Electrochemical probe and synthesis method thereof
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A synthetic method and electrochemical technology, applied in the fields of biomedicine and life sciences, to achieve the effects of good stability, good selectivity, and simple structure
Inactive Publication Date: 2014-07-30
QINGDAO UNIV OF SCI & TECH
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The electrochemical probe proposed by the present invention is used for the electrochemical detection of thiol compounds, which effectively overcomes the shortcomings of the prior art such as complicated and cumbersome operations, without the need for electrode modification and sample derivation treatment, and realizes high selectivity, high sensitivity, Convenient, low-cost rapid detection
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Embodiment 1
[0027] Embodiment 1: the synthetic steps of electrochemical probe:
[0028] a. Add 3.5g of o-phenylenediamine, 13.0g of potassium thiocyanate, and 200mL of methanol into the container, and add bromine solution in methanol under the condition of a dry-ice acetone low-temperature bath. After the reaction is completed, stir at room temperature for 1.5h, suction filter, and filter Pour into 400mL of water, add 25mL of ammonia water to the filtrate after suction filtration, suction filtration, washing with water, and drying to obtain a yellow intermediate (I): 4,5-bis(isothiocyanato)-1,2-o-phenylenediamine , its structural formula is as follows:
[0029]
[0030] The methanol solution of bromine is 3mLBr 2 Dissolve in 50mL methanol.
[0031] b. Weigh 3.0g of the above intermediate (I) and 5.5g of sodium sulfide, add 150mL of water, heat in an oil bath at 70°C for 0.5h, add 1.5mL of carbon disulfide in an ice-water bath, after the reaction is complete, heat in an oil bath at 50...
Embodiment 2
[0045] Embodiment 2: the electrochemical performance of electrochemical probe
[0046] Instruments and reagents
[0047] CHI832B electrochemical analyzer (Shanghai Chenhua Instrument Factory); all electrochemical experiments used a three-electrode system, with platinum wire as the auxiliary electrode, Ag / AgCl (saturated KCl) electrode as the reference electrode, and a bare gold electrode as the working electrode ( Diameter: 2.0mm). Differential pulse voltammetry experiments were performed in conventional electrochemical cells at room temperature. The pH value of the solution was detected with a PHS-3DpH acidity meter (compound saturated calomel electrode, Shanghai Leici Instrument Factory).
[0048] Preparation of GSH solution: Accurately weigh 3.07mgGSH in a beaker, dissolve it with a small amount of water, transfer it to a 10mL volumetric flask, and dilute with secondary water to obtain 1.0×10 -3 MGSH solution.
[0049] Preparation of electrochemical probe solution: Accu...
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Abstract
The invention provides an electrochemical probe used for detecting biological active sulfhydryl matters and a synthesis method of the electrochemical probe. The invention provides a new electrochemical probe by fusing tetrathiafulvalene (TTF) group and a group with sulfhydryl reaction activity for the first time, and the name of the electrochemical probe is 2-[4,5-bis(propylsulfalkyl)]-1,3-dithiole-2-ylidene][1,3]dithiolo(4,5-f)-2,1,3-benzoselenadiazole. The probe has the characteristics that the molecular structure of the probe simultaneously contains a flexible sulfhydryl reaction activity group and the TTF group, and thus the probe not only has sensitive electrochemical signals, but also the probe and sulfhydryl matters are subjected to specific reaction. Therefore, the high-sensitivity and high-selectivity detection on the sulfhydryl matters can be realized by utilizing the probe. The electrochemical probe can provide a new approach and means for the further application of electroanalytical chemistry in life sciences of biology, clinical medicines, early-stage diagnosis and treatment of cancers, and the like.
Description
technical field [0001] The invention belongs to the fields of biomedicine and life sciences, and in particular relates to an electrochemical probe for detecting thiols and a synthesis method thereof. Background technique [0002] Biologically active sulfhydryl compounds widely exist in various tissues, cells and body fluids in vivo, such as L-cysteine (L-Cys), homocysteine (Hcy) and glutathione, etc., which serve as Important antioxidant substances in the body can participate in a variety of biochemical reactions and play an important role in the regulation of cell growth and function. Reduced glutathione (GSH) is the most abundant non-protein sulfhydryl compound in animal and plant cells. Since it was first discovered in 1921, its content in human tissues and cells and its relationship with various diseases have been widely discussed. Attention has been extensively studied. Studies have shown that changes in the concentration of glutathione and related sulfhydryl comp...
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