of 600 to 800°C for 2 to 6 hours at a ramping rate of 3 to 5°C / min.
[0021]
[0022] The electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention, the electrochemical biosensor including the same, and the method for manufacturing the same enable efficient electrochemical quantitative and qualitative analysis of specific molecules.
[0023] In addition, the electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention, the electrochemical biosensor including the same, and the method for manufacturing the same have the possibility of being applied to the human body through detection in biological samples such as urine and serum.
[0024] In addition, the electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention, the electrochemical biosensor including the same, and the manufacturing method thereof are not only simple and easy to manufacture, but also have excellent economic feasibility due to low manufacturing cost.
[0025] In addition, the electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention, the electrochemical biosensor including the same, and the manufacturing method thereof can selectively detect trifluoperazine in a short period of time even with a small amount of biological sample.
[0026]
[0027] Figure 1(a) is a graph showing the XRD (X-ray diffraction) analysis performed on lanthanum nickel oxide nanoparticles, lanthanum oxide (La2O3), and nickel oxide (NiO) having a perosite structure manufactured in Example 1.
[0028] Figure 1(b) is a graph showing the FT-IR (Fourier transform infrared) spectrum of lanthanum nickel oxide nanoparticles, lanthanum oxide (La2O3), and nickel oxide (NiO) having a perosite structure manufactured in Example 1.
[0029] FIG. 2 is a graph for performing XPS analysis of lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Example 1, FIG. 2(a) shows an XPS full survey spectrum of lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Example 1, FIG. 2(b) shows a high-resolution XPS spectrum of La 3d in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Example 1, FIG. 2(c) shows a high-resolution XPS spectrum of Li 2d in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Example 1, and FIG. 2(d) shows a high-resolution XPS spectrum of O 1s in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Example 1.
[0030] FIG. 3 is a drawing showing field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and mapping using energy dispersive X-ray (EDX) of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, respectively. FIG. 3(a) and FIG. 3(b) are FESEM images of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, FIG. 3(c) to FIG. 3(e) are TEM images of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, FIG. 3(f) is a HRTEM image of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, and FIG. 3(g) is a drawing showing a selected area electron diffraction (SAED) pattern of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1. FIG. 3(h) is a mapping image of La atoms, Ni atoms, and O atoms mixed in lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, FIG. 3(i) is a mapping image of La atoms in lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, FIG. 3(j) is a mapping image of Ni atoms in lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, FIG. 3(k) is a mapping image of O atoms in lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1, and FIG. 3(l) is an EDX analysis graph of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Example 1.
[0031] FIG. 4(a) is a graph showing Nyquist plots of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1, the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, and the screen-printed carbon electrode (=SPCE), respectively.
[0032] Figure 4(b) shows a 5.0 mM [Fe(CN)6] solution containing 0.1 mM KCl. 3- / 4- This is a graph showing the CV curves of each of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1, the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, and the screen-printed carbon electrode (=SPCE).
[0033] FIG. 4(c) shows the results of cyclic voltammetry (CV) performed at 50 mV / s in 0.1 M PB (pH 7) containing 100 μM of trifluoroperazine to evaluate the electro-oxidation of trifluoroperazine in each of the trifluoroperazine detection electrode manufactured in Example 1 (= LNO / SPCE), the trifluoroperazine detection electrode manufactured in Comparative Example 1 (= La2O3 / SPCE), the trifluoroperazine detection electrode manufactured in Comparative Example 2 (= NiO / SPCE), and the screen-printed carbon electrode (= SPCE), and FIG. 4(d) is a graph showing the effects according to various loading amounts of the trifluoroperazine detection electrode manufactured in Example 1.
[0034] Figure 5(a) is a graph showing the effect of pH on the electrochemical behavior of 100 μM trifluoroperazine on the trifluoroperazine detection electrode manufactured in Example 1 through CV using various supporting electrolytes (pH 3 to 9) at 50 mV / s.
[0035] Figure 5(b) shows the results of measuring the electrochemical activity of the trifluoperazine detection electrode prepared in Example 1 for trifluoperazine oxidation through CV in various concentrations of trifluoperazine in 0.1 M phosphate buffer (PB; phosphate buffer) (pH 7).
[0036] FIG. 5(c) is a graph showing a resulting linear plot of the electrooxidation reaction and trifluoperazine concentration for the trifluoperazine detection electrode manufactured in Example 1, and FIG. 5(d) is a graph showing a linear plot of the log electrooxidation reaction versus the log trifluoperazine concentration.
[0037] Figure 6(a) is a graph showing CV curves for various scan rates of 20 to 160 mV / s in 100 μM trifluoroperazine dissolved in 0.1 M phosphate buffer (PB; phosphate buffer) (pH 7) for the trifluoroperazine detection electrode manufactured in Example 1, and Figure 6(b) is a graph showing the electrooxidation reaction (I pa ) vs. V 1 / 2 is a graph showing the linear relation, and Figure 6(c) shows the logarithmic electrooxidation reaction (I pa ) and the linear relationship between log V, and Fig. 6(d) shows the peak potential (E pa ; is a graph showing the relationship between peak potential and log V, and Fig. 6(e) is a diagram showing the electrooxidation mechanism.
