Method for detecting hypochlorite

A technology for detecting hypochlorous acid and solution, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by chemical reaction of materials, etc., can solve the problems of difficult synthesis, complex reagent structure, etc., and achieve cost The effect of low cost, high sensitivity and selectivity, and simple detection means

Inactive Publication Date: 2012-12-12
SHANXI UNIV
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Problems solved by technology

However, these methods are not easy to synthesize due

Method used

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  • Method for detecting hypochlorite
  • Method for detecting hypochlorite
  • Method for detecting hypochlorite

Examples

Experimental program
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Embodiment 1

[0026] Synthesis of FHP: Dissolve 1mmoL of fluorescein hydrazide and 1mmoL of 2-pyridine formaldehyde in 20mL of methanol, drop 1mmoL of anhydrous acetic acid, reflux for 2 hours, recrystallize with 1:1 methanol and petroleum ether to obtain yellow FHP , yield 60%. The crystal was grown in methanol to obtain a light yellow single crystal.

[0027] Characterization of FHP:

[0028] 1 H NMR (300MHz, 25°C, DMSO-d 6 ):δ9.95(bs,2H),8.57(s,N=C-H,1H),8.49(d,Ar-H,1H),7.96(t,Pyridine-H,1H),7.81(t,Pyridine- H, 1H), 7.65(m, Ar-H, 3H), 7.35(t, Pyridine-H, 1H), 7.12(d, Pyridine-H, 1H), 6.69(d, Xanthene-H, 2H, J= 2.4Hz), 6.54(d, Xanthene-H, 2H, J=8.8Hz), 6.48(dd, Xanthene-H, 2H, J=8.8Hz, J=2.4Hz); 13 C NMR (75MHz, DMSO-d 6 ):δ164.22,158.84,153.17,151.90,151.21,149.54,146.49,137.00,134.56,129.25,127.93,127.80,124.59,123.52,119.21,112.65,109.50,102.73,64.95;ESI-MS m / z 436[FHP+ H] + ,458[FHP+Na] + ;Elemental analysis (calcd.%) for C 26 h 17 N 3 o 4 :C,71.72;H,3.94;N,9.65;Found:C,7...

Embodiment 2

[0030] Prepare HEPES buffer solution with pH=7.0, prepare 2mM FHP solution with ethanol, and prepare 2mM Cu with acetonitrile +Acetonitrile solution; 2ml of HEPES buffer solution, 40μL of FHP ethanol solution and 80μl of Cu + Add acetonitrile solution to a clean UV cuvette in turn, and detect it on a UV-visible spectrophotometer. There is no absorption peak at 350-600nm; While adding the sample, it is tested on the UV-visible spectrophotometer. With the addition of the sample to be tested, an absorption peak appears at 502nm, and the absorption intensity gradually increases. See the UV-visible absorption diagram. figure 2 .

Embodiment 3

[0032] Prepare HEPES buffer solution with pH=7.0, prepare 2mM FHP solution with ethanol, and prepare 2mM Cu with acetonitrile + acetonitrile solution; in 14 fluorescent cuvettes, add 2mL of HEPES buffer solution and 40μL of FHP ethanol solution, and 80μL of Cu + Acetonitrile solution, and then add 2.5 molar equivalents of ClO in FHP - , and 25 molar equivalents of various others (ClO 2 - , F - , Cl - ,ClO 3 - ,NO 2 - ,CN – ,S 2- ,SCN - ,P 2 o 7 4- ,AcO - ,CO 3 2- , SO 4 2- ,ClO 4 - ) anion, get the UV absorption diagram see image 3 .

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Abstract

The invention provides a method for detecting hypochlorite. The method can quantitatively detect hypochlorite based on 2-pyridylaldehyde fluorescein hydrazone (FHP) and Cu<+>. The method is concretely characterized in that the Cu<+> is oxidized into Cu<2+> by the hypochlorite in an HEPES buffer solution with the pH of 7, and a complex is prepared from the Cu<2+> and the FHP, so a change in an ultraviolet-visible spectrum appears, thereby the detection of the hypochlorite is realized. The detection method has the advantages of high sensitivity and selectivity to the hypochlorite, simple, sensitive and rapid detection process, and accurate detection result.

Description

technical field [0001] The invention relates to a hypochlorite detection technology, in particular to a method for rapidly and quantitatively detecting hypochlorite. Background technique [0002] NaOCl is widely used as a bleach and disinfectant in a concentration range of 10 -5 ~10 -2 mol / L. Its protonated form (hypochlorous acid, HClO), is a biologically important reactive oxygen species (ROS), used as an antimicrobial in organisms and in water treatment. However, excess HClO can cause tissue damage and diseases such as: hepatic ischemia-reperfusion injury, atherosclerosis, lung injury, rheumatoid and cardiovascular diseases, neuronal degeneration, arthritis and cancer. [0003] Currently reported methods for detecting hypochlorite include: colorimetric method (S.M.Chen, J.X.Lu, C.D.Sun, H.M.Ma.Analyst 135(2010) 577–582), luminescence method (J.Ballesta-Claver, M.C.Valencia- Miron, L.F.Capitán-Vallvey.Anal.Chim.Acta.522(2004)267–273), electrochemical method (A.P.Soldat...

Claims

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Application Information

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IPC IPC(8): G01N21/78
Inventor 颜叙秀霍方俊阴彩霞
Owner SHANXI UNIV
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