CN105334248B - A method of making an electrochemical sensor for the detection of homocysteine - Google Patents

A method of making an electrochemical sensor for the detection of homocysteine Download PDF

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CN105334248B
CN105334248B CN201510802844.2A CN201510802844A CN105334248B CN 105334248 B CN105334248 B CN 105334248B CN 201510802844 A CN201510802844 A CN 201510802844A CN 105334248 B CN105334248 B CN 105334248B
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electrode
conductive polymer
electrochemical sensor
homocysteine
modified
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CN105334248A (en
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何丹农
王丹
张春明
吴晓燕
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上海纳米技术及应用国家工程研究中心有限公司
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Abstract

本发名提供一种用于同型半胱氨酸检测的电化学传感器的制备方法,包括导电聚合物修饰电极的制备和聚甲基紫修饰的导电聚合物电化学传感器的制备,将导电聚合物修饰电极置于含有8×10‑5mol/L甲基紫的磷酸缓冲溶液中,在+1.6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水乙醇和二次蒸馏水依次轮流冲洗若干次,得到聚甲基紫修饰的导电聚合物电化学传感器。 The name of the present provides a method for preparing an electrochemical sensor for detecting homocysteine, comprising a conductive polymer electrode Preparation and polymethylmethacrylate Violet conductive polymer modified electrochemical sensors, conductive polymers modified electrode is placed a phosphate buffer solution containing 8 × 10-5mol / L methyl violet, the lower electrodeposition +1.6 V for five minutes, then removed after the conductive polymer modified scan electrode, using double distilled water and ethanol sequentially rinsed several turns, give polymethacrylic violet conductive polymer electrochemical sensor. 该传感器制备方法简单,灵敏度高。 The sensor preparation method is simple, a high sensitivity.

Description

一种用于同型半胱氨酸检测的电化学传感器的制备方法 A method of making an electrochemical sensor for the detection of homocysteine

技术领域 FIELD

[0001] 本发明涉及一种电化学传感器,具体是一种用于同型半胱氨酸快速检测的电化学传感器制备方法。 [0001] The present invention relates to an electrochemical sensor, in particular a method of preparing an electrochemical sensor homocysteine ​​rapid detection.

背景技术 Background technique

[0002] 同型半胱氨酸亦称高半胱氨酸,是一种含巯基的氨基酸,近年来,医学研究已经证实血浆中同型半胱氨酸的含量变化与冠心病和脑血管疾病发病率的提高有着密切的联系。 [0002] Also known homocysteine ​​Homocysteine ​​is an amino acid containing a thiol group, in recent years, medical studies have demonstrated changes in plasma levels of homocysteine ​​and the incidence of coronary heart disease and cerebrovascular disease the increase is closely linked. 因此,检测同型半胱氨酸的水平对的相关疾病的病理研究具有重要意义。 Therefore, pathological studies related diseases detectable level of homocysteine ​​is of great significance.

[0003] 目前已建立了多种分析方法用于同型半胱氨酸的检测,如光度检测法,紫外分光光度法,荧光法,光谱测定法,电化学检测法和酶免疫测定法等。 [0003] It has been established to detect various analytical methods for homocysteine, as photometric detection, UV spectrophotometry, fluorescence, spectrometry, electrochemical detection method and the enzyme immunoassay method or the like. 但是上述很多方法存在着预处理复杂、成本高、灵敏度低等缺点。 However, there are many ways the above pretreatment complexity, high cost, low sensitivity disadvantages. 因此对同型半胱氨酸进行及时、准确、灵敏的检测, 成为亟待解决的迫切问题。 Therefore homocysteine ​​timely, accurate and sensitive detection is an urgent problem to be solved.

发明内容 SUMMARY

[0004]本发明的目的是针对现有技术存在的上述不足,提供一种快速、灵敏、简便的同型半胱氨酸检测的电化学传感器。 [0004] The object of the present invention is directed to the above-described disadvantages of the prior art, provides a fast, sensitive and simple electrochemical sensor homocysteine ​​detection. 本传感器是基于材料对电化学检测信号的放大作用,构建了新型复合材料修饰的电化学传感器。 This sensor is based on electrochemical detection signal amplification of the material to construct a new composite modified electrochemical sensor.