[0038] Figure 7 is a graph showing the electrochemical characteristics of trifluoperazine in the trifluoperazine detection electrode manufactured in Example 1 by the DPV method (differential pulse voltammetry methode). Figure 7(a) is a DPV curve showing the degree of trifluoperazine detection in the trifluoperazine detection electrode manufactured in Example 1 at various concentrations of trifluoperazine dissolved in 0.1 M PB (pH 7), Figure 7(b) is a graph showing two linear plots of the electro-oxidation reaction (Ipa) current versus the concentration of trifluoperazine, and Figures 7(c) and 7(d) are graphs showing the electrochemical characteristics of trifluoperazine in 0.1 M PB (pH 7) as well as K as an interferent to evaluate the selectivity of the trifluoperazine detection electrode manufactured in Example 1. + , Cu 2+ , Na + , Cl - , SO4 2- , NO 2- , the results of DPV in a solution containing glucose (Glu), perphenazine (PPZ), promethazine (PMZ), prochlorperazine (PCP), and chloropromazine (CPZ).
[0039] Figures 8(a) and 8(b) are graphs showing the results of DPV performed on urine and serum to evaluate the applicability of the trifluoroperazine detection electrode manufactured in Example 1 to a biological environment.
[0040]
[0041] Hereinafter, with reference to the attached drawings, embodiments of the present invention will be described in detail so that those skilled in the art can easily implement the present invention. The present invention may be implemented in various different forms and is not limited to the embodiments described herein. In the drawings, parts irrelevant to the description have been omitted for clarity of description, and the same reference numerals are assigned to identical or similar components throughout the specification.
[0042]
[0043] The electrode for an electrochemical biosensor for selectively detecting trifluoroperazine of the present invention may include an electrode and lanthanum nickelate nanoparticles having a perovskite structure formed on one surface of the electrode.
[0044] At this time, the electrode may include various electrodes used in the art as a working electrode, and may preferably be a screen-printed carbon electrode, a glassy carbon electrode, or a carbon paste electrode, and more preferably may be a screen-printed carbon electrode.
[0045] Meanwhile, the lanthanum nickel oxide nanoparticles of the present invention may have a rhombus-shaped structure.
[0046] In addition, the lanthanum nickel oxide nanoparticles may have a thickness of 5 to 11 μm, preferably 6 to 10 μm, and more preferably 7 to 8 μm. If the thickness is less than 5 μm, there may be a problem of reduced reactivity, and if it exceeds 11 μm, I pa There may be a problem with the value being lowered.
[0047] Additionally, the lanthanum nickel oxide nanoparticles may have a crystalline size of 11 to 16 nm, preferably a crystalline size of 12 to 15 nm, and more preferably a crystalline size of 13 to 14 nm.
[0048] In addition, the lanthanum nickel oxide nanoparticles may have an average particle size of 15 to 25 nm, preferably a crystal size of 17 to 23 nm, and more preferably a crystal size of 19 to 21 nm. If the average particle size exceeds 25 nm, there may be a problem in that the performance of the electrochemical biosensor is deteriorated.
[0049] Additionally, lanthanum nickel oxide nanoparticles can have single crystalline properties.
[0050] In addition, the lanthanum nickel oxide nanoparticles may contain 58.2 to 60.2 wt%, preferably 58.7 to 59.7 wt%, of lanthanum element, 22.4 to 24.4 wt%, preferably 22.9 to 23.9 wt%, of nickel element, and 16.4 to 18.4 wt%, preferably 16.9 to 17.9 wt%, of oxygen element, based on the total wt%.
[0051]
[0052] Meanwhile, the electrochemical biosensor for selectively detecting trifluoperazine of the present invention may include the electrode for the electrochemical biosensor for selectively detecting trifluoperazine described above.
[0053]
[0054] Furthermore, the method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention includes the first step and the second step.
[0055] The first step of the method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoroperazine of the present invention may be to prepare an electrode and an aqueous solution of lanthanum nickel oxide nanoparticles, respectively. In this case, the electrode is as described above.
[0056] Additionally, the lanthanum nickel oxide nanoparticle aqueous solution can be manufactured by including steps 1-1 to 1-5.
[0057] Step 1-1 of the method for producing an aqueous solution of lanthanum nickel oxide nanoparticles may be a method for producing a metal mixture by mixing a lanthanum precursor and a nickel precursor. At this time, the lanthanum precursor and the nickel precursor may be mixed in a molar ratio of 1:0.8 to 1.2, preferably 1:0.9 to 1.1. If the molar ratio is outside this range, there may be a problem in producing the desired compound.
[0058] In addition, the lanthanum precursor may include at least one selected from lanthanum nitrate hexahydrate (La(NO3)3·6H2O), lanthanum chloride (LaCl3), and lanthanum (III) acetate sesquihydrate (La(OOCCH3)3·1.5H2O), and preferably lanthanum nitrate hexahydrate (La(NO3)3·6H2O).
