Synthesis of multi-signal fluorescent probe and application of multi-signal fluorescent probe in simultaneously distinguishing Hcy, Cys, SO2 and GSH
A fluorescent probe and fluorescent molecular probe technology, applied in the field of analytical chemistry, can solve the problem that multi-signal fluorescent probes cannot be distinguished and detected
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Embodiment 1
[0022] Example 1. Synthesis of 9-(butylthio)-11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3- f ]pyrido[3,2,1- ij ]quinoline-10-carbaldehyde
[0023]a. Add 2.0 g (6.58 mmol) of 9-chloro-11-oxo-2,3,6,7-tetrahydro-1H,5H,11Hpyrano[2,3- f ]pyrido[3,2,1- ij ] quinoline-10-carbaldehyde and 0.715 mg (7.90 mmol) n-butanethiol were added to 20 mL of anhydrous dichloromethane, 0.2 mL of triethylamine was added dropwise, and the reaction was stirred at room temperature;
[0024] b. The reaction solution in step a is spin-dried under reduced pressure, recrystallized with an appropriate amount of absolute ethanol, filtered, and dried to obtain 9-(butylthio)-11-oxo-2,3,6,7-tetrahydro -1H, 5H, 11H-pyrano[2,3- f ]pyrido[3,2,1- ij ] Quinoline-10-carbaldehyde 1.8 g, the productive rate is 76.5%.
Embodiment 2
[0025] Example 2. Synthesis of multi-signal fluorescent probe tert-butyl ( E )-3-(9-(butylthio)-11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3- f ]pyrido[3,2,1- ij ]quinolin-10-yl)-2-cyanoacrylate (R 1 = n-butyl, R 2 = tert-butyl)
[0026] . 1.0 g (2.8 mmol) of 9-(butylthio)-11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3- f ]pyrido[3,2,1- ij ] quinoline-10-carbaldehyde and 0.435 g (3.08 mmol) tert-butyl cyanoacetate were added in 20 mL of anhydrous dichloromethane, then 0.3 mL of triethylamine was added dropwise, and the reaction was stirred at room temperature;
[0027] . After the reaction is complete, the step The middle reaction liquid is added dropwise in 30 mL absolute ethanol, filters, and the gained solid is dried, obtains the multi-signal fluorescent molecular probe tert-butyl group described in claim 1 ( E )-3-(9-(butylthio)-11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3- f ]pyrido[3,2,1- ij ] Quinoline-10-yl)-2-cyanoacrylate 740mg, productive rate...
Embodiment 3
[0028] Example 3. Multi-signal fluorescent molecular probes (here in R 1 = ethyl, R 2 = tert-butyl probe as an example, no special instructions, other probes have similar operation steps) Differentiate detection of Hcy, Cys, NaHSO in vitro 3 and GSH applications
[0029] The multi-signal fluorescent molecular probe spectral property experiment described in the present invention: the probe is dissolved in dimethyl sulfoxide (DMSO) to configure a probe solution with a concentration of 1 mM, and Cys and Hcy with a concentration of 1 mM are respectively configured NaHSO 3 (SO 2 Under physiological conditions, it mainly exists in the form of sulfite) and GSH aqueous solution. The specific test method is: take 20 μL of 1 mM probe solution, 780 μL of analytically pure DMSO, the required amount of PBS buffered aqueous solution and the required amount of 1 mM Cys / Hcy / NaHSO 3 / GSH aqueous solution in a 2 mL sample tube, and all tests kept the volume ratio of the organic phase to ...
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