Rate hydrogen sulfide chemical dosimeter and preparation method and application thereof

A technology of hydrogen sulfide chemistry and dosimetry, applied in the field of detection, can solve problems such as the decrease in the accuracy of analysis results, and achieve the effects of high yield, accurate detection and simple synthesis method

Inactive Publication Date: 2016-06-15
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of chemical dosimeter based on the change of the absolute intensity of the optical signal at a single wavelength has its own insurmountable shortcomings, that is, it is easily affected by many factors during quantitative analysis, such as absolute concentration and distribution, pH value, temperature and temperature of the system to be tested. Polarity, the stability of the detection instrument, etc., which will reduce the accuracy of the analysis results

Method used

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  • Rate hydrogen sulfide chemical dosimeter and preparation method and application thereof
  • Rate hydrogen sulfide chemical dosimeter and preparation method and application thereof
  • Rate hydrogen sulfide chemical dosimeter and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 0.235g of 1,2-lutidine iodide and 0.310g of 4-nitrobenzaldehyde into a 50ml round bottom flask, add 20ml of n-butanol, add 0.01g of piperazine, heat the mixed solution to reflux, and react for 40min . After the reaction was detected by TLC, it was cooled to room temperature, a large amount of solids were precipitated, filtered under reduced pressure, and n-butanol was recrystallized to obtain 0.230 g of an orange-red solid. The yield was 62.5%.

[0032] Melting point determination: mp: 239-242°C

[0033] Infrared spectrometry: TR (KBr, cm -1 )3346, 2997, 1635, 1616, 1567, 1516, 1457, 1349

[0034] H NMR spectrum determination: 1 HNMR (400MHZ, DMSO): δ (ppm): 9.02 (d, J = 6.0Hz, 1H), 8.60 (m, 2H), 8.36 (d, J = 8.8Hz, 2H), 8.16 (d, J = 8.8 Hz, 2H), 8.08(d, J=16Hz, 1H), 8.03(m, 1H), 7.86(d, J=16Hz, 1H), 4.45(s, 3H).

Embodiment 2

[0036] Weigh 0.2350g of 1,2-lutidine iodide and 0.3875g of 4-nitrobenzaldehyde into a 50ml round bottom flask, add 25ml of n-butanol, add 0.025g of piperazine, heat the mixed solution to reflux, and react for 30min . After the reaction was detected by TLC, it was cooled to room temperature, a large amount of solids were precipitated, filtered under reduced pressure, and n-butanol was recrystallized to obtain 0.242 g of an orange-red solid. The yield was 65.8%.

[0037] Melting point determination: mp: 239-242°C

[0038] Infrared spectrometry: TR (KBr, cm -1 )3346, 2997, 1635, 1616, 1567, 1516, 1457, 1349

[0039] H NMR spectrum determination: 1 HNMR (400MHZ, DMSO): δ (ppm): 9.02 (d, J = 6.0Hz, 1H), 8.60 (m, 2H), 8.36 (d, J = 8.8Hz, 2H), 8.16 (d, J = 8.8 Hz, 2H), 8.08(d, J=16Hz, 1H), 8.03(m, 1H), 7.86(d, J=16Hz, 1H), 4.45(s, 3H).

Embodiment 3

[0041] Weigh 0.2350g of 1,2-lutidine iodide and 0.355g of 4-nitrobenzaldehyde into a 50ml round bottom flask, add 22ml of n-butanol, add 0.018g of piperazine, heat the mixed solution to reflux, and react for 30min . After the reaction was detected by TLC, it was cooled to room temperature, a large amount of solids were precipitated, filtered under reduced pressure, and n-butanol was recrystallized to obtain 0.235 g of an orange-red solid. The yield was 63.9%.

[0042] Melting point determination: mp: 239-242°C

[0043] Infrared spectrometry: TR (KBr, cm -1 )3346, 2997, 1635, 1616, 1567, 1516, 1457, 1349

[0044] H NMR spectrum determination: 1 HNMR (400MHZ, DMSO): δ (ppm): 9.02 (d, J = 6.0Hz, 1H), 8.60 (m, 2H), 8.36 (d, J = 8.8Hz, 2H), 8.16 (d, J = 8.8 Hz, 2H), 8.08(d, J=16Hz, 1H), 8.03(m, 1H), 7.86(d, J=16Hz, 1H), 4.45(s, 3H).

[0045] Effect experiment 1

[0046] Get the ratio hydrogen sulfide chemical dosimeter obtained in Example 1 and dissolve it in the DMF solvent...

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Abstract

The invention discloses a rate hydrogen sulfide chemical dosimeter and a preparation method and application thereof. The rate hydrogen sulfide chemical dosimeter is iodized 1-methyl-2-(4-nitro)styryl pyridinium with the structural formula shown in the description. The preparation method of the rate hydrogen sulfide chemical dosimeter comprises the steps that iodized 1,2-dimethyl pyridinium and 4-nitrobenzaldehyde are added into a normal butanol solution according to the certain proportion, then, piperazine is added, a reaction is performed on the reflux condition to obtain the rate hydrogen sulfide chemical dosimeter. The rate hydrogen sulfide chemical dosimeter has the good rate chemical dosimeter characteristics, hydrogen sulfide can be rapidly and accurately detected on the physiological conditions, the selectivity of hydrogen sulfide is high, and the antijamming capability of other biological active small molecules is high. The rate hydrogen sulfide chemical dosimeter is simple in synthesis method, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a ratio hydrogen sulfide chemical dosimeter, a preparation method thereof and an application for detecting hydrogen sulfide under physiological conditions. Background technique [0002] Hydrogen sulfide (H 2 S) is a colorless gas with a typical smell of rotten eggs and has been considered a toxic chemical pollutant for centuries. In recent years, a large number of experimental studies have shown that H 2 S is the third gas signal compound discovered endogenously produced by organisms after NO and CO. It plays an important role in regulating the redox potential inside and outside cells and other signaling processes related to human health and disease. Such as modulating blood pressure, mediating neurotransmitters, regulating inflammatory response, inhibiting oxidative stress response, etc. In addition, intracellular H 2 Altered S levels have also been linked to d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/26G01N31/16G01N21/33
CPCC07D213/26G01N21/33G01N31/16
Inventor 丁静葛海燕葛燕青
Owner TAISHAN MEDICAL UNIV
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