[0059] In addition, the nickel precursor may include at least one selected from nickel nitrate hexahydrate (Ni(NO3)3·6H2O) and nickel chloride (NiCl2), and preferably nickel nitrate hexahydrate (Ni(NO3)3·6H2O).
[0060] Step 1-2 of the method for producing a lanthanum nickel oxide nanoparticle aqueous solution can produce a mixed metal composition by adding and stirring sodium hydroxide (NaOH) and calcium carbonate (K2CO3) to the metal mixture produced in step 1-1.
[0061] Steps 1-3 of the method for producing an aqueous solution of lanthanum nickel oxide nanoparticles can be performed by drying the mixed metal composition produced in steps 1-2 to obtain a dried mixed metal product. At this time, the drying can be performed at a temperature of 40 to 60°C, preferably 45 to 55°C, for 8 to 16 hours, preferably 10 to 14 hours.
[0062] Steps 1 to 4 of the method for producing an aqueous solution of lanthanum nickel oxide nanoparticles can produce lanthanum nickel oxide nanoparticles having a perosite structure by calcining the mixed metal dried product obtained in Steps 1 to 3. At this time, the lanthanum nickel oxide nanoparticles having a perosite structure are as described above. In addition, the calcination can be performed at a temperature of 600 to 800°C, preferably 650 to 750°C, at a ramping rate of 3 to 5°C / min, preferably 3.5 to 4.5°C / min, for 2 to 6 hours, preferably 3 to 5 hours.
[0063] Steps 1 to 5 of the method for producing a lanthanum nickel oxide nanoparticle aqueous solution can produce a lanthanum nickel oxide nanoparticle aqueous solution by dissolving the lanthanum nickel oxide nanoparticles produced in steps 1 to 4 in ultrapure water and then performing ultrasonic treatment.
[0064]
[0065] The second step of the method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoperazine of the present invention comprises applying the aqueous solution of lanthanum nickel oxide nanoparticles manufactured in the first step to one surface of the electrode, and then drying the solution to form lanthanum nickel oxide nanoparticles having a perosite structure on one surface of the electrode to a thickness of 5 to 11 μm, preferably 6 to 10 μm, and more preferably 7 to 8 μm. At this time, the drying can be performed in an oven at 40 to 60°C, preferably 45 to 55°C, for 2 to 20 minutes, preferably 7 to 13 minutes.
[0066]
[0067] Hereinafter, the present invention will be described in more detail through examples, but the following examples do not limit the scope of the present invention, and should be interpreted as helping to understand the present invention.
[0068]
[0069] Preparation Example 1: Preparation of lanthanum nickelate nanoparticles having a perovskite structure
[0070] (1) A metal mixture was prepared by mixing a lanthanum precursor and a nickel precursor in a molar ratio of 1:1. At this time, lanthanum nitrate hexahydrate (La(NO3)3·6H2O) was used as the lanthanum precursor, and nickel nitrate hexahydrate (Ni(NO3)3·6H2O) was used as the nickel precursor.
[0071] (2) 10 ml of 1.0 M sodium hydroxide (NaOH) and 10 ml of 1.2 M calcium carbonate (K2CO3) were added to the prepared metal mixture and stirred for 6 hours to prepare a mixed metal composition.
[0072] (3) The manufactured mixed metal composition was washed three times with water and ethanol, and then dried at a temperature of 50°C for 12 hours to obtain a dried mixed metal product.
[0073] (4) The obtained mixed metal dried product was calcined at a temperature of 700°C for 4 hours at a ramping rate of 4°C / min to produce lanthanum nickel oxide nanoparticles having a perosite structure.
[0074]
[0075] Experimental Example 1: Structural Analysis 1
[0076] In order to confirm the crystal phase and purity of the lanthanum nickel oxide nanoparticles, lanthanum oxide (La2O3), and nickel oxide (NiO) having a perosite structure manufactured in Preparation Example 1, X-ray diffraction (XRD) analysis was performed. XRD analysis was performed using a PANalytical X'PERT PRO diffractometer (EMPYREAN, Malvern Panalytical, Netherlands) using Cu Kα radiation (λ = 1.541Å), and the results are shown in Fig. 1(a) below.
[0077] As can be seen in Fig. 1(a), the diffraction peaks at 2θ values of 26.11°, 29.11°, 29.96°, 39.50°, 46.06°, 52.14°, 55.42°, 62.26°, 72.09°, and 79.13° can be indexed to the (100), (002), (101), (102), (110), (103), (112), (202), (203), and (114) planes of pure lanthanum oxide (La2O3) with a hexagonal structure, respectively.
[0078] Additionally, the diffraction peaks at 2θ values of 37.32°, 43.36°, 62.99°, 75.56°, and 79.56° can be indexed to the (111), (200), (220), (311), and (222) planes of pure nickel oxide (NiO) with a cubic structure, respectively.
[0079] In addition, the diffraction peaks of the lanthanum nickel oxide nanoparticles (denoted as LNO) having a perosite structure manufactured in Preparation Example 1 exhibit 2θ values of 23.16°, 32.79°, 40.53°, 47.34°, 53.08°, 58.78°, 68.74°, 69.63°, 74.06°, 78.49°, 83.38°, and 87.70°, which can be indexed to the (012), (110), (202), (024), (122), (214), (220), (208), (306), (134), (226), and (404) planes. Through this, it was confirmed that the lanthanum nickel oxide nanoparticles (denoted as LNO) having a perosite structure manufactured in Preparation Example 1 had a rhombohedral structure.
