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Reagent and detection method for series detection of Pi and o-phenylenediamine based on visualization

An o-phenylenediamine and reagent technology, which is applied in the field of reagents and detection based on visual serial detection of Pi and o-phenylenediamine, can solve problems such as undeveloped probes, and achieve the effects of low cost and simple detection means.

Pending Publication Date: 2022-05-13
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Probes that can detect these two analytes sequentially have not yet been developed

Method used

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  • Reagent and detection method for series detection of Pi and o-phenylenediamine based on visualization
  • Reagent and detection method for series detection of Pi and o-phenylenediamine based on visualization
  • Reagent and detection method for series detection of Pi and o-phenylenediamine based on visualization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) 10-(diethylamino)[c]-3-hydroxyl-5,6-benzodihydro[c]xanthene (HTD): 6-hydroxyl-1-tetraketone (0.9g, 4.05 mmol) into concentrated sulfuric acid (3 mL) solution and cooled to 0°C. Then add 4-(diethylamino) salicylaldehyde (1.176g, 6.09mmol), reflux at 90°C for 7h, cool to 25°C, cool the obtained sample with 60g ice cubes, and finally use CH 2 Cl 2 / CH 3 OH (v / v 10:1) was extracted to obtain a precipitate, which was purified by silica gel column chromatography (CH 2 Cl 2 / CH 3 O) purification to obtain the target molecule HTD.

[0031] (2) CoZn ZIF@HTD: Co(NO 3 ) 2 ·6H 2 O(1mmol) and Zn(NO 3 ) 2 ·6H 2 O (1 mmol) was dissolved in 30 mL of anhydrous methanol, and then 2-methylimidazole solution (4 mmol) and HTD (20 mg) were added to the above mixed solution. The final mixture was incubated without disturbance at room temperature for 24 h. After the reaction, the product was transferred to a centrifuge tube, washed with methanol solution for three times by rep...

Embodiment 2

[0033] Add Pi to the cuvette containing the CoZn ZIF@HTD stock solution with a micro-injector, and record the spectrum on the fluorescence spectrophotometer while adding the sample. With the addition of Pi, the fluorescence intensity at 620nm gradually increases. The concentration of Pi added Is (0, 50, 100, 150, 200, 250μM), fluorescence spectrum I 620 The relative fluorescence intensity is (157, 281, 424, 580, 692781a.u). Then take the Pi concentration as the abscissa, and take I 620 Fluorescence intensity at place is plotted on the ordinate (seeing Fig. 3), obtains Pi detection working curve; Linear regression equation is: Y=2.5765c+163.7619, and the unit of c is 10 -6 mol / L. Fluorescence emission plot and linear regression equation see Figure 3a and Figure 3b , to get a standard card.

[0034] Add o-phenylenediamine to the cuvette containing CoZn ZIF@HTD / Pi with a micro-injector, and record the spectrum on the fluorescence spectrophotometer while adding the sample. ...

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Abstract

The invention provides a reagent for series detection of inorganic phosphoric acid (Pi) and o-phenylenediamine (OPD) based on visual test paper, and a preparation method of the reagent comprises the following steps: adding 6-hydroxy-1-tetraketone into a concentrated sulfuric acid solution, cooling to 0 DEG C, then adding 4-(diethylamino) salicylaldehyde, carrying out a reflux reaction, cooling, then extracting to obtain a precipitate, washing with water, and drying to obtain the reagent for the series detection of inorganic phosphoric acid (Pi) and o-phenylenediamine (OPD). Carrying out silica gel column chromatography purification to obtain HTD; the preparation method comprises the following steps: dissolving Co (NO3) 2.6 H2O and Zn (NO3) 2.6 H2O in absolute methanol, then adding a 2-methylimidazole solution and HTD into the mixed solution, standing and hatching, after the reaction is finished, repeatedly centrifugally washing by using a methanol solution, and drying to obtain the target product CoZnZIF-coated HTD. And continuous detection of Pi and o-phenylenediamine can be realized through a fluorospectro photometer. The detection process is simple, sensitive and rapid, and the result is accurate.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a reagent and a detection method based on visual tandem detection of Pi and o-phenylenediamine. Background technique [0002] The latest research shows that inorganic phosphate (Phosphate, Pi), as one of the essential electrolytes in the body, not only participates in the process of maintaining the balance of phosphate in the body, but also provides the nutrients needed for the growth of aquatic plants. It is worth noting that high Pi in the blood is directly related to many cardiovascular complications, so a reasonable intake of Pi is worth considering. O-phenylenediamine (OPD), as an aromatic amine, is an important intermediate in organic synthesis, and is mainly used in the preparation of polymers, pesticides, dyes, etc. Aromatic amines are carcinogenic and have the potential risk of causing gene mutations. When the content of o-phenylenediamine in the human body exceeds t...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/06G01N21/78G01N21/64
CPCC08G83/008C09K11/06G01N21/78G01N21/6428G01N21/6447C09K2211/187C09K2211/188C09K2211/1466Y02P20/55
Inventor 张蕾张雅琼
Owner LIAONING UNIVERSITY
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