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Method for manufacturing novel dendritic fluorescent chemosensor and application

A chemical sensor and dendritic technology, applied in the field of analysis and testing, can solve the problems of high price of synthetic raw materials, unsatisfactory sensitivity, complicated post-reaction processing, etc., and achieve the effects of good fluorescence characteristics, simple synthesis method and good stability.

Inactive Publication Date: 2011-04-20
UNIV OF JINAN
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  • Abstract
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Problems solved by technology

In the report of (1), only the simple modification of hydrazine hydrate is carried out to Rhodamine B, and its selectivity is relatively high, but the sensitivity is not so ideal; in the report of (2), the synthetic raw materials involved in the design and synthesis of fluorescent chemical sensors Problems such as high price, many reaction steps and complex post-reaction treatment
Recognition of Fe with a Synthetic Fluorescent Chemosensor 3+ patents have not yet been reported

Method used

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  • Method for manufacturing novel dendritic fluorescent chemosensor and application
  • Method for manufacturing novel dendritic fluorescent chemosensor and application
  • Method for manufacturing novel dendritic fluorescent chemosensor and application

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0023] (1) Synthesis of rhodamine B hydrazide (RBH): 1.2 g of rhodamine B was added to a 100 mL round bottom flask, and completely dissolved in 30 mL of absolute ethanol. Pipette 3.0 mL of 85% hydrazine hydrate, add it dropwise into a round bottom flask, and vibrate vigorously at room temperature. The mixture was heated and stirred at reflux for 2h. The solvent ethanol was evaporated, cooled to room temperature, and allowed to stand for 30 min. Use 50mL 1mol·L -1 HCl was dissolved in the mixture to give a dark red clear solution. Then slowly add about 70mL 1mol·L -1 NaOH, until the pH of the solution is about 7, vibrate, stand still, a brick red precipitate precipitates out, filter under reduced pressure, wash with distilled water several times, and dry to obtain rhodamine B hydrazide. Stored in a desiccator for later use, the yield is 75%.

[0024] (2) Synthesis of Compound 1: Put 3.2g (30mmol) of aminoacetaldehyde dimethyl acetal and 30mL of methanol in a 50mL round bot...

Embodiment 2

[0028] (1) Synthesis of rhodamine B hydrazide (RBH): 1.2 g of rhodamine B was added to a 100 mL round bottom flask, and completely dissolved in 30 mL of absolute ethanol. Pipette 3.0 mL of 85% hydrazine hydrate, add it dropwise into a round bottom flask, and vibrate vigorously at room temperature. The mixture was heated and stirred at reflux for 2h. The solvent ethanol was evaporated, cooled to room temperature, and allowed to stand for 30 min. Use 50mL 1mol·L -1 HCl was dissolved in the mixture to give a dark red clear solution. Then slowly add about 70mL 1mol·L -1 NaOH, until the pH of the solution is about 7, vibrate, stand still, a brick red precipitate precipitates out, filter under reduced pressure, wash with distilled water several times, and dry to obtain rhodamine B hydrazide. Stored in a desiccator for later use, the yield is 75%.

[0029] (2) Synthesis of Compound 1: Put 3.2g (30mmol) of aminoacetaldehyde dimethyl acetal and 30mL of methanol in a 50mL round bot...

Embodiment 3

[0033] Detection method of dendritic fluorescent chemical sensor: sensing Fe 3+ , adopt fluorescence method to detect, and the steps of its specific method are as follows:

[0034] (1) The dendritic fluorescent chemical sensor was made into 1.0×10 ethanol -5 mol L -1 solution; with 0.1mol L -1 Tris hydroxymethyl aminomethane (Tris) solution with an appropriate amount of 0.1mol L -1 The HCl solution was formulated into a buffer solution with a pH of 7.2, and the above two solutions were mixed at a volume ratio of 1:2 to obtain solution A.

[0035] (2) Use a pipette to pipette 3.00 mL of the above solution into a 10 mL colorimetric tube, and add 1 to 10 μg of Fe 3+ Dilute the standard solution with ethanol+water (V / V=1:5) to the mark, shake well, and after standing for 15min, measure the fluorescence intensity at 580nm, the fluorescence intensity varies with Fe 3+ Concentration increases and gradually strengthens.

[0036] (3) Fe in food samples 3+ For the determination o...

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Abstract

The invention discloses a method for manufacturing a dendritic fluorescent chemosensor and the method for detecting Fe<3+> in a sample. The method for manufacturing the dendritic fluorescent chemosensor is mainly technically characterized by comprising the following steps of: performing reaction on aminoacetaldehyde dimethyl acetal, methyl acrylate and ethylenediamine in a methanol medium under the protection of argon at the temperature of 55 to 65 DEG C for 24 to 30 h to obtain a dendritic compound; and reacting in darkness the dendritic compound with rhodamine B hydrazide in the methanol medium under the protection of the argon at room temperature for 48 to 58 h by taking 4-hydroxybenzaldehyde as a crosslinker, and performing filtration and washing to obtain the dendritic fluorescent chemosensor. In the detection method, the mixed solution of ethanol and water serves as the medium, and the Fe<3+> content of various samples is determined by utilizing a fluorophotometer in Tris-HCl buffer solution with the pH value of 6.8 to 7.5. The dendritic fluorescent chemosensor has the linear range of 0 to 10.0 mu g.mL<-1>, the detection limit of 0.026 mu g.mL<-1>, and sensitivity and selectivity which are valuable in analytical chemistry.

Description

technical field [0001] The invention relates to a preparation method of a novel dendritic fluorescent chemical sensor and its application in determination, in particular to a method for detecting Fe 3+ The preparation method and application of a specific fluorescent chemical sensor belong to the field of analysis and testing. Background technique [0002] Chemical sensors, which use optical or electronically conductive elements as recognition units, have been widely used in analytical techniques to detect specific substances. Among many sensors, fluorescence sensors have attracted people's attention due to their high sensitivity and convenient use, and have developed rapidly in recent years. Dendritic fluorescent chemical sensors are a class of compounds that introduce fluorescent dyes into the end groups of dendrimers, which have specific spatial and three-dimensional structures, and have good stability and spectral characteristics. [0003] With the development of supram...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C07D491/107G01N21/76G01J1/00
Inventor 李慧芝许崇娟裴梅山张瑾
Owner UNIV OF JINAN
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