[0080] In addition, as can be confirmed in Fig. 1(a), the lanthanum nickel oxide nanoparticles, lanthanum oxide (La2O3), and nickel oxide (NiO) having a perosite structure manufactured in Preparation Example 1 have a sharp intensity peak, and no other peaks are detected, confirming that the purity of each material is high.
[0081] Meanwhile, as a result of calculating the crystalline size, lanthanum oxide (La2O3) was calculated to be approximately 5.62 nm, nickel oxide (NiO) was calculated to be approximately 6.21 nm, and lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 were calculated to be 13.68 nm.
[0082]
[0083] Experimental Example 2: Structural Analysis 2
[0084] The Fourier transform infrared (FT-IR) spectra of lanthanum nickel oxide nanoparticles, lanthanum oxide (La2O3), and nickel oxide (NiO) having a perosite structure prepared in Preparation Example 1 were measured. The FT-IR spectra were measured using The JASCO 4600LE (Shimadzu, Japan) equipment at a wavelength of 4000 to 400 cm -1 The measurements were made over a range of wavenumbers, and the results are shown in Figure 1(b).
[0085] As can be seen in Figure 1(b), 657cm -1 and 1467cm -1 The absorption band is due to the La-O vibrational mode and the presence of carbonate or bicarbonate ions. Also, 441 cm -1 The absorption band is MO(Ni-O) stretching vibration, 1040 cm -1 The absorption band is due to the MOM (Ni-O-Ni) stretching vibration at 3432 cm -1 The broad band observed at 1638 cm is due to OH stretching. -1 The band is due to the HOH bending vibration mode.
[0086] Meanwhile, in the spectrum of the lanthanum nickel oxide nanoparticles (denoted as LNO) having a perosite structure manufactured in Preparation Example 1, both lanthanum oxide (La2O3) bands and nickel oxide (NiO) bands were observed, and through these results, it was confirmed that the lanthanum nickel oxide nanoparticles having a perosite structure were successfully manufactured.
[0087]
[0088] Experimental Example 3: Structural Analysis 3
[0089] To confirm the chemical composition and valence state of the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1, XPS analysis was performed. The XPS analysis was performed using an X-ray photoelectron microscope (XPS) of a Thermo science multi-lab 2000 (Thermo Fisher Scientific, USA), and the results are shown in Fig. 2.
[0090] FIG. 2(a) shows the XPS full survey spectrum of lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1, FIG. 2(b) shows the high-resolution XPS spectrum of La 3d in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1, FIG. 2(c) shows the high-resolution XPS spectrum of Li 2d in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1, and FIG. 2(d) shows the high-resolution XPS spectrum of O 1s in lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1.
[0091] As can be seen in Figure 2(b), the binding energy of La 3d is La 3d 5 / 2 It exhibits two broad peaks at 834.26 eV and 837.6 eV attributed to the satellite, which confirms that La is in the +3 oxidation state. In addition, as can be seen in Fig. 2(c), the Li 2d decomposition spectrum is Ni 2p 3 / 2 and Ni 2p 1 / 2 The binding energies are 854.77 eV and 872.13 eV, corresponding to Ni 2p 3 / 2 The satellite peak due to was observed at 861.21 eV, which is Ni3+ It was confirmed that this was due to . In addition, as can be confirmed in Fig. 2(d), O 1s was confirmed to have two binding energy peaks at 529.42 eV and 530.91 eV, which were attributed to metal-oxygen or lattice oxygen vacancies (O1) and surface-adsorbed oxygen vacancies (O2).
[0092]
[0093] Experimental Example 4: Structural Analysis 4
[0094] Field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and mapping using energy dispersive X-ray (EDX) of the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 were performed using JEOL-JSM-6500F and JEOL-JEM-2100F (JEOL, USA) equipment, respectively, and are shown in Fig. 3.
[0095] FIG. 3(a) and FIG. 3(b) are FESEM images of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, FIG. 3(c) to FIG. 3(e) are TEM images of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, FIG. 3(f) is an HRTEM image of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, FIG. 3(g) is a drawing showing a selected area electron diffraction (SAED) pattern of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, FIG. 3(h) is a mapping image showing a mixture of La atoms, Ni atoms, and O atoms of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, and FIG. 3(i) is a mapping image showing a mixture of La atoms, Ni atoms, and O atoms of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1. Fig. 3(j) is a La atom mapping image of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, Fig. 3(k) is a O atom mapping image of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1, and Fig. 3(l) is an EDX analysis graph of lanthanum nickel oxide nanoparticles having a perovskite structure manufactured in Preparation Example 1.
[0096] As can be seen in FIGS. 3(a) and 3(b), the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 were confirmed to have an aggregated spherical particle shape. In addition, as can be seen in FIGS. 3(c) to 3(e), the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1, which are spherical, were confirmed to have an average particle size of ±20 nm.
