CN111398390A - 纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 - Google Patents
纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 Download PDFInfo
- Publication number
- CN111398390A CN111398390A CN202010377333.1A CN202010377333A CN111398390A CN 111398390 A CN111398390 A CN 111398390A CN 202010377333 A CN202010377333 A CN 202010377333A CN 111398390 A CN111398390 A CN 111398390A
- Authority
- CN
- China
- Prior art keywords
- photo
- molybdenum carbide
- dopamine
- carbon paste
- paste electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910039444 MoC Inorganic materials 0.000 title claims abstract description 50
- -1 molybdenum carbide modified carbon Chemical class 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229960003638 dopamine Drugs 0.000 claims abstract description 38
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 230000004044 response Effects 0.000 claims abstract description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003755 preservative agent Substances 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- CNEOGBIICRAWOH-UHFFFAOYSA-N methane;molybdenum Chemical compound C.[Mo] CNEOGBIICRAWOH-UHFFFAOYSA-N 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 2
- 239000004475 Arginine Substances 0.000 claims description 2
- LEVWYRKDKASIDU-QWWZWVQMSA-N D-cystine Chemical compound OC(=O)[C@H](N)CSSC[C@@H](N)C(O)=O LEVWYRKDKASIDU-QWWZWVQMSA-N 0.000 claims description 2
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 2
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 2
- AGPKZVBTJJNPAG-WHFBIAKZSA-N L-isoleucine Chemical compound CC[C@H](C)[C@H](N)C(O)=O AGPKZVBTJJNPAG-WHFBIAKZSA-N 0.000 claims description 2
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 claims description 2
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 2
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 2
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 2
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 claims description 2
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 claims description 2
- ROHFNLRQFUQHCH-UHFFFAOYSA-N Leucine Natural products CC(C)CC(N)C(O)=O ROHFNLRQFUQHCH-UHFFFAOYSA-N 0.000 claims description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004472 Lysine Substances 0.000 claims description 2
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims description 2
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims description 2
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004473 Threonine Substances 0.000 claims description 2
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 claims description 2
