Functional rareearth complexes long-life fluorochrome, synthesis and uses thereof
A technology of rare earth complexes and fluorescent dyes, which is applied in the field of synthesis of fluorescent dyes, to achieve the effects of low detection limit, good chemical stability and photostability, and high sensitivity
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Embodiment 1
[0032] The preparation of the rare earth europium complex with thienoyltrifluoroacetone and 5-amino-1,10-phenanthroline as ligands is as follows:
[0033] a, 1,10-phenanthroline is used as raw material to prepare 5-nitro-1,10-phenanthroline, which is synthesized by the following reaction:
[0034]
[0035] Add 5.00g of 1,10-phenanthroline into the three-necked flask, and add 7.5ml of concentrated sulfuric acid into the three-necked flask to mix the two evenly, continue to stir, heat in an oil bath, and pipette 15ml of concentrated sulfuric acid and 15ml of concentrated nitric acid Put the mixture in a constant pressure dropping funnel, slowly add the mixture dropwise under the condition of heating and stirring, the temperature does not exceed 170°C, react for 3h, cool to room temperature, pour the reaction solution into the prepared ice water, and use 10% The sodium hydroxide solution adjusts the pH to about 6.0, and a yellow substance precipitates out; it is filtered by su...
Embodiment 2
[0046] The preparation of the rare earth terbium complex with thienoyltrifluoroacetone and 5-amino-1,10-phenanthroline as ligands is as follows:
[0047] A, take 1,10-phenanthroline as raw material and prepare 5-nitro-1,10-phenanthroline, with embodiment 1.
[0048] B, take 5-nitro-1,10-phenanthroline as raw material and prepare 5-amino-1,10-phenanthroline, with embodiment 1.
[0049] c, take terbium oxide as raw material to prepare terbium chloride, and synthesize through the following reactions:
[0050] Tb 4 o 7 +HClO 4 →Tb(ClO 4 ) 3 ·6H 2 o
[0051] Weigh 123.27 mg of terbium oxide in perchloric acid, heat to dissolve, remove excess perchloric acid, add ethanol to dilute to obtain a transparent solution.
[0052] d. Using thienoyltrifluoroacetone, 5-amino-1,10-phenanthroline, and terbium chloride as raw materials to prepare rare earth terbium complexes, synthesize them through the following reactions:
[0053]
[0054] Dissolve 440.60 mg of thienoyltrifluoroace...
Embodiment 3
[0056] The DNA of Staphylococcus aureus is detected by labeling with the rare earth europium complex prepared in Example 1 3 , adopt the detection method of the sandwich model reported by patent (Tan Weihong, Wang Kemin, Gong Ping, He Xiaoxiao, silicon-shell nanoparticle detection method for SARS virus genome fragment, Chinese patent, disclosure date on March 23rd, 2005, publication number CN 1597987A) ,Such as image 3 shown. Specific steps:
[0057] a. Formylation of glass slides and probe DNA modified with amino groups 1 Fixation on the surface of the glass slide, specific steps: (1) immerse the square glass slide (diameter 13mm) in the chromic acid lotion and soak overnight, wash in distilled water, immerse in 25% ammonia water overnight, wash in double distilled water, immerse in 2% In 95% ethanol solution of aminosilane reagent, adjust the pH to 4.5 with glacial acetic acid, react at room temperature for 30 min, ultrasonically clean with ethanol and double distilled w...
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