Fluorescent probe reagent for concurrent selection and determination of multiple metal ions, and preparation and appliance
A metal ion and multi-metal technology, applied in the field of probe reagents for simultaneous selection and determination of multi-metal ions, can solve problems such as unreported
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Embodiment 1
[0094] Embodiment one: the synthesis of intermediate:
[0095] In a 250ml three-neck flask, add rhodamine B (1.64g, 3.42mM) and 60mL of ethanol. in N 2 Under protection, the temperature was raised to 78°C, and tris(2-aminoethyl)amine (4.0 g, 27.36 mM) was gradually added dropwise at a rate of 1 drop per second, and refluxed for 36 h until the solution became colorless. The solvent ethanol was evaporated, 60 mL of water was added, and extracted three times with dichloromethane (60 mL×3), and the organic phases were combined. Dry with anhydrous magnesium sulfate, filter, and evaporate the solvent to obtain a red oily liquid, which is purified by column chromatography, and the eluent is: chloroform / methanol / triethylamine (v / v / v=9 / 1 / 1), to obtain 1.52g colorless oily liquid intermediate, yield 77.6%.
Embodiment 2
[0096] Embodiment two: the synthesis of product:
[0097] In a 250ml three-neck flask, add the intermediate (1.10g, 1.92mM), 2-hydroxy-1-naphthaldehyde (660mg, 3.84mM), dissolve in 100mL of methanol, and heat up to 40°C. in N 2 Reflux overnight under protection, evaporate the solvent, and purify by silica gel column chromatography under reduced pressure. The collection rate of the eluent is 25-30ml per minute. The eluent is chloroform, and 1.5g of yellow solid is obtained, with a yield of 85.2%. 1 HNMR (500MHz, CD 3 OD)δ:14.214(s,2H,OH),8.611(s,2H,CH=N),7.924(d,J=4.5Hz,1H,Ar-H),7.774(d,J=8.5Hz,2H ,Ar-H),7.546(d,J=9.5Hz,2H,Ar-H),7.507(d,J=8.0Hz,2H,Ar-H),7.475(t,J=4.5Hz,2H,Ar -H),7.330(t,J=7.5Hz,2H,Ar-H),7.157(t,J=7.5Hz,2H,Ar-H),7.116(t,J=4.5Hz,1H,Ar-H ),6.790(d,J=9.5Hz,2H,Ar-H),6.435(d,J=8.5Hz,2H,Ar-H),6.392(d,J=2.5Hz,2H,Ar-H), 6.265(d,J=9.0Hz,2H,Ar-H),3.448(s,4H,CH 2 CH 2 N=C),3.285-3.244(m,10H,NCH 2 CH 3 ,CH 2 CH 2 N-CO), 3.726(t, J=6.0Hz, 4H, CH 2 CH 2N=C),2.496...
Embodiment 3
[0099] The preparation method of various reagents in the analytical method of the present invention is:
[0100] (1) Preparation method of the probe solution: weigh 88mg of the probe (molecular formula: C 56 h 58 N 6 o 4
[0101] Molecular weight: 879.10), 1,4-dioxane was dissolved and prepared into 100mL of a solution with a concentration of 1mM.
[0102] (2) Cu 2+ Stock solution preparation method: weigh 0.1853g of copper perchlorate, dissolve in water, and prepare 50mL of a solution with a concentration of 10mM.
[0103] (3) Co. 2+ Stock solution preparation method: weigh 0.1830 g of cobalt perchlorate, dissolve it in water, and prepare 50 mL of a solution with a concentration of 10 mM.
[0104] (4) Fe 3+ Stock solution preparation method: Weigh 0.1171g of ferric perchlorate, dissolve it in water, and prepare 50mL of a solution with a concentration of 10mM.
[0105] (5) Zn 2+ Stock solution preparation method: Weigh 0.1321g of zinc perchlorate, dissolve it in wate...
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