- 235000004279 alanine Nutrition 0.000 claims description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 2
- 235000018417 cysteine Nutrition 0.000 claims description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 2
- 229960003067 cystine Drugs 0.000 claims description 2
- 235000013922 glutamic acid Nutrition 0.000 claims description 2
- 239000004220 glutamic acid Substances 0.000 claims description 2
- 229960000310 isoleucine Drugs 0.000 claims description 2
- AGPKZVBTJJNPAG-UHFFFAOYSA-N isoleucine Natural products CCC(C)C(N)C(O)=O AGPKZVBTJJNPAG-UHFFFAOYSA-N 0.000 claims description 2
- 229930182817 methionine Natural products 0.000 claims description 2
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004474 valine Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 5
- 239000008055 phosphate buffer solution Substances 0.000 claims 2
- 229960003767 alanine Drugs 0.000 claims 1
- 229960003121 arginine Drugs 0.000 claims 1
- 229960002433 cysteine Drugs 0.000 claims 1
- 229960002989 glutamic acid Drugs 0.000 claims 1
- 229960003136 leucine Drugs 0.000 claims 1
- 229960003646 lysine Drugs 0.000 claims 1
- 229960004452 methionine Drugs 0.000 claims 1
- 229960005190 phenylalanine Drugs 0.000 claims 1
- 229960002429 proline Drugs 0.000 claims 1
- 229960001153 serine Drugs 0.000 claims 1
- 229960002898 threonine Drugs 0.000 claims 1
- 229960004295 valine Drugs 0.000 claims 1
- 238000001514 detection method Methods 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000012886 linear function Methods 0.000 description 4
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000003745 diagnosis Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 description 2
- 239000002858 neurotransmitter agent Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000013076 target substance Substances 0.000 description 2
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 1
- 206010062767 Hypophysitis Diseases 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229960001149 dopamine hydrochloride Drugs 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 210000003016 hypothalamus Anatomy 0.000 description 1
- 238000000444 liquid chromatography-electrochemical detection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000036651 mood Effects 0.000 description 1
- 230000001537 neural effect Effects 0.000 description 1
- 210000002569 neuron Anatomy 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 210000003635 pituitary gland Anatomy 0.000 description 1
- 230000009090 positive inotropic effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
本发明属于分析化学与光致电化学传感器领域,具体涉及纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用。通过超声剥离方法剥离纳米碳化钼,将其修饰到碳糊电极上,构建了碳化钼修饰碳糊电极光电化学传感器。该传感器对多巴胺具有选择性响应。方法简单,成本低。
