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Thia-calyx [4] arene fluorescent reagent with selective bonding La<3+>lu<3+>, synthesis and application

An aromatic hydrocarbon fluorescence and thia calix technology, applied in the field of analytical chemistry, can solve the problems of unidentified and detected rare earth ions

Inactive Publication Date: 2015-05-20
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the thia[4]arene fluorescent probes reported in the literature are used to identify metal ions K+, Fe3+, Cu2+, Ag+, Pb2+ and anion F-, AcO-, etc., no one can identify and detect rare earth Ion related reports

Method used

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  • Thia-calyx [4] arene fluorescent reagent with selective bonding La&lt;3+&gt;lu&lt;3+&gt;, synthesis and application
  • Thia-calyx [4] arene fluorescent reagent with selective bonding La&lt;3+&gt;lu&lt;3+&gt;, synthesis and application
  • Thia-calyx [4] arene fluorescent reagent with selective bonding La&lt;3+&gt;lu&lt;3+&gt;, synthesis and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0114] Embodiment one: Reagent s1 , s2 preparation of

[0115] 1. Synthesis of intermediate 1,3-alternate-bis(phthalimide)thiacalix[4]arene

[0116] N 2 Under protection, in a 50ml round bottom flask, add thiacalix[4]arene, hydroxyethylphthalimide, triphenylphosphine, anhydrous THF, under ice bath, stir evenly, slowly drop DEAD, add thiacalix[4]arene in molar ratio: hydroxyethylphthalimide: DEAD=1:8:3, add after adding, stir at room temperature for 48h, evaporate solvent, add hot Methanol was cooled to precipitate a white solid, and ethyl acetate / n-hexane (1 / 4, v / v) was used as the eluent to obtain a white intermediate material through column chromatography.

[0117] 2. Intermediate 1,3-alternate-bis(2-phthalimide)-2,4-bis(2-methoxyethoxy)-tetra(p-tert-butyl)thiacalix[ 4] Aromatics ( 1-a ) and the intermediate 1,3-alternate-bis(2-phthalimide)-2,4-tetra(p-tert-butyl)thiacalix[4]crown-5arene ( 1-b )Synthesis

[0118] N 2 Under protection, in a round bottom flask, add 1,...

Embodiment 2

[0129] The preparation method of reagent among the present invention is:

[0130] (1) Reagents s1 Solution: Weigh 12.3mg of the reagent s1 , dissolved in DMF, and prepared into a 100mL solution with a concentration of 100μmol L -1 ;

[0131] (2) Reagents s2 Solution: weigh 12.7mg of the reagent s2 , dissolved in DMF, and prepared into a 100mL solution with a concentration of 100μmol L -1 ;

[0132] (3) La 3+ Standard solution: weigh 43.3mg lanthanum nitrate hexahydrate [La(NO 3 ) 3 ·6H 2 O], dissolved in distilled water, prepared into a 50mL solution, La 3+ The concentration is 2.00×10 -3 mol L -1 ; Dilute step by step with DMF to a suitable concentration as required;

[0133] (4) Lu 3+ Standard solution: weigh 46.9mg lutetium nitrate hexahydrate [La(NO 3 ) 3 ·6H 2 O] dissolved in DMF, prepared into 50 mL solution, Lu 3+ The concentration is 2.00×10 -3 mol L -1 , according to the need to use DMF to gradually dilute to a suitable concentration;

[0134] (...

Embodiment 3

[0138] Embodiment three: Reagent s1 to la 3+ 、Lu 3+ ion detection

[0139] Add reagents to 10.0 mL volumetric flask s1 DMF stock solution (1.00 x 10 -4 mol L -1 , 1mL), the metal ion La 3+ (2.00×10 -3 mol L -1 , 1 mL) or Lu 3+ (2.00×10 -3 mol L -1 , 1 mL), Tris-HCl buffer (1.00×10 -3 mol / L, 1.0 mL, pH 6), with DMF / H 2 O (9 / 1, v / v) solvent was diluted to the mark, shaken, and transferred to a 1cm quartz cuvette for fluorescence spectrum measurement.

[0140] Set the fluorescence excitation wavelength to 360nm, for the reagent s1 (1.00×10 -5 mol L -1 ) DMF / H 2 O (9 / 1, v / v, pH 6) solution for fluorescence spectroscopy test, reagent s1 There is fluorescence emission at a wavelength of 424 nm. Join La 3+ or Lu 3+ (2.00×10 -4 mol L -1 ), the reagent s1 The fluorescence intensity of the solution at 542nm or 535nm was significantly enhanced, and the emission wavelengths all appeared red-shifted. The photos under the ultraviolet light showed that the soluti...

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Abstract

The invention relates to two thia-calyx [4] arene fluorescent reagents s1 and s2 with selective bonding La<3+>lu<3+>. The chemical names of the two thia-calyx [4] arene fluorescent reagents are respectively 1,3-alternation-bis(8-hydroxyquinoline-2-aldehyde amine oxethyl)-2,4-bis(2-methoxyl oxethyl)-quadri (p-tert-butyl) thia-calyx [4] arene and 1,3-alternaiton-bis(8-hydroxyquinoline-2-aldehyde amine oxethyl)-2,4-quadri(p-tert-butyl) thia-calyx [4] arene. Spectrofluorimetry for quantitatively measuring La<3+> and Lu<3+> ions with reagents s1 and s2 is established. The La<3+> and Lu<3+> ions are subjected to fluorescence detection by the reagents s1 and s2 in N,N-dimethylformamide / water (v / v=9 / 1) and tri-hydroxymethyl aminomethane-HCl buffered solution (pH 6) with high selection and high sensitivity. The detection linear range reaches two orders of magnitude, and detection limit is as low as 10<-9>mol*L<-1>.

Description

technical field [0001] The invention belongs to the field of analytical chemistry. Specifically, it is a kind of fluorescence method to detect La 3+ or Lu 3+ Methods. Background technique [0002] Fluorescent probes are based on the organic combination of molecular recognition and fluorescence technology. Through the selective binding of probes to specific objects, different signal transduction mechanisms are used to convert the recognition information into fluorescent signals that are easy to detect. detection at the molecular level. Using fluorescence enhancement or quenching to realize the detection of specific target molecules and ions is the main method for the application of fluorescent probes. Due to the high sensitivity and high selectivity of fluorescence analysis, real-time in-situ detection, simple equipment, and can provide rich spectral information, various ion detection, DNA and protein in analytical chemistry, biochemistry, environmental science, pharmaceu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C07D341/00C07D513/08G01N21/64
Inventor 曾晞余梅冉茂乾袁剑英牟兰
Owner GUIZHOU UNIV
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