[0005]本发明涉及用于同型半胱氨酸检测的电化学传感器的制备方法,包括以下步骤: [0006]第一步:导电聚合物修饰电极的制备: [0005] The present invention relates to a method of preparing an electrochemical sensor for detecting homocysteine, comprising the steps of: [0006] First Step: Preparation of conducting polymer modified electrode:

[0007]首先将玻碳电极进行抛光处理后在二次蒸馏水中超声清洗;然后清洗后的玻碳电极放入M聚合物单体、M水溶性醌类磺酸盐和氧化石墨烯溶液中,通氮气30分钟后,采用三电极体系进行恒电流电沉积,然后将所得修饰电极进行电化学还原,获得导电聚合物/醌类磺化物/氧化石墨烯复合材料修饰电极。 After [0007] First, the polished glassy carbon electrode in a secondary distilled water ultrasonic cleaning; glassy carbon electrode was then cleaned polymer into monomers M, M sulfonates and water-soluble quinones graphene oxide solution, after 30 minutes, nitrogen, three-electrode system using a constant current electrodeposition, and the resulting modified electrode for electrochemical reduction, to obtain the conductive polymer / quinone sulfonate / graphene oxide composite modified electrode.

[0008]第二步:聚甲基紫修饰的导电聚合物电化学传感器的制备: [0008] Second Step: Preparation of poly methyl violet conducting polymer-modified electrochemical sensor:

[0009]将导电聚合物修饰电极置于含有8Xl(T5m〇l/L甲基紫的磷酸缓冲溶液中,在+1.6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水乙醇和二次蒸馏水依次轮流冲洗若干次,得到聚甲基紫修饰的导电聚合物电化学传感器。 [0009] The conducting polymer comprising modified electrode was placed 8XL (T5m〇l / L phosphate buffer solution of methyl violet, the electrodeposition at +1.6 V for five minutes and then taken out through the conductive polymer modified scanning electrodes, with double distilled water and ethanol in turn sequentially rinsed several times to obtain poly-violet conductive polymer electrochemical sensor.

[0010]所述醌类磺酸盐为蒽醌或菲醌的一种。 The [0010] quinone is anthraquinone sulfonate or phenanthrenequinone.

[0011 ]所述M聚合物单体为吡咯、苯胺、3,4-乙烯二氧噻吩中的一种。 [0011] The polymerizable monomers M pyrrole, aniline, 3,4-ethylene dioxythiophene of one. 具体实施例 Specific Example

[0012]实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。 [0012] In embodiments of the present invention is a technical premise, given the specific operation and detailed embodiments, but the scope of the present invention is not limited to the following examples.

[0013] 实施例1: [0013] Example 1:

[00M]将预处理好的玻碳电极放入PH=7.0的磷酸缓冲溶液中,以20 mV/s的扫描速率在-0.2V〜+ 2.0V的电位范围内进行循环扫描处理1〇min。 [00M] will be placed in the pretreated glassy carbon electrode PH = 7.0 phosphate buffer solution, at a scan rate of 20 mV / s scan 1〇min is circulated within the potential range of -0.2V~ + 2.0V.

[0015] 然后将电极放入含有0_1 M的吡咯单体、0.0005 M菲醒磺酸盐、0•5 mg/ml氧化石墨烯水溶液,通N2 30min后,采用三电极体系进行恒电流电沉积,施加电流为0.5 mA cnf2, 电沉积的电量为1.2库伦;将所得到的聚吡咯膜洗净后在放置在三电极体系中进行电化学还原,施加电压为1.1 V,电解液为F>BS缓冲溶液,反应后用水反复清洗即可得到聚吡咯/菲醌磺酸盐/石墨烯复合材料修饰电极; [0015] The electrode was then placed into a container of a pyrrole monomer 0_1 M, 0.0005 M phenanthrene wake sulfonates, 0 • 5 mg / ml aqueous solution of graphene oxide, the through-N2 30min, three-electrode system using a constant current electrodeposition, applying a current of 0.5 mA cnf2, electrodeposition of electricity was 1.2 coulombs; polypyrrole film obtained after washing is placed in a three-electrode system for the electrochemical reduction, the applied voltage is 1.1 V, the electrolytic solution is F> BS buffer solution, washed repeatedly with water after the reaction to obtain polypyrrole / phenanthrene quinone sulfonate / graphene composite material modified electrode;