Description
技术领域
本发明属于分析化学与光致电化学传感器领域,具体为一种检测多巴胺的纳米碳化钼修饰碳糊电极光致电化学传感器制备方法。另外,本发明还涉及采用所述的光致电化学传感器测多巴胺的方法。
背景技术
多巴胺是一种下丘脑和脑垂体腺中的关键神经元物质,中枢神经系统中多巴胺的浓度则会直接影响到人们的情绪,同时多巴胺的大剂量使用时有正性肌力作用,而且收缩血管的作用明显,同时能够使血压升高。多巴胺的测定方法的研究在对于神经生理学研究、疾病诊断及其相关药物的质量控制都具有十分重要的意义。因此,检测这一类微量神经递质以及其代谢产物对研究这一类递质的生理机能和有关的疾病诊断显得极其重要。在目前测定盐酸多巴胺的方法主要分为毛细管电泳法、分光光度法、高效液相色谱法、电化学分析法以及化学发光法等几类。其中液相色谱分离-电化学检测法是目前在生物样品中测定多巴胺的最为有效的方法。这些方法无法满足实际需要。光致电化学分析法因为其测定灵敏度高、方法简单快捷,从而在分析检测中也获得了广泛的应用与发展。
发明内容
鉴于现有技术的不足,本发明的目的在于提供一种检测多巴胺的纳米碳化钼修饰电极光致电化学传感器制备方法及应用,以及提供一种采用所述的光致电化学传感器测多巴胺的方法。
本发明的目的是这样实现的:用纳米碳化钼修饰碳糊电极,构建光致电化学传感器以实现对多巴胺的测定;一种检测多巴胺的纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用,包括如下步骤:
(1)纳米碳化钼的制备
取1mg~50mg碳化钼(MoC)与1mL~100mL N,N-二甲基甲酰胺于烧杯中,将小磁子放入烧杯中,然后用保鲜膜封住烧杯杯口,置于磁力搅拌器中搅拌1min~100min,之后将小磁子取出,最后把用保鲜膜封好的小烧杯放入超声波清洗器中超声0.1h-100h,得剥离的MoC。利用透射电镜对碳化钼的形貌表征(图1)。从图1(A)中可以知,剥离的MoC是薄层片状结构,且片层较薄。而未剥离的MoC有局部阴影,这说明未剥离的MoC是多层MoC叠加在一起形成的片状结构,TEM图像中的黑色阴影部分说明MoC试剂粉末分散的不均匀,而且颜色深浅不一同时也说明了厚度存在较大的差异。从两个图的对比中可以看出,超声剥离对于MoC的分散有显著的效果。
(2)纳米碳化钼修饰碳糊电极的制备
吸取1μL~50μL纳米碳化钼溶液滴涂于刚处理过的碳糊电极的表面并将其铺展开,做好标记,置于泡沫板上使其自然干燥,得纳米碳化钼修饰碳糊电极光致电化学传感器。
一种利用上述方法制备的光致电化学传感器检测多巴胺含量的方法,将光致电化学传感器插入含多巴胺的PBS溶液中时,多巴胺被氧化,得光致电化学信号I,以I为分析信号,进行多巴胺的测定。
由于上述方法制备的光致电化学传感器可以检测多巴胺,因此,本发明提供了光致电化学传感器在检测多巴胺含量中的应用。
与现有技术相比,本发明涉及的光致电化学传感器具有如下优点和显著地进步:目标物多巴胺的浓度在1.0×10-10M到1.0×10-5M范围内与光致电化学信号成线性函数关系式。线性函数关系式为:I/nA=570.7log(c/M)+6459.5(c是多巴胺的浓度),其中R2=0.9901,相对标准偏差(RSD)为3.21%,检出限为3.0×10-11M。
碳糊电极的光致电信号趋于零,这是因为没有感光材料可以激发。而碳化钼修饰的碳糊电极有明显的电流峰值。同时,通过剥离的碳化钼与未剥离的碳化钼相比较,剥离的碳化钼修饰的碳糊电极比未剥离的碳化钼修饰的碳糊电极电流峰值大,电流变化更为稳定平稳。因此,说明成功构建了基于碳化钼修饰碳糊电极的传感器,剥离的碳化钼修饰的碳糊电极具有良好的光致电现象。
以上所用的PBS浓度为10mM,由Na2HPO4、Na2HPO4和NaCl组成,其中NaCl的浓度为0.9%。
附图说明
图1透射电镜图。剥离的碳化钼(A);未剥离的碳化钼(B)。
图2不同电极光致电化学信号。A、D、F为裸电极、剥离碳化钼修饰电极、未剥离碳化钼修饰电极在PBS中的响应,B、C、E为裸电极、剥离碳化钼修饰电极、未剥离碳化钼修饰电极在含1mM DA的PBS中的响应。
图3pH优化。左图,a`~e`是pH 6.5~8.5时剥离MoC修饰电极的光致电化学响应;a~e是pH 6.5~8.5时裸电极的光致电化学响应;右图为修饰电极与裸电极信号差值折线图。
图4电位优化。左图,A~G是电压为-0.3V~0.3V时剥离MoC修饰电极在含1mM DA的PBS中的响应;a~g电压为-0.3V~0.3V时裸电极的光致电化学响应。右图为修饰电极与裸电极信号差值折线图。
图5纳米碳化钼用量优化。左图,A~E是修饰剂体积为5~25mL时剥离MoC修饰电极的光致电化学响应;a~e裸电极的光致电化学响应;右图为修饰电极与裸电极信号差值折线图
图6光致电化学信号与多巴胺浓度关系图。
具体实施方式
下面结合具体实施例进一步说明本发明,但不构成对发明的进一步限制。
实施例1pH优化
将电极分别在pH为6.5、7.0、7.4、8.0、8.5、9.0的10mM PBS中测定光致电化学信号。图3为在不同pH条件下测定的光致电化学信号响应。可以看出,光致电化学信号随pH变化呈现先增大后减小的趋势。当pH小于7.4时,光致电化学信号随着pH的增加而增加,然而当pH大于7.4时,光致电化学信号却随着pH的增加而减小。当pH为7.4时,光致电化学信号值达到最大。所以选择检测介质的pH为7.4。
实施例2电位优化
制备的光致化学传感器可能会因为电极电位的不同来改变自身的电子传递系统,从而对光致电化学信号测定产生一定的影响。分别在-0.3V、-0.2V、-0.1V、0.0V、0.1V、0.2V、0.3V不同工作电位下测定光致电化学信号。图4为不同电位下的光致电化学信号响应。显而易见,纳米碳化钼修饰碳糊电极在电位为-0.1V时光致电化学信号最大,所以最终选择的电极电位为-0.1V。
实施例3纳米碳化钼用量的优化
用移液枪分别准确移取0μL、5μL、10μL、15μL、20μL、25μL的纳米碳化钼溶液滴涂在碳糊电极上,测定光致电化学信号。图5为不同纳米碳化钼用量情况下的光致电化学信号。可以看出,当纳米碳化钼用量在5μL-15μL之间时,光致电化学信号随着其的体积的增加而增加;而当纳米碳化钼用量大于15μL时,光致电化学信号反而降低,并在纳米碳化钼用量为15μL时,所得到的的分析信号值最大。所以选15μL为纳米碳化钼的最佳用量。
实施例4方法灵敏度
(1)纳米碳化钼的制备
取25mg碳化钼(MoC)与50mL N,N-二甲基甲酰胺于烧杯中,将小磁子放入烧杯中,然后用保鲜膜封住烧杯杯口,置于磁力搅拌器中搅拌30min,之后将小磁子取出,最后把用保鲜膜封好的小烧杯放入超声波清洗器中超声12h,得剥离的MoC。
(2)纳米碳化钼修饰碳糊电极的制备
吸取15μL纳米碳化钼溶液滴涂于刚处理过的碳糊电极的表面并将其铺展开,做好标记,置于泡沫板上使其自然干燥,得纳米碳化钼修饰碳糊电极光致电化学传感器。
考察了方法测定的灵敏度和线性范围等分析特性。在优选的条件下,目标物多巴胺的浓度在1.0×10-10M到1.0×10-5M范围内与光致电化学信号成线性函数关系式(图6)。线性函数关系式为:I/nA=570.7log(c/M)+6459.5(c是多巴胺的浓度,mol/L),其中R2=0.9901,相对标准偏差(RSD)为3.21%,检出限为3.0×10-11M。
实施例5方法的选择性
利用构建的传感器分别对多巴胺、甲硫氨酸、赖氨酸、苏氨酸、丝氨酸、精氨酸、亮氨酸、缬氨酸、异亮氨酸、脯氨酸、苯丙氨酸、谷氨酸、丙氨酸、半胱氨酸、胱氨酸进行考察,发现上述物质为1mM时对传感器的响应中,其中空白为325nA,多巴胺的信号为2978nA,其余的物质产生的信号在278nA和341nA之间。说明传感器对多巴胺具有选择性,可实现对多巴胺的选择性测定。即,只有多巴胺对光致电化学信号有明显的增强做作用,说明传感器对多巴胺具有选择性,可实现对多巴胺的选择性测定。
Claims (2)
1.纳米碳化钼修饰碳糊电极光致电化学传感器制备方法,包括如下步骤:
(1)纳米碳化钼的制备
取1mg~50mg碳化钼(MoC)与1mL~100mL N,N-二甲基甲酰胺于烧杯中,将小磁子放入烧杯中,然后用保鲜膜封住烧杯杯口,置于磁力搅拌器中搅拌1min~100min,之后将小磁子取出,最后把用保鲜膜封好的小烧杯放入超声波清洗器中超声0.1h-100h,得剥离的MoC;
(2)纳米碳化钼修饰碳糊电极的制备
吸取1μL~50μL纳米碳化钼溶液滴涂于刚处理过的碳糊电极的表面并将其铺展开,置于泡沫板上使其自然干燥,得纳米碳化钼修饰碳糊电极光致电化学传感器。
(3)一种利用上述方法制备的纳米碳化钼修饰碳糊电极光致电化学传感器检测多巴胺含量的方法,将光致电化学传感器插入含多巴胺的PBS溶液中时,得光致电化学信号I,以I为分析信号,进行多巴胺的测定;
由于上述方法制备的光致电化学传感器可以检测多巴胺,因此,本发明提供了光致电化学传感器在检测多巴胺含量中的应用。
2.根据权利要求1的纳米硒化锌修饰碳糊电极光致电化学传感器制备方法,其特征在于所述的纳米硒化锌修饰碳糊电极光致电化学传感器具有如下特性:
利用构建的传感器分别对多巴胺、甲硫氨酸、赖氨酸、苏氨酸、丝氨酸、精氨酸、亮氨酸、缬氨酸、异亮氨酸、脯氨酸、苯丙氨酸、谷氨酸、丙氨酸、半胱氨酸、胱氨酸进行考察,发现上述物质为1mM时对传感器的响应中,只有多巴胺对光致电化学信号有明显的增强做作用,说明传感器对多巴胺具有选择性,可实现对多巴胺的选择性测定。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010377333.1A CN111398390B (zh) | 2020-05-07 | 2020-05-07 | 纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010377333.1A CN111398390B (zh) | 2020-05-07 | 2020-05-07 | 纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111398390A true CN111398390A (zh) | 2020-07-10 |
CN111398390B CN111398390B (zh) | 2022-11-25 |
Family
ID=71431786
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010377333.1A Active CN111398390B (zh) | 2020-05-07 | 2020-05-07 | 纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111398390B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112924503A (zh) * | 2021-01-26 | 2021-06-08 | 青岛科技大学 | 一种光电流读出电位型传感器信号的方法 |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102176386A (zh) * | 2011-01-12 | 2011-09-07 | 南开大学 | 染料敏化太阳能电池对电极及其制备方法 |
CN102980929A (zh) * | 2012-12-06 | 2013-03-20 | 江南大学 | 用于高灵敏检测多巴胺的纳米光电化学传感器 |
CN105021672A (zh) * | 2015-06-23 | 2015-11-04 | 江南大学 | 基于原位氧化还原反应的光电化学方法检测多巴胺 |
CN108311167A (zh) * | 2018-03-21 | 2018-07-24 | 合肥工业大学 | 一种负载型碳化钼/金属纳米颗粒复合催化剂及其制备方法和催化降解重金属铬的应用 |
CN109813774A (zh) * | 2019-03-14 | 2019-05-28 | 青岛科技大学 | 一种光致电化学传感器检测瘦肉精雷托帕明的方法 |
