CN104849329A - Resveratrol measuring method by multi-wall carbon nanotube modified electrode - Google Patents
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Abstract
本发明公开了一种多壁碳纳米管修饰电极测白藜芦醇的方法，首先制备多壁碳纳米管修饰电极，然后用所述多壁碳纳米管修饰电极为工作电极，旋状铂丝电极为对电极，Ag/AgCl(3mol/L KCl)电极为参比电极，伏安法测定-0.36V处白藜芦醇的氧化峰电流，定量计算白藜芦醇。本发明的多壁碳纳米管修饰电极测白藜芦醇的方法，方法简单，多壁碳纳米管修饰电极制备方便，可多次反复使用，检测速度快，准确率高。
The invention discloses a method for measuring resveratrol with a multi-walled carbon nanotube modified electrode. Firstly, the multi-walled carbon nanotube modified electrode is prepared, and then the multi-walled carbon nanotube modified electrode is used as a working electrode. The electrode is the counter electrode, and the Ag/AgCl (3mol/L KCl) electrode is the reference electrode. The oxidation peak current of resveratrol at -0.36V is measured by voltammetry, and the resveratrol is quantitatively calculated. The method for measuring resveratrol by the multi-wall carbon nanotube modified electrode of the present invention is simple, the multi-wall carbon nanotube modified electrode is convenient to prepare, can be used repeatedly, has fast detection speed and high accuracy.
Description
技术领域technical field
本发明属于电化学检测领域，具体涉及一种多壁碳纳米管修饰电极测白藜芦醇的方法。The invention belongs to the field of electrochemical detection, and in particular relates to a method for measuring resveratrol by a multi-walled carbon nanotube modified electrode.
背景技术Background technique
白藜芦醇是多酚类化合物，主要来源于葡萄、虎杖、花生、桑椹等植物。白藜芦醇是一种生物活性很强的天然多酚类物质，又称为芪三酚，是肿瘤的化学预防剂，也是对降低血小板聚集，预防和治疗动脉粥样硬化、心脑血管疾病的化学预防剂。美国农业部的研究结果表明，花生红衣与仁中也含有相当多的白藜芦醇。白藜芦醇的实验研究已经证实具有对心血管疾病和癌症的有益作用。白藜芦醇对激素依赖性肿瘤有明显的预防作用。还可对骨质疏松、痤疮及老年痴呆症有预防作用，具有抗病毒及免疫调节作用。对人体内部一种单体抗衰老酶起作用，进而发挥预防各种年龄相关疾病、延长预期寿命的潜在作用。Resveratrol is a polyphenolic compound, mainly derived from grapes, knotweed, peanuts, mulberries and other plants. Resveratrol is a natural polyphenolic substance with strong biological activity, also known as stilbene triphenols, it is a chemopreventive agent for tumors, and it is also effective in reducing platelet aggregation, preventing and treating atherosclerosis, cardiovascular and cerebrovascular diseases. chemopreventive agents. The research results of the US Department of Agriculture show that the red coat and kernel of peanuts also contain quite a lot of resveratrol. Experimental studies of resveratrol have demonstrated beneficial effects on cardiovascular disease and cancer. Resveratrol has obvious preventive effect on hormone-dependent tumors. It can also prevent osteoporosis, acne and Alzheimer's disease, and has antiviral and immune regulation effects. It acts on a monomeric anti-aging enzyme in the human body, thereby playing a potential role in preventing various age-related diseases and prolonging life expectancy.
碳纳米管是继C60之后发现的碳的又一同素异形体，其径向尺寸较小，管的外径一般在几纳米到几十纳米，管的内径更小，有的只有1nm左右；而其长度一般在微米级，长度和直径比非常大，可达103～106。因此，碳纳米管被认为是一种典型的一维纳米材料。碳纳米管自从被人类发现以来，就一直被誉为未来的材料，是近年来国际科学的前沿领域之一。Carbon nanotubes are another allotrope of carbon discovered after C60, and their radial dimensions are small. The outer diameter of the tube is generally several nanometers to tens of nanometers, and the inner diameter of the tube is even smaller, some of which are only about 1nm; Its length is generally in the order of microns, and the ratio of length to diameter is very large, up to 103-106. Therefore, carbon nanotubes are considered as a typical one-dimensional nanomaterial. Carbon nanotubes have been hailed as future materials since they were discovered by humans, and they are one of the frontier fields of international science in recent years.
碳纳米管经过适当处理后制成的修饰电极,表现出十分稳定的电化学作用。目前对白藜芦醇的测定方法主要是高效液相色谱法、气相色谱、质谱法、毛细管电泳法、二次微分简易示波伏安法等。但这些方法要么重现性欠佳，需要昂贵的设备，要么检测灵敏度太低。而通过电化学方法采用化学修饰电极检测白藜芦醇是较好的途径。本文利用多层碳纳米管电极选择性测定白藜芦醇，结果令人满意。The modified electrode made of carbon nanotubes after proper treatment shows a very stable electrochemical effect. At present, the methods for the determination of resveratrol mainly include high performance liquid chromatography, gas chromatography, mass spectrometry, capillary electrophoresis, and simple secondary differential oscillometric voltammetry. However, these methods either have poor reproducibility, require expensive equipment, or have low detection sensitivity. It is a better way to detect resveratrol by electrochemical method using chemically modified electrodes. In this paper, the selective determination of resveratrol by multilayer carbon nanotube electrode is satisfactory.
发明内容Contents of the invention
本发明的目的在于，提供一种多壁碳纳米管修饰电极测白藜芦醇的方法。The object of the present invention is to provide a method for measuring resveratrol with a multi-walled carbon nanotube modified electrode.
本发明提供一种多壁碳纳米管修饰电极测白藜芦醇的方法，包括以下步骤：The invention provides a method for measuring resveratrol with a multi-walled carbon nanotube modified electrode, comprising the following steps:
将玻碳电极首先用金相砂纸打磨，再依次用0.05μm的氧化铝粉在平板玻璃上抛光至镜面光滑，每次抛光后均用二次蒸馏水冲洗，再分别于无水乙醇和二次蒸馏水中超声洗涤5min，得到处理过的玻碳电极；The glassy carbon electrode was first polished with metallographic sandpaper, and then polished on flat glass with 0.05 μm alumina powder in turn until the mirror surface was smooth. Ultrasonic washing in medium for 5 minutes to obtain the treated glassy carbon electrode;
将单壁碳纳米管用研钵粉碎，加入浓盐酸超声分散并除去其中金属催化剂，清洗至中性，加入浓HNO3，140℃回流5h，冷却至室温后，洗至近中性，置于烘箱中120℃干燥后，得到多壁碳纳米管；Crush single-walled carbon nanotubes with a mortar, add concentrated hydrochloric acid to ultrasonically disperse and remove the metal catalyst, wash until neutral, add concentrated HNO 3 , reflux at 140°C for 5 hours, cool to room temperature, wash until nearly neutral, and place in an oven After drying at 120°C, multi-walled carbon nanotubes were obtained;
称取上述多壁碳纳米管1mg加入10ml DMF，超声5分钟，形成黑色悬浮液；Weigh 1 mg of the above multi-walled carbon nanotubes, add 10 ml DMF, and ultrasonicate for 5 minutes to form a black suspension;
取20μL所述黑色悬浮液，滴至所述处理过的玻碳电极表面，红外灯下干燥，得到多壁碳纳米管修饰电极；Take 20 μL of the black suspension, drop it on the surface of the treated glassy carbon electrode, and dry it under an infrared lamp to obtain a multi-walled carbon nanotube modified electrode;
用所述多壁碳纳米管修饰电极为工作电极，旋状铂丝电极为对电极，Ag/AgCl(3mol/L KCl)电极为参比电极，取pH2.0的Britton-Robinson缓冲溶液于10.0mL的电解池中，通入氮气除氧10min，在0～0.8V用循环伏安法活化电极直到循环伏安曲线稳定，然后加入白藜芦醇待测液，氮气保护条件下以100mV/s的扫速，记录0～0.8V的循环伏安曲线，测定-0.36V处的氧化峰电流，用于白藜芦醇的定量分析。Use described multi-walled carbon nanotube modified electrode as working electrode, spiral platinum wire electrode as counter electrode, Ag/AgCl (3mol/L KCl) electrode as reference electrode, get the Britton-Robinson buffer solution of pH2.0 at 10.0 In the electrolytic cell of mL, pass nitrogen gas to deoxygenate for 10 minutes, activate the electrode by cyclic voltammetry at 0-0.8V until the cyclic voltammetry curve is stable, then add resveratrol to be tested, and use 100mV/s under the condition of nitrogen protection. The sweep speed was recorded, the cyclic voltammetry curve of 0-0.8V was recorded, and the oxidation peak current at -0.36V was measured, which was used for the quantitative analysis of resveratrol.
本发明的有益效果在于：本发明的多壁碳纳米管修饰电极测白藜芦醇的方法，方法简单，多壁碳纳米管修饰电极制备方便，可多次反复使用，检测速度快，准确率高。The beneficial effects of the present invention are: the method for measuring resveratrol by the multi-walled carbon nanotube modified electrode of the present invention is simple, the multi-walled carbon nanotube modified electrode is convenient to prepare, can be used repeatedly, and has fast detection speed and high accuracy. high.
附图说明Description of drawings
图1所示为本发明多壁碳纳米管修饰电极测白藜芦醇的方法的检测伏安图。Fig. 1 shows the detection voltammogram of the method for measuring resveratrol by the multi-walled carbon nanotube modified electrode of the present invention.
具体实施方式Detailed ways
下文将结合具体附图详细描述本发明具体实施例。应当注意的是，下述实施例中描述的技术特征或者技术特征的组合不应当被认为是孤立的，它们可以被相互组合从而达到更好的技术效果。Specific embodiments of the present invention will be described in detail below in conjunction with specific drawings. It should be noted that the technical features or combinations of technical features described in the following embodiments should not be regarded as isolated, and they can be combined with each other to achieve better technical effects.
本发明提供一种多壁碳纳米管修饰电极测白藜芦醇的方法，包括以下步骤：The invention provides a method for measuring resveratrol with a multi-walled carbon nanotube modified electrode, comprising the following steps:
将玻碳电极首先用金相砂纸打磨，再依次用0.05μm的氧化铝粉在平板玻璃上抛光至镜面光滑，每次抛光后均用二次蒸馏水冲洗，再分别于无水乙醇和二次蒸馏水中超声洗涤5min，得到处理过的玻碳电极；The glassy carbon electrode was first polished with metallographic sandpaper, and then polished on flat glass with 0.05 μm alumina powder in turn until the mirror surface was smooth. Ultrasonic washing in medium for 5 minutes to obtain the treated glassy carbon electrode;
将单壁碳纳米管用研钵粉碎，加入浓盐酸超声分散并除去其中金属催化剂，清洗至中性，加入浓HNO3，140℃回流5h，冷却至室温后，洗至近中性，置于烘箱中120℃干燥后，得到多壁碳纳米管；Crush single-walled carbon nanotubes with a mortar, add concentrated hydrochloric acid to ultrasonically disperse and remove the metal catalyst, wash until neutral, add concentrated HNO 3 , reflux at 140°C for 5 hours, cool to room temperature, wash until nearly neutral, and place in an oven After drying at 120°C, multi-walled carbon nanotubes were obtained;
称取上述多壁碳纳米管1mg加入10ml DMF，超声5分钟，形成黑色悬浮液；Weigh 1 mg of the above multi-walled carbon nanotubes, add 10 ml DMF, and ultrasonicate for 5 minutes to form a black suspension;
取20μL所述黑色悬浮液，滴至所述处理过的玻碳电极表面，红外灯下干燥，得到多壁碳纳米管修饰电极；Take 20 μL of the black suspension, drop it on the surface of the treated glassy carbon electrode, and dry it under an infrared lamp to obtain a multi-walled carbon nanotube modified electrode;
用所述多壁碳纳米管修饰电极为工作电极，旋状铂丝电极为对电极，Ag/AgCl(3mol/L KCl)电极为参比电极，取pH2.0的Britton-Robinson缓冲溶液于10.0mL的电解池中，通入氮气除氧10min，在0～0.8V用循环伏安法活化电极直到循环伏安曲线稳定，然后加入白藜芦醇待测液，氮气保护条件下以100mV/s的扫速，记录0～0.8V的循环伏安曲线，测定-0.36V处的氧化峰电流，用于白藜芦醇的定量分析。Use described multi-walled carbon nanotube modified electrode as working electrode, spiral platinum wire electrode as counter electrode, Ag/AgCl (3mol/L KCl) electrode as reference electrode, get the Britton-Robinson buffer solution of pH2.0 at 10.0 In the electrolytic cell of mL, pass nitrogen gas to deoxygenate for 10 minutes, activate the electrode by cyclic voltammetry at 0-0.8V until the cyclic voltammetry curve is stable, then add resveratrol to be tested, and use 100mV/s under the condition of nitrogen protection. The sweep speed was recorded, the cyclic voltammetry curve of 0-0.8V was recorded, and the oxidation peak current at -0.36V was measured, which was used for the quantitative analysis of resveratrol.
图1所示为本发明多壁碳纳米管修饰电极测白藜芦醇的方法的检测伏安图，测量结果如图1所示。Fig. 1 shows the detection voltammogram of the method for measuring resveratrol by a multi-walled carbon nanotube modified electrode of the present invention, and the measurement results are shown in Fig. 1 .
本发明的多壁碳纳米管修饰电极测白藜芦醇的方法，方法简单，多壁碳纳米管修饰电极制备方便，可多次反复使用，检测速度快，准确率高。The method for measuring resveratrol by the multi-walled carbon nanotube modified electrode of the present invention is simple, the multi-walled carbon nanotube modified electrode is convenient to prepare, can be used repeatedly, has high detection speed and high accuracy.
本文虽然已经给出了本发明的一些实施例，但是本领域的技术人员应当理解，在不脱离本发明精神的情况下，可以对本文的实施例进行改变。上述实施例只是示例性的，不应以本文的实施例作为本发明权利范围的限定。Although some embodiments of the present invention have been given herein, those skilled in the art should understand that the embodiments herein can be changed without departing from the spirit of the present invention. The above-mentioned embodiments are only exemplary, and the embodiments herein should not be used as limitations on the scope of rights of the present invention.
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| CN105572209A (en) * | 2015-12-23 | 2016-05-11 | 湖北民族学院 | Method utilizing liquid phase to strip graphene modified electrode to measure content of resveratrol |
| CN107144612A (en) * | 2017-04-20 | 2017-09-08 | 信阳师范学院 | Carbendazim detection method |
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| US20080105544A1 (en) * | 2003-12-15 | 2008-05-08 | Fuji Xerox Co., Ltd. | Electrode for electrochemical measurement |
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| CN105572209A (en) * | 2015-12-23 | 2016-05-11 | 湖北民族学院 | Method utilizing liquid phase to strip graphene modified electrode to measure content of resveratrol |
| CN105572209B (en) * | 2015-12-23 | 2018-04-03 | 湖北民族学院 | The method that graphene modified determination of electrode Resveratrol content is peeled off using liquid phase |
| CN107144612A (en) * | 2017-04-20 | 2017-09-08 | 信阳师范学院 | Carbendazim detection method |
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