[0016]将上述导电聚合物修饰电极置于含有8X10-5mol/L甲基紫的磷酸缓冲溶液中,在+ 1.6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水乙醇和二次蒸馏水依次轮流冲洗若干次,得到聚甲基紫修饰的导电聚合物电化学传感器。 [0016] The above conductive polymer modified electrode in a phosphate buffer solution containing 8X10-5mol / L methyl violet, the electrodeposition at + 1.6 V for five minutes, then removed after the conductive polymer modified scanning electrodes, with no double distilled water and ethanol, rinsed several times successively in turn, give polymethacrylic violet conductive polymer electrochemical sensor.

[0017] 实施例2: [0017] Example 2:

[0018] 将预处理好的玻碳电极放入pH=5.0的磷酸盐缓冲溶液中,以15 mV/s的扫描速率在-0.2V〜+ 1.0V的电位范围内进行循环扫描处理15min; [0018] The glassy carbon electrode in the pretreated phosphate buffer solution pH = 5.0, at a scan rate of 15 mV / s scan process is circulated within 15min -0.2V~ + 1.0V potential range of;

[0019] 然后将电极放入含有0.2 M的吡咯单体、0.0005 M蒽醌磺酸盐、1.0 mg/ml氧化石墨烯水溶液,通N2 3〇min后,采用三电极体系进行恒电流电沉积,施加电流为2 mA cnf2, 电沉积的电量为2.0库伦;将所得到的聚吡咯膜洗净后在放置在三电极体系中进行电化学还原,施加电压为I.2 V,电解液为PBS缓冲溶液,反应后用水反复清洗即可得到聚吡咯/蒽醌磺酸盐/石墨烯复合材料修饰电极; [0019] The electrode was then placed into a monomer containing 0.2 M of pyrrole, 0.0005 M anthraquinone sulfonate, 1.0 mg / ml aqueous solution of graphene oxide, the N2 3〇min pass, three-electrode system using a constant current electrodeposition, applying a current of 2 mA cnf2, electrodeposition is 2.0 coulomb of electricity; polypyrrole film after washing the resulting three-electrode system placed in the electrochemical reduction is carried out, the applied voltage is I.2 V, the electrolytic solution is a PBS buffer solution, washed repeatedly with water after the reaction to obtain polypyrrole / anthraquinone sulfonate / graphene composite material modified electrode;

[0020] 将上述导电聚合物修饰电极置于含有SXl(T5m〇l/L甲基紫的磷酸缓冲溶液中,在+ 1.6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水己醇和二次蒸馏水依次轮流冲洗若干次,得到聚甲基紫修饰的导电聚合物电化学传感器。 [0020] The above conductive polymer modified electrode in a solution containing phosphate buffer SXL (T5m〇l / L of methyl violet, at + 1.6 V electrodeposition five minutes, then removed after the conductive polymer modified scanning electrodes, dried over anhydrous hexanol bidistilled water rinsed several times successively in turn, give polymethacrylic violet conductive polymer electrochemical sensor.

[0021] 实施例3: [0021] Example 3:

[0022] 将预处理好的玻碳电极放入PH=7.0的磷酸盐缓冲溶液中,以20 mV/s的扫描速率在-0.2V〜+ 2.0V的电位范围内进行循环扫描处理50min; [0022] will be placed in the pretreated glassy carbon electrode PH = 7.0 phosphate buffer solution, at a scan rate of 20 mV / s scan process is circulated within 50min -0.2V~ + 2.0V potential range of;

[0023]然后将电极放入含有含0_05 M的苯胺单体、0.1 M菲醌磺酸盐、1.0 mg/ml氧化石墨烯水溶液,通Ns 30min后,采用三电极体系进行恒电流电沉积,施加电流为ig cnf2, 电沉积的电量为1.6库伦;将所得到的聚苯胺膜洗净后在放置在三电极体系中进行电化学还原,施加电压为1.0 V,电解液为PBS缓冲溶液,反应后用水反复清洗即可得到聚苯胺/菲醌磺酸盐/石墨烯复合材料修饰电极; [0023] The electrode was then placed into a container containing aniline monomers 0_05 M, 0.1 M phenanthrenequinone salts, 1.0 mg / ml aqueous solution of graphene oxide, Ns pass after 30min, three-electrode system using a constant current electrodeposition, applied current ig cnf2, electrodeposition of electricity was 1.6 coulombs; polyaniline film after washing the resulting three-electrode system placed in the electrochemical reduction is carried out, the applied voltage is 1.0 V, the electrolytic solution is a PBS buffer solution, after the reaction repeatedly washed with water to obtain a polyaniline / phenanthrene quinone sulfonate / graphene composite material modified electrode;

[0024]将上述导电聚合物修饰电极置于含有8X10-5mol/L甲基紫的磷酸缓冲溶液中,在+ 1.6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水乙醇和二次蒸馏水依次轮流冲洗若干次,得到聚甲基紫修饰的导电聚合物电化学传感器。 [0024] The above conductive polymer modified electrode in a phosphate buffer solution containing 8X10-5mol / L methyl violet, the electrodeposition at + 1.6 V for five minutes, then removed after the conductive polymer modified scanning electrodes, with no double distilled water and ethanol, rinsed several times successively in turn, give polymethacrylic violet conductive polymer electrochemical sensor.

Claims (3)

  1. 取1. 一种用于同型半胱氨酸检测的电化学传感器的制备方法,其特征在于,包括以下步骤: 第一步:导电聚合物修饰电极的制备: 首先将玻碳电极进行抛光处理后在二次蒸馏水中超声清洗;然后清洗后的玻碳电极放入M聚合物单体、水溶性醌类磺酸盐和氧化石墨烯溶液中,通氮气3〇分钟后,采用三电极体系进行恒电流电沉积,然后将所得修饰电极进行电化学还原,获得导电聚合物/醌类磺化物/石墨烯复合材料修饰电极; ' 第二步:聚甲基紫修饰的导电聚合物电化学传感器的制备: 将导电聚合物修饰电极置于含有8 X l(T5m〇l/L甲基紫的磷酸缓冲溶液中,在+1 • 6 V下电沉积五分钟,然后取出经过扫描的导电聚合物修饰电极,用无水乙醇和二次蒸馏水依次轮流冲洗若千次,得到聚甲基紫修饰的导电聚合物电化学传感器。 Take 1. A method for preparing an electrochemical sensor for the detection of homocysteine, which is characterized in that it comprises the following steps: First Step: Preparation of conducting polymer modified electrode: glassy carbon electrode is first polished after in the secondary distilled water ultrasonic cleaning; glassy carbon electrode was then cleaned polymer into monomers M, water-soluble quinones graphene oxide salt solution and, after nitrogen 3〇 minutes, using a three-electrode system for constant preparation of poly methyl violet conductive polymer electrochemical sensors: 'the second step; current electrodeposition, and the resulting modified electrode for electrochemical reduction, to obtain the conductive polymer / quinone sulfonate / graphene composite electrode modified : the conductive polymer modified electrode in a phosphate buffer solution containing 8 X l (T5m〇l / L methyl violet, the electrodeposition at +1 • 6 V for five minutes, then removed after the conductive polymer modified scan electrode , with ethanol and doubly distilled water rinse, if CPM their turn, give polymethacrylic violet conductive polymer electrochemical sensor.
  2. 2.根据权利要求1所述一种用于同型半胱氨酸检测的电化学传感器的制备方法,其特征在于,所述醌类磺酸盐为蒽醌或菲醌磺酸盐中的一种。 2. The method of claim 1 prepared electrochemical sensor for the detection of homocysteine ​​claim, wherein the quinone is anthraquinone sulfonate or sulfonate phenanthrenequinone .
  3. 3.根据权利要求1所述一种用于同型半胱氨酸检测的电化学传感器的制备方法,其特征在于,所述M聚合物单体为吡咯、苯胺、3,4-乙烯二氧噻吩中的一种。 3. The method of claim 1 prepared electrochemical sensor for the detection of homocysteine ​​claim, wherein said polymer of a monomer M pyrrole, aniline, 3,4-ethylene dioxythiophene in kind.
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