CN109839416A (zh) * | 2019-03-12 | 2019-06-04 | 青岛科技大学 | 纳米二硒化钨修饰金电极光致电化学传感器检测多巴胺的方法 |
CN110803685A (zh) * | 2019-11-13 | 2020-02-18 | 南方科技大学 | 一种石墨化碳泡沫支撑碳材料/碳化钼复合材料及其制备方法和用途 |
-
2020
- 2020-05-07 CN CN202010377333.1A patent/CN111398390B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102176386A (zh) * | 2011-01-12 | 2011-09-07 | 南开大学 | 染料敏化太阳能电池对电极及其制备方法 |
CN102980929A (zh) * | 2012-12-06 | 2013-03-20 | 江南大学 | 用于高灵敏检测多巴胺的纳米光电化学传感器 |
CN105021672A (zh) * | 2015-06-23 | 2015-11-04 | 江南大学 | 基于原位氧化还原反应的光电化学方法检测多巴胺 |
CN108311167A (zh) * | 2018-03-21 | 2018-07-24 | 合肥工业大学 | 一种负载型碳化钼/金属纳米颗粒复合催化剂及其制备方法和催化降解重金属铬的应用 |
CN109839416A (zh) * | 2019-03-12 | 2019-06-04 | 青岛科技大学 | 纳米二硒化钨修饰金电极光致电化学传感器检测多巴胺的方法 |
CN109813774A (zh) * | 2019-03-14 | 2019-05-28 | 青岛科技大学 | 一种光致电化学传感器检测瘦肉精雷托帕明的方法 |
CN110803685A (zh) * | 2019-11-13 | 2020-02-18 | 南方科技大学 | 一种石墨化碳泡沫支撑碳材料/碳化钼复合材料及其制备方法和用途 |
Non-Patent Citations (4)
Title |
---|
KE LI 等: "A Molybdenum Carbide Nanotubes Modified Electrode as the Functionalized Sensing latform for Electrochemical Detection of Dopamine", 《ELECTROANALYSIS》 * |
XU HUN 等: ""A photoelectrochemical sensor for ultrasensitive dopamine detection based on single-layer NanoMoS2 modified gold electrode"", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
王会 等: "新型纳米碳/碳化钼的制备及应用研究", 《化工新型材料》 * |
高新: "纳米粒子、介孔碳复合材料修饰电极的制备及其在神经递质分子定量检测中的应用", 《中国优秀博硕论文全文数据库(硕士)医药卫生科技辑(月刊)》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112924503A (zh) * | 2021-01-26 | 2021-06-08 | 青岛科技大学 | 一种光电流读出电位型传感器信号的方法 |
Also Published As
Publication number | Publication date |
---|---|
CN111398390B (zh) | 2022-11-25 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Xu et al. | Preparation of multiwall carbon nanotubes film modified electrode and its application to simultaneous determination of oxidizable amino acids in ion chromatography | |
Poinsot et al. | Recent advances in amino acid analysis by capillary electrophoresis | |
Afkhami et al. | A new chiral electrochemical sensor for the enantioselective recognition of naproxen enantiomers using l-cysteine self-assembled over gold nanoparticles on a gold electrode | |
Liu et al. | Electrochemical behaviors and electrochemical determination of carbamazepine at ionic liquid modified carbon paste electrode in the presence of sodium dodecyl sulfate | |
Taei et al. | A voltammetric sensor for simultaneous determination of ascorbic acid, noradrenaline, acetaminophen and tryptophan | |
Babaei et al. | A new sensor for simultaneous determination of tyrosine and dopamine using iron (III) doped zeolite modified carbon paste electrode | |
Hendawy et al. | Nanomaterial-based carbon paste electrodes for voltammetric determination of naproxen in presence of its degradation products | |
Duarte et al. | A highly improved method for sensitive determination of amitriptyline in pharmaceutical formulations using an unmodified carbon nanotube electrode in the presence of sulfuric acid | |
Ghoreishi et al. | Electrochemical determination of tyrosine in the presence of uric acid at a carbon paste electrode modified with multi-walled carbon nanotubes enhanced by sodium dodecyl sulfate | |
CN111398390B (zh) | 纳米碳化钼修饰碳糊电极光致电化学传感器制备方法及应用 | |
Mohammadizadeh et al. | Carbon paste electrode modified with ZrO 2 nanoparticles and ionic liquid for sensing of dopamine in the presence of uric acid | |
Andrade et al. | A novel multicommutation stopped-flow system for the simultaneous determination of sulfamethoxazole and trimethoprim by differential pulse voltammetry on a boron-doped diamond electrode | |
Brahman et al. | Highly sensitive stripping voltammetric determination of a biomolecule, pyruvic acid in solubilized system and biological fluids | |
Chitravathi et al. | Electrochemical studies of sodium levothyroxine at surfactant modified carbon paste electrode | |
Narayana et al. | Development of Electrochemical sensor based on Poly (xylenol orange) film towards the determination of L-Dopa and its simultaneous resolution in the presence of Uric acid: A cyclic Voltammetric study | |
Xu et al. | Simultaneous determination of total homocysteine, cysteine and methionine in hypothyroid patients’ plasma by liquid chromatography using platinum/poly (methyl violet) modified electrode | |
CN109839416B (zh) | 纳米二硒化钨修饰金电极光致电化学传感器检测多巴胺的方法 | |
van Staden et al. | Enantioselective, potentiometric membrane electrodes based on cyclodextrins: Application for the determination of R-baclofen in its pharmaceutical formulation | |
Mohammadi et al. | Application of a modified carbon paste electrode using core–shell magnetic nanoparticle and modifier for simultaneous determination of norepinephrine, acetaminophen and tryptophan | |
CN111426729B (zh) | 纳米硒化锌修饰金电极光致电化学传感器制备方法及应用 | |
Zeng et al. | Voltammetric determination of epinephrine with a 3‐mercaptopropionic acid self‐assembled monolayer modified gold electrode | |
CN110031526A (zh) | 一种基于K2Fe4O7电极的多巴胺无酶传感器、制备方法及其应用 | |
Liu et al. | Improved Voltammetric Response of L‐Tyrosine on Multiwalled Carbon Nanotubes‐Ionic Liquid Composite Coated Glassy Electrodes in the Presence of Cupric Ion | |
CN113295749B (zh) | 氮掺杂石墨烯/离子液体复合材料修饰玻碳电极、其制备方法及肾上腺素定量检测方法 | |
Liu et al. | A highly sensitive sensor for synephrine detection based on multi-walled carbon nanotubes modified glass carbon electrodes |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |