CN108152260B - A kind of fluorescent optical sensor and preparation method thereof detecting uric acid - Google Patents
A kind of fluorescent optical sensor and preparation method thereof detecting uric acid Download PDFInfo
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- CN108152260B CN108152260B CN201711409787.7A CN201711409787A CN108152260B CN 108152260 B CN108152260 B CN 108152260B CN 201711409787 A CN201711409787 A CN 201711409787A CN 108152260 B CN108152260 B CN 108152260B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention belongs to the analysis detection fields that metal-organic framework materials are used for disease markers, and in particular to a kind of fluorescent optical sensor and preparation method thereof for detecting uric acid.By by the uric acid solution and NH of various concentration same volume2After-BDC-MOF nanometer sheet solution, uricase solution and o-phenylenediamine solution concussion mixing, is placed 30 minutes at 37 DEG C, detect fluorescence signal, construct fluorescence signal-concentration working curve；Then the fluorescence signal in test sample substitutes into working curve, the uric acid in quantitative analysis sample can be realized.This method is quick, sensitive and efficient.
Description
Technical field
The invention belongs to the analysis detection fields that metal-organic framework materials are used for disease markers, and in particular to Yi Zhongjian
Survey the fluorescent optical sensor and preparation method thereof of uric acid.
Background technique
Biomolecule uric acid (2,4,6-trihydroxy purine, abbreviation UA) is the final product of purine metabolism in human body, in people
It is played an important role in the metabolism of body.Frequently as the sign of the diseases such as gout, nephrosis, high lithemia, body when uric acid exception
The variation of uric acid content can sufficiently reflect the situation of the functions such as human body metabolism, immune in liquid.Its molecular formula is
C15H14N4O3, it is not soluble in water, it is also insoluble in acid, it is readily soluble under alkaline condition, the detection to the substance is thus greatly limited,
Commonly used detection method has liquid chromatography, fluorescence method, electrochemical method etc..Under the action of uricase, uric acid can be by
It is oxidized to allantoin and hydrogen peroxide.Therefore, the method that one kind is quick, sensitive, accurately detects the substance is found, and has weight
Want research significance.
Work based on 3-dimensional metal organic framework material building biosensor for uric acid detection is also rarely reported, such as
Utilize UIO-66-NO2@XC-72 composite material to uric acid detected (RSC Adv., 2017,7,5628-5635) and
Uric acid is detected using the fluorescent optical sensor of CD-MONT-2 ' building fluorescence enhancement (J. Mater. Chem. C, 2017,
5,601-606), but these work have material preparation complexity, many and diverse disadvantage of detection process.Compared to traditional method
The middle 3-dimensional metal organic framework material utilized, the two-dimensional metallic organic framework material that synthesizes has preferably special in the present invention
Property.
With the development of research, the material of various novelties is developed.The research direction of material science is also from traditional
To composite material, two-dimentional, one-dimensional or even zero dimension material direction is developed for body material, homogenous material.Two-dimensional material refers to by SP2Hydridization
The material of the single layer or several layers of atomic building that bond together to form.In two-dimensional material, free electron can be in single layer space certainly
By moving, furthermore two-dimensional material also possesses unique two dimensional topology, these features make two-dimensional material have it is some with it is traditional
The entirely different new kink characteristics of body material, in general two-dimensional material possess excellent electronics conduction, optically and mechanically change performance.
Two-dimensional metallic organic framework material (2D-MOF) causes the concern of more and more scholars in recent years, because it
The advantages that porosity of existing metal-organic framework materials, high specific surface area, easy functionalization, while there is two-dimensional material to be had
The excellent electronics having conducts, optically and mechanically changes energy.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of fluorescent optical sensor and its system for detecting uric acid
Preparation Method.The present invention has fluorescence and analogue enztme characteristic using synthesized two-dimensional metallic organic framework material, in conjunction with uric acid
The specific recognition capability of enzyme provides a kind of quick, sensitive, efficient uric acid detection method.
In order to achieve the above-mentioned object of the invention, the present invention proposes following technical scheme:
A kind of preparation method for the fluorescent optical sensor detecting uric acid, including the following steps:
1) the uric acid solution of various concentration unit is prepared；
2) by the two-dimensional metallic organic framework material NH with fluorescent characteristic2- BDC-MOF nanometer sheