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Fluorescence derivation analysis method based on photocatalysis

An analytical method and photocatalytic technology, applied in the field of fluorescence analysis, can solve the problems affecting the accuracy of analytical results, separation, and high instrument requirements, and achieve the effects of controllable derivatization process, simple derivatization operation, and high derivatization efficiency.

Inactive Publication Date: 2020-12-15
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the fluorescence derivation process based on chemical oxidation generally requires the use of a large amount of strong oxidant, which is likely to cause secondary pollution to the environment, and the degree of oxidation is uncontrollable, which may affect the accuracy of the analysis results.
In the patent 201410012160.8, the author used nano-copper oxide to catalyze hydrogen peroxide to enhance the fluorescence of terephthalic acid. The catalytic process used strong oxidant hydrogen peroxide, and these oxidants could not be separated from the sample after being added to the sample solution.
Photochemical and electrochemical derivatization methods usually take a long time, have high requirements on instruments, and easily cause waste of organic reagents

Method used

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  • Fluorescence derivation analysis method based on photocatalysis
  • Fluorescence derivation analysis method based on photocatalysis
  • Fluorescence derivation analysis method based on photocatalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Fluorescence derivatization process: Add 1 mL of a certain concentration of folic acid solution, 1 mL of 0.1 mol L -1 NaAC-HAC buffer solution, pH 4.2, 100 μL 1 g L -1 Nano-TiO 2 suspension and 7.9 mL deionized water (the final concentration of photocatalyst is 0.01 g / L). The mixed solution was magnetically stirred under a 20W UV lamp for 2 min. Filter the mixture through a 0.22 μm filter membrane at room temperature. With the excitation wavelength of 280 nm, the fluorescence intensity of the filtrate at 440 nm was measured.

[0030] Such as figure 1 As shown, the fluorescence excitation and emission spectra before and after photocatalytic oxidation of folic acid, where a1 and a2 are the excitation spectra before and after folic acid oxidation, and b1 and b2 are the emission spectra before and after folic acid oxidation respectively. It can be clearly seen from the figure that The fluorescence intensity of the excitation spectrum and emission spectrum of folic ac...

Embodiment 2

[0034] This embodiment applies the analysis method of folic acid in the embodiment 1 to the detection of folic acid in the tablet:

[0035] Pretreatment of folic acid tablets: Grind a piece of folic acid into powder, dissolve it in distilled water and dilute to 100 mL, sonicate at room temperature for 10 min, filter with a separatory funnel, and take the supernatant after standing for a period of time Store in the refrigerator as a sample solution for later use. The entire operation process is carried out under low light.

[0036] Fluorescence derivatization process: Add 1 mL of the above folic acid sample solution, 1 mL of 0.1 mol L -1 NaAC-HAC buffer solution, pH 4.2, 100 μL 1 g L -1 TiO 2 suspension, and 7.9 mL deionized water. The mixed solution was magnetically stirred under a 20W UV lamp for 2 min. Filter the mixture through a 0.22 μm filter membrane at room temperature. With the excitation wavelength of 280 nm, the fluorescence intensity of the filtrate at 440 nm ...

Embodiment 3

[0039] This embodiment provides a fluorescence analysis method based on photocatalytic oxidation derivation for detecting terephthalic acid, which specifically includes the following steps:

[0040] Fluorescence derivation process: Add 1.00 mL of a certain concentration of terephthalic acid solution, 1 mL of 0.004mol L -1 Sodium hydroxide solution, 1 mL 1 g L -1 Tin oxide suspension and 7 mL deionized water (the final concentration of photocatalyst is 0.1 g / L). The mixed solution was magnetically stirred under a 150W UV lamp for 30 min. A hydrogen on the benzene ring is replaced by a hydroxyl group, and a fluorescence peak appears at 425 nm. Filter the mixture through a 0.22 μm filter membrane at room temperature. With the excitation wavelength of 315 nm, the fluorescence intensity of the filtrate at 425 nm was measured.

[0041] Establishment of the standard curve: after photocatalytic oxidation of terephthalic acid standard solutions with different concentrations, they...

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Abstract

The invention discloses a fluorescence derivation analysis method based on photocatalysis, which comprises the following steps: S1, under an illumination condition, a photocatalyst catalyzing a fluorescence-free to-be-detected substance solution to derive into a fluorescent substance solution, and separating the photocatalyst and the fluorescent substance solution; S2, establishing a standard curve: measuring fluorescence intensity of oxidation products of standard solutions with different concentrations at specific wavelengths, and drawing the standard curve by taking the concentration of theto-be-measured solution as an abscissa and the fluorescence intensity as an ordinate; and S3, determining the to-be-detected substance in the sample: replacing the standard substance solution with the sample subjected to isopyknic treatment, operating according to the step S2, and substituting the measured fluorescence intensity into the standard curve obtained in the step S2 to obtain the concentration of the to-be-detected substance in the sample. An external strong oxidant is not needed, the method is environment-friendly, the photocatalyst is easily separated from a to-be-detected object,the analysis result is accurate, and the consumed time is short.

Description

technical field [0001] The invention relates to the field of fluorescence analysis, in particular to a photocatalysis-based fluorescence derivation analysis method. Background technique [0002] In recent years, with the rapid development of analytical instruments and modern analytical technologies, various analytical methods emerge in an endless stream, among which the fluorescence method is an analytical method that combines the three advantages of high analytical sensitivity, strong selectivity and easy use. Fluorescent methods can be used for direct detection of substances that are themselves fluorescent. For some substances with no fluorescence or extremely weak fluorescence, especially for the detection of some drugs, indirect fluorescence method is usually used for detection. The indirect fluorescence method is generally divided into two types, one is based on the energy transfer between the compound and the fluorescent probe, and the detection of the substance is re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
CPCG01N21/64
Inventor 陈芳吴姝胡琪吴康兵
Owner HUAZHONG UNIV OF SCI & TECH
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