[0097] As can be seen in Fig. 3(f), the lattice fringe of the d-spacing of the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 was measured to be 0.275 nm, which was close to the theoretical d-value of 0.272 nm belonging to the (110) plane of the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 with a rhombohedral structure.
[0098] As can be seen in Fig. 3(g), the bright diffraction spots of the (021), (110), and (024) planes measured in the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 can be indexed to the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 having a rhombic structure. From these results, it was confirmed that the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 had single crystalline characteristics.
[0099] As can be seen from FIGS. 3(h) to 3(k), it was confirmed that the La, Ni, and O elements present in the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 were uniformly distributed. Specifically, as can be seen from FIG. 3(l), it was confirmed that the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 contained 59.2 wt% of lanthanum element, 23.4 wt% of nickel element, and 17.4 wt% of oxygen element with respect to the total wt%.
[0100]
[0101] Example 1: Preparation of trifluoperazine detection electrode
[0102] (1) A screen-printed carbon electrode was prepared as a working electrode. In addition, 5.0 mg of lanthanum nickel oxide nanoparticles having a perosite structure prepared in Preparation Example 1 were dissolved in 1.0 ml of ultrapure water, and the solution was sonicated for 30 minutes to prepare an aqueous solution of lanthanum nickel oxide nanoparticles.
[0103] (2) 8.0 μL of the manufactured lanthanum nickel oxide nanoparticle aqueous solution was dropped onto one side of the working electrode, and then dried in an oven at 50°C for 10 minutes to manufacture a trifluoroperazine detection electrode in which lanthanum nickel oxide nanoparticles having a perosite structure were formed on one side of the working electrode to a thickness of 8.0 μm.
[0104]
[0105] Comparative Example 1: Preparation of trifluoperazine detection electrode
[0106] (1) A screen-printed carbon electrode was prepared as a working electrode. In addition, 5.0 mg of lanthanum oxide (La2O3) was dissolved in 1.0 ml of ultrapure water and sonicated for 30 minutes to prepare an aqueous lanthanum oxide solution.
[0107] (2) 8.0 μL of the prepared lanthanum oxide aqueous solution was dropped onto one side of the working electrode, and then dried in an oven at 50°C for 10 minutes to prepare a trifluoroperazine detection electrode in which lanthanum oxide was formed to a thickness of 8.0 μm on one side of the working electrode.
[0108]
[0109] Comparative Example 2: Preparation of trifluoperazine detection electrode
[0110] (1) A screen-printed carbon electrode was prepared as a working electrode. In addition, 5.0 mg of nickel oxide (NiO) was dissolved in 1.0 ml of ultrapure water and sonicated for 30 minutes to prepare a nickel oxide aqueous solution.
[0111] (2) 8.0 μl of the prepared nickel oxide aqueous solution was dropped onto one side of the working electrode, and then dried in an oven at 50°C for 10 minutes to prepare a trifluoroperazine detection electrode in which nickel oxide was formed to a thickness of 8.0 μm on one side of the working electrode.
[0112]
[0113] Experimental Example 5: Electrochemical Analysis
[0114] In order to perform electrochemical analysis on the trifluoroperazine detection electrodes manufactured in Example 1 and Comparative Examples 1 and 2, a three-electrode system was manufactured. Specifically, the trifluoroperazine detection electrode manufactured in Example 1, the trifluoroperazine detection electrode manufactured in Comparative Example 1, the trifluoroperazine detection electrode manufactured in Comparative Example 2, and a screen-printed carbon electrode (SPCE) were each used as working electrodes, a platinum wire was used as a counter electrode, and a saturated Ag / AgCl electrode was used as a reference electrode.
[0115]
[0116] (1) Electrochemical impedance spectroscopy (EIS)
[0117] Electrochemical impedance spectroscopy (EIS) was performed in 0.1 M KCl and 5.0 mM [Fe(CN)6] 3- / 4-The electron transfer characteristics of the trifluoroperazine detection electrode manufactured in Example 1, the trifluoroperazine detection electrode manufactured in Comparative Example 1, the trifluoroperazine detection electrode manufactured in Comparative Example 2, and the screen-printed carbon electrode were evaluated. Electrochemical impedance spectroscopy (EIS) was performed at a voltage frequency of 0.1 to 100 kHz and an amplitude potential of 5 mV.
[0118] Figure 4(a) is a graph showing the Nyquist plots of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1, the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, and the screen-printed carbon electrode (=SPCE), respectively. The Nyquist plots represent the charge transfer resistance (R ct ; charge transfer resistance), double layer capacitance (C dI ; double layer capacitance), Warburg resistance (Z W ; Warburg resistance), solution resistance (R s ; solution resistance) was used. As can be seen in Fig. 4(a), the screen-printed carbon electrode (=SPCE) has a charge transfer resistance (R) of 35 Ω. ct ) represents an empty electrode and [Fe(CN)6] 3- / 4- It is due to the solution performance. In addition, a large semicircle was observed in the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, and the charge transfer resistance (R) of 1148 Ω ct), which indicates that the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1 had poor performance in terms of electron transfer and conductivity. In addition, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2 had a charge transfer resistance (R) of 686 Ω. ct ), which is lower than the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1. This result is because NiO has lower semiconductor properties than La2O3, and NiO and [Fe(CN)6] 3- / 4- It was confirmed that the electron transfer rate between the redox systems was improved. Meanwhile, the trifluoroperazine detection electrode (= LNO / SPCE) manufactured in Example 1 had a charge transfer resistance (R) of 254 Ω. ct ), and it was confirmed that the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1 showed higher electron transfer kinetics than other detection electrodes. In other words, it was confirmed that the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1 had excellent conductivity and a fast electron transfer medium, and was thus an electrochemical detection material.
