A monothiosquaric acid dye fluorescent probe for detecting mercury ions and its preparation

A monothiosquarate, fluorescent probe technology, applied in the direction of azo dyes, organic dyes, fluorescence/phosphorescence, etc., to achieve the effect of specific detection

Inactive Publication Date: 2014-10-01
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the design of fluorescent probes with excellent performance in all aspects and the ability to detect mercury ions at low concentrations is still a great challenge.

Method used

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  • A monothiosquaric acid dye fluorescent probe for detecting mercury ions and its preparation
  • A monothiosquaric acid dye fluorescent probe for detecting mercury ions and its preparation
  • A monothiosquaric acid dye fluorescent probe for detecting mercury ions and its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The single sulfur sulfur acid dye formula (where R =-(CH 2 Cure n -CH 3 , n = 3) Preparation

[0033] Add 1,3-two- [4- (n, n-di-borne amino group) -2-hydroxybenzyl group in 100 mL three-port bottle], Lawson reagent (233 mg, 0.58 mmol), and 35 ml no water toluene, heating back 4 h under nitrogen protection.Removal distillation removes solvent, silicon column layer is pure, and the elimation agent is petroleum ether: ethyl acetate (20: 1, v / v).C.Ftir (kbr): ν max 2955, 1682, 1614, 1397, 1345, 1285, 1216, 1186, 1109, 910, 889, 802, 773, 718 cm -1 ;; 1 H nmr (400 mHz, CDCL 3 ): Δ 0.97 (T, J = 7.3 Hz, 12H), 1.37 (DQ, DQ, J = 14.7, 7.4 Hz, 8H), 1.70-1.58 (m, 8H), 3.44-3.32 (m, 8H), 6.10 (DD, J = 4.1, 2.4 Hz, 2H), 6.41-6.28 (m, 2H), 8.17 (D, J = 9.3 Hz, 0.6h), 8.94 (D, J = 9.4 Hz, 0.6h), 9.22 (D, J = 9.3 Hz, 0.8H), 11.07 (s, 0.8h), 11.68 (s, 0.6h), 11.76 (s, 0.6h); 13 C nmr (100 MHz, CDCL 3 , 177.22, 179.46, 185.04, 185.49, 197.03, 201.98; ESI-MS: m / z 537.2 ([M+H] + ).

Embodiment 2

[0035] The single sulfur sulfur acid dye formula (where R =-(CH 2 Cure n -CH 3 , N = 1) Preparation

[0036] Add 1,3-2- [4- (n, n-diolinel) -2-hydroxybenzyl groups] -2,4-cyclonecitone (82 mg, 0.20 mmol) to the 50 mL three-bottle bottle.Lawson reagent (162 mg, 0.40 mmol), and 30 ml no water toluene, in N 2 Heating back is 1.5 h under protection.The TLC tracking reaction raw material point disappears, decompression distillation removes solvents, and then washed the residue with petroleum ether to remove soluble impurities. The silicone column layer is pure. The eluent is petroleum ether: ethyl acetate (10: 1, v / v), Green solids are about 56 mg, the yield is about 66%, and the melting point is 260-262 ° C.FTIR (KBR): νMax 2955, 2931, 1679, 1601, 1387, 1333, 1272, 1238, 1210, 1142, 1074, 1009, 959, 805, 779, 713 CM -1 It 1 H nmr (400 mHz, CDCL 3 ): Δ 1.28 (t, j = 7.1 Hz, 12H), 3.51 (q, j = 7.1 Hz, 8H), 6.16 (s, 2H), 6.46-6.34 (m, 2H), 8.22 (d, j = 11.55.5Hz, 0.6h), 8.99 (d, j = 7.3 Hz...

Embodiment 3

[0038] Founded dyes have strong absorption and efficient fluorescent launch in near infrared, making it widely used, as a superior prescription dye probe (where R =-(CH CH 2 Cure n -CH 3 N = 3) The specific recognition of mercury ions based on chemical reactions makes it a good mercury ion probe. figure 1 and figure 2 A prescription dye probe is given respectively (where R =-(CH 2 Cure n -CH 3, N = 3) Ethanol / hepes (70:30, V / V) buffer system with 7.2 response to different metal ions in the cushion system, the existence of mercury ions will cause obvious absorption spectrum and fluorescence spectrum displacement.Realize the detection of mercury ions.Based on the qualitative testing of mercury ions, the quantitative test of mercury ion is achieved.Experiments give me mercury drops of fluorescent changes image 3 It can be seen from the ticking curve that the detection of mercury ions in the range of 0-6 is good linear, and spectral experiment data proves that the dye probe is gener...

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Abstract

The invention discloses a monothiosquaric acid dye fluorescent probe for detecting mercury ions and its preparation method and application. The oxo squaraine and Lawson's reagent are mixed in proportion, dissolved in toluene, and dissolved in Under the protection of an inert gas, reflux for 1.5 to 4 hours; the resulting reaction mixture was cooled to room temperature, and the solvent was distilled off under reduced pressure to obtain a crude product; the product was obtained by silica gel column chromatography. The monothiosquaric acid dye fluorescent probe of the invention has good stability, can realize rapid, sensitive and specific detection of low-concentration mercury ions, has simple synthesis method and low production cost.

Description

Technical field [0001] The present invention is a chemical analysis test technology field, which involves a fluorescent probe and application methods and applications for detecting mercury ions to detect mercury ions. Background technique [0002] Care is recognized as a toxic element in nature, and the abuse of heavy metals has greatly threatened the natural environment and human water sources of mercury.After the quality of mercury and mercury ions can be converted into methyl mercury after being discharged into the environment.Methalis mercury is enriched in the organism through the food chain. After entering the human body, people have severe nausea, vomiting, abdominal pain, and renal damage, which is extremely harmful.Therefore, the detection of mercury ions is of great significance.The U.S. Environmental Protection Agency stipulates that the mercury content of the mercury content of human drinking water is 2 PPB. Therefore, in order to meet this standard, scientists have b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06C09B57/00G01N21/64
Inventor 傅南雁
Owner FUZHOU UNIV
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