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Reagent, and its application in detection of divalent zinc ions

A reagent, pyridoxal technology, applied in the field of optical probes, can solve problems such as zinc ions are not applicable, achieve high sensitivity and selectivity, simple detection process, and simple detection methods

Inactive Publication Date: 2013-11-20
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to Zn 2+ with a stable d 10 Electronic configuration, many commonly used spectroscopic and electrochemical analysis methods, such as ultraviolet-visible spectroscopy, electron paramagnetic resonance and cyclic voltammetry, are not suitable for the determination of zinc ions

Method used

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  • Reagent, and its application in detection of divalent zinc ions
  • Reagent, and its application in detection of divalent zinc ions
  • Reagent, and its application in detection of divalent zinc ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Synthesis of pyridoxal fluorescein hydrazone: Dissolve 1mmoL of fluorescein hydrazide and 2mmoL of pyridoxal in 20mL of ethanol, add dropwise 1mmoL of anhydrous acetic acid, reflux for 2 hours, and reconstitute with 1:1 methanol and petroleum ether. The yellow pyridoxal fluorescein acylhydrazone was obtained by crystallization, and the yield was 65%.

[0024] Characterization of pyridoxal fluorescein acylhydrazone:

[0025] 1 H NMR (300MHz, 25°C, DMSO-d 6 ):δ11.75(s,1H),10.11(s,2H),9.09(s,N=C-H,1H),8.05(s,1H),7.99(t,1H),7.67(m,2H), 7.17(t,1H),6.71(s,2H),6.54(m,2H),6.48(m,2H),4.41(s,2H),2.61(s,3H); 13 C NMR (75MHz, DMSO-d 6 ): δ163.6, 158.4, 151.3, 150.4, 143.0, 142.0, 135.9, 137.00, 134.7, 129.7, 129.0, 127.80, 127.6, 126.5, 123.4, 112.3, 107.4, 102.0, 64.5, 57.7, 14 .25[PFH+H] + ;Elemental analysis (calcd.%) for C 28 h 21 N 3 o 6 :C,67.87;H,4.27;N,8.48;Found:C,67.85;N,8.52;H,4.21.

Embodiment 2

[0027] Prepare HEPES (10mM) buffer solution with pH=7.0, prepare 2mM divalent zinc ion aqueous solution, and prepare 2mM pyridoxal fluorescein acylhydrazone solution with ethanol; mix 2mL of HEPES buffer solution and 8μL pyridoxal fluorescein acylhydrazone Hydrazone ethanol solution was added to a clean fluorescence cuvette, detected on a fluorescence spectrophotometer, along with Zn 2+ The addition of , the fluorescence intensity at 526nm gradually increased. Fluorescence emission map see figure 1 .

Embodiment 3

[0029] Prepare a HEPES buffer solution with a pH=7.0 and a concentration of 10mM, and prepare a 2mM pyridoxal fluorescein acylhydrazone solution with ethanol; add 2mL of HEPES buffer solution and 8μL of pyridoxal fluorescein to each of the 27 fluorescent cuvettes. Su-acylhydrazone ethanol solution, then add 25 molar equivalents of Zn 2+ , and 100 molar equivalents of various other analytes (Hg 2+ , Ni 2+ ,Cu + , Mn 2+ , Ru 3+ ,Cd 2+ ,Pb 2+ ,La 3+ , Ce 4+ ,Yb 3+ ,Er 3+ ,Mg 2+ ,Sn 2+ ,Al 3+ ,Nd 3+ , K + ,Sm 3+ , Fe 2+ , Fe 3+ , Eu 3+ , Ag + , Vo 2+ ,Cr 3+ ,Zr 4+ ,Co 2+ ,Cu 2+ , detected on a fluorescence spectrophotometer, draw the histogram of the 526nm fluorescence intensity corresponding to different analytes, and obtain the fluorescence emission diagram (see figure 2 ), Zn 2+ The fluorescence intensity of pyridoxal fluorescein acylhydrazone changed from 99 to about 510, and other analytes basically did not cause changes in the fluorescence intensit...

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Abstract

The invention provides a reagent for detecting divalent zinc ions. The reagent is a fluorescein derivative pyridoxal fluorescein hydrzone. The pyridoxal fluorescein hydrzone is prepared through refluxing fluorescein hydrazide and pyridoxal hydrochloride in acetic-acid-containing ethanol, and has the advantages of cheap raw materials, simple reaction condition and easy production. The invention also provides a quantitative detection method of the divalent zinc ions. The method is used for quantitatively detecting the content of the divalent zinc ions in an HEPES solution having a pH value of 7.0 based on the pyridoxal fluorescein hydrzone. The detection method is highly sensitive and selective to the divalent zinc ions, and has a simple, sensitive and rapid detection process and an accurate detection result.

Description

technical field [0001] The invention relates to an optical probe, in particular to a reagent and its synthesis method, as well as the application of the reagent in detecting divalent zinc ions. Background technique [0002] Zinc is an important metal element second only to iron in the human body, and is widely distributed in human cells and body fluids. Many facts indicate that zinc plays an important role in cell biology and cell nutrition processes. Zn 2+ It is one of the important metal ions that make up more than 300 kinds of biological enzyme active centers. In addition, the key role of zinc in cell growth and survival has been recognized in biology, physiology and pathology. For example, protein structure and function, DNA and RNA synthesis, gene expression and brain metabolism are closely related to zinc. relevant. At the same time, zinc, like calcium, is also a signal ion in various types of cells. However, most of the zinc in organisms exists in the form of com...

Claims

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Application Information

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IPC IPC(8): C07D491/107C09K11/06G01N21/64
Inventor 阴彩霞霍方俊
Owner SHANXI UNIV
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