[0119]
[0120] (2) CV curve
[0121] Figure 4(b) shows a 5.0 mM [Fe(CN)6] solution containing 0.1 mM KCl. 3- / 4-In this graph, the CV curves of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1, the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, and the screen-printed carbon electrode (=SPCE) were measured and displayed, respectively. As can be seen in Fig. 4(b), compared to the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1 and the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1 showed the highest redox peak current. This indicates that the lanthanum nickel oxide nanoparticles having a perosite structure manufactured in Preparation Example 1 exhibited excellent electrochemical behavior and [Fe(CN)6] 3- / 4- It was confirmed that the trifluoroperazine detection electrode (= LNO / SPCE) manufactured in Example 1 exhibited strong electrocatalytic activity for the redox reaction. In addition, the peak-to-peak separation (ΔEp) of the trifluoroperazine detection electrode (= LNO / SPCE) manufactured in Example 1 was 0.23 V, which was lower than the ΔEp of other detection electrodes, confirming that the electron transfer rate was fast. In addition, the trifluoroperazine detection electrode (= LNO / SPCE) manufactured in Example 1 exhibited a redox peak current (I pa / I pc ; redox peak current) scan speed is 20 mV / s -1 at 200mV / s -1 It was confirmed that it increases linearly as the number increases.
[0122] Meanwhile, the effective surface area of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1 was 0.659 cm 2 , the effective surface area of the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1 was 0.476 cm2 , the effective surface area of the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2 is 0.605 cm 2 was calculated as
[0123] In conclusion, it can be confirmed that the trifluoroperazine detection electrode manufactured in Example 1 has a large effective surface area and excellent conductivity compared to other detection electrodes, thereby promoting electrochemical detection performance for trifluoroperazine (TFP).
[0124]
[0125] (3) Electrocatalytic activity for trifluoroperazine
[0126] In order to evaluate the electro-oxidation of trifluoroperazine in each of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1, the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1, the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2, and the screen-printed carbon electrode (=SPCE), cyclic voltammetry (CV) was performed at 50 mV / s in 0.1 M PB (pH 7) containing 100 μM of trifluoroperazine, and the results are shown in Fig. 4(c). As can be seen in Fig. 4(c), an oxidation peak (I) was observed in all detection electrodes. pa ) appeared, and no reduction peak appeared in the reverse scan, which confirmed that trifluoroperazine was irreversibly oxidized on the detection electrode surface. Meanwhile, the trifluoroperazine detection electrode (= LNO / SPCE) manufactured in Example 1 had a peak potential of 0.759 V, indicating a higher oxidation peak (I) for trifluoroperazine. pa ) was confirmed to have.
[0127] As a result, the oxidation peak (I) of the trifluoroperazine detection electrode (=LNO / SPCE) manufactured in Example 1 pa) is 48.59 μA, the oxidation peak (I) of the trifluoroperazine detection electrode (=NiO / SPCE) manufactured in Comparative Example 2 pa ) is 38.10 μA, the oxidation peak (I) of the trifluoroperazine detection electrode (=La2O3 / SPCE) manufactured in Comparative Example 1 pa ) is 34.91 μA, the oxidation peak (I) of the screen-printed carbon electrode (=SPCE) pa ) was measured as 23.45 μA. The oxidation peak (I pa ) showed excellent electrochemical activity for trifluoroperazine detection.
[0128] Fig. 4(d) is a graph showing the effect according to various loading amounts of the trifluoroperazine detection electrode manufactured in Example 1. As can be seen in Fig. 4(d), the electro-oxidation reaction of 100 μM trifluoroperazine was confirmed to steadily increase as the volume increased from 4 μL to 8 μL. However, when the volume increased to 10 μL, the electro-oxidation reaction decreased conversely. This is believed to be due to the high loading level of the trifluoroperazine detection electrode manufactured in Example 1, which increases the interfacial transfer resistance and hinders electron transfer. In conclusion, it was found that the optimal capacity for trifluoroperazine detection was 8 μL.
[0129] Meanwhile, the effect of pH on the electrochemical behavior of 100 μM trifluoroperazine on the trifluoroperazine detection electrode prepared in Example 1 was measured through CV using various supporting electrolytes (pH 3 to 9) at 50 mV / s, and the results are shown in Fig. 5(a). As can be seen in Fig. 5(a), the electro-oxidation reaction of trifluoroperazine was significantly enhanced as the pH increased from 3 to 7. On the other hand, when the pH increased from 8 to 9, the electro-oxidation reaction of trifluoroperazine was confirmed to decrease. This decrease indicates that protonation was low during the electrode reaction. In conclusion, considering the high sensitivity of trifluoroperazine detection, the ideal supporting electrolyte is pH 7.
[0130] Furthermore, the electrochemical activity of the trifluoperazine detection electrode prepared in Example 1 for trifluoperazine oxidation was measured through CV in various concentrations of trifluoperazine in 0.1 M phosphate buffer (PB; phosphate buffer) (pH 7), and the results are shown in Fig. 5(b). As can be seen in Fig. 5(b), the electrooxidation reaction of trifluoperazine was confirmed to gradually increase as the trifluoperazine concentration increased from 25 μM to 200 μM.
[0131] Meanwhile, Fig. 5(c) shows the resulting linear plot of the electrooxidation reaction and the trifluoroperazine concentration, and as can be seen in Fig. 5(c), it was confirmed that the trifluoroperazine detection electrode manufactured in Example 1 had excellent sensitivity for trifluoroperazine oxidation.
[0132] In addition, Fig. 5(d) shows a linear plot of the log electrooxidation reaction versus the log trifluoroperazine concentration, and as can be seen in Fig. 5(d), the obtained slope value is 0.85, which is almost equal to 1, confirming that the trifluoroperazine detection in the trifluoroperazine detection electrode manufactured in Example 1 follows first-order kinetics.
[0133] Meanwhile, the CV curves for various scan rates of 20 to 160 mV / s in 100 μM trifluoperazine dissolved in 0.1 M phosphate buffer (PB; phosphate buffer) (pH 7) for the trifluoperazine detection electrode manufactured in Example 1 are shown in Fig. 6(a). As can be confirmed in Fig. 6(a), it was confirmed that the response of the electrooxidation reaction increased as the scan rate increased to 160 mV / s.
[0134] In addition, Fig. 6(b) shows the electrooxidation reaction (I pa ) vs. V 1 / 2 It shows a linear relation, and as can be seen in Fig. 6(b), it was confirmed that the electrooxidation of trifluoroperazine was controlled by the diffusion process on the surface of the trifluoroperazine detection electrode manufactured in Example 1.
[0135] Furthermore, Fig. 6(c) shows the logarithmic electrochemical oxidation reaction (I pa ) and the log V, and as can be seen in Fig. 6(c), the log electrooxidation reaction (I) of the trifluoroperazine detection electrode manufactured in Example 1 pa) was confirmed to have good linearity with log V. Since the observed linear slope of 0.58 is very close to 0.50, it was confirmed that the trifluoroperazine oxidation of the electrochemical biosensor including the trifluoroperazine detection electrode manufactured in Example 1 has a diffusion-controlled process.
[0136] Meanwhile, Fig. 6(d) shows the peak potential (E pa ; peak potential) and the log V, and as can be seen in Fig. 6(d), as the scan speed increases, the peak potential (E pa ; A change in peak potential) was observed. Specifically, the trifluoroperazine detection electrode manufactured in Example 1 was found to transfer two electrons by trifluoroperazine oxidation. This electro-oxidation mechanism is shown in Fig. 6(e). The trifluoroperazine detection electrode manufactured in Example 1 oxidizes trifluoroperazine (TFP) containing N and S atoms, thereby converting the oxidized trifluoroperazine (Oxidized TFP) into a cationic radical containing N and S atoms.
[0137]
[0138] (4) Electrochemical measurement of trifluoroperazine
[0139] The electrochemical properties of trifluoroperazine were measured at the trifluoroperazine detection electrode manufactured in Example 1 using the DPV method (differential pulse voltammetry methode) and are shown in Fig. 7.
[0140] Figure 7(a) is a DPV curve showing the degree of detection of trifluoperazine at the trifluoperazine detection electrode prepared in Example 1 in various concentrations of trifluoperazine dissolved in 0.1 M PB (pH 7). As can be seen in Figure 7(a), the electro-oxidation reaction (I pa) was confirmed to increase linearly as the trifluoperazine concentration increased from 0.165 μM to 495.5 μM.
[0141] Figure 7(b) shows the electrooxidation reaction (I pa ) is a graph showing two linear plots of current versus trifluoperazine concentration. As can be seen in Fig. 7(b), the first linear plot was observed in the range of 0.165 to 235.5 μM, and the second linear plot was observed in the range of 235.5 to 495.5 μM. This confirms that a rapid response was obtained at a low concentration of trifluoperazine due to the rapid molecular movement of trifluoperazine. However, it was confirmed that the movement of trifluoperazine was hindered when the concentration of trifluoperazine was further increased.
[0142] Meanwhile, through these results, the detection limit (LOD; limit of detection) of the trifluoroperazine detection electrode manufactured in Example 1 was 0.017 μM, the quantification limit (LOQ; limit of quantification) was 0.059 μM, and the sensitivity was 0.059 μA / μM. -1 cm -2 It was calculated as follows. Compared to the previously used trifluoperazine detection biosensor, it was confirmed to have a low detection limit and excellent sensitivity.
[0143] Figures 7(c) and 7(d) show the results of evaluating the selectivity of the trifluoroperazine detection electrode manufactured in Example 1, in which 20 μM trifluoroperazine was added to 0.1 M PB (pH 7) as well as K as an interferent. + , Cu 2+ , Na + , Cl - , SO4 2- , NO 2-, glucose (Glu), perphenazine (PPZ), promethazine (PMZ), prochlorperazine (PCP), and chloropromazine (CPZ) are graphs showing the results of DPV in a solution dissolved in the solution. As can be seen in Fig. 7(c) and Fig. 7(d), even when 10 times the amount of interfering substances is included, the electrooxidation reaction (I pa ) was confirmed to have no noticeable change. In other words, the relative error of the signal was only ±5%, confirming that the trifluoroperazine detection electrode manufactured in Example 1 had excellent selectivity for trifluoroperazine detection.
[0144]
[0145] (5) Detection of trifluoperazine in biological samples
[0146] FIG. 8(a) and FIG. 8(b) are graphs showing the results of DPV in urine and serum to evaluate the applicability of the trifluoperazine detection electrode manufactured in Example 1 to a biological environment. DPV was performed using various concentrations of trifluoperazine. As can be seen in FIG. 8(a) and FIG. 8(b), the recovery rates were measured to be 98.4% to 99.6% in urine and 99.2 to 99.9% in serum. In addition, the relative standard deviation (RSD) value obtained from urine was calculated to be 1.81%, and the relative standard deviation value obtained from serum was calculated to be 1.61%.
[0147] As a result, it was confirmed that the biosensor using the trifluoroperazine detection electrode manufactured in Example 1 was reliable and feasible for trifluoroperazine oxidation in actual human samples.
[0148]
[0149] Simple modifications or changes of the present invention can be easily implemented by a person having ordinary skill in the art, and all such modifications or changes can be considered to be included in the scope of the present invention.
Claims
1. Electrode; and Lanthanum nickelate nanoparticles having a perovskite structure formed on one surface of the electrode; An electrode for an electrochemical biosensor for selectively detecting trifluoperazine, characterized by including:
2. In paragraph 1, An electrode for an electrochemical biosensor for selectively detecting trifluoroperazine, characterized in that the above lanthanum nickel oxide nanoparticles have a rhombohedral structure.
3. In paragraph 1, An electrode for an electrochemical biosensor for selectively detecting trifluoroperazine, characterized in that the above lanthanum nickel oxide nanoparticles have a thickness of 5 to 11 μm.
4. In paragraph 1, An electrode for an electrochemical biosensor for selectively detecting trifluoroperazine, characterized in that the above lanthanum nickel oxide nanoparticles have a crystalline size of 11 to 16 nm.
5. In paragraph 1, An electrode for an electrochemical biosensor for selectively detecting trifluoroperazine, characterized in that the above lanthanum nickel oxide nanoparticles have an average particle size of 15 to 25 nm.
6. In paragraph 1, An electrode for an electrochemical biosensor for selectively detecting trifluoroperazine, characterized in that the above lanthanum nickel oxide nanoparticles contain 58.2 to 60.2 wt% of lanthanum element, 22.4 to 24.4 wt% of nickel element, and 16.4 to 18.4 wt% of oxygen element with respect to the total weight%.
7. An electrochemical biosensor for selectively detecting trifluoperazine comprising an electrode for the electrochemical biosensor of claim 1.
8. Step 1: Preparing an electrode and a lanthanum nickel oxide nanoparticle aqueous solution, respectively; and A second step of applying the above lanthanum nickel oxide nanoparticle aqueous solution to one surface of the electrode and then drying it to form lanthanum nickel oxide nanoparticles having a perosite structure with a thickness of 5 to 11 ㎛ on one surface of the electrode; A method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoperazine, characterized in that it comprises:
9. In the 8th paragraph, the aqueous solution of lanthanum nickel oxide nanoparticles Step 1-1 of preparing a metal mixture by mixing a lanthanum precursor and a nickel precursor; Sodium hydroxide (NaOH) and calcium carbonate (K) were added to the above metal mixture. 2 CO 3 ) and stirring to prepare a mixed metal composition; Step 1-2; Step 1-3 of drying the above mixed metal composition to obtain a mixed metal dried product; Step 1-4 of producing lanthanum nickel oxide nanoparticles having a perosite structure by calcining the above mixed metal dry material; and Step 1-5 of preparing an aqueous solution of lanthanum nickel oxide nanoparticles by dissolving the lanthanum nickel oxide nanoparticles in ultrapure water and then performing ultrasonic treatment; A method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoperazine, characterized in that the electrode is manufactured including:
10. In paragraph 9, The above step 1-1 prepares a metal mixture by mixing a lanthanum precursor and a nickel precursor in a molar ratio of 1:0.8 to 1.2, The drying in steps 1 to 3 above is performed at a temperature of 40 to 60℃ for 8 to 16 hours. A method for manufacturing an electrode for an electrochemical biosensor for selectively detecting trifluoperazine, characterized in that the sintering in steps 1 to 4 is performed at a temperature of 600 to 800°C for 2 to 6 hours at a ramping rate of 3 to 5°C / min.
Citation Information
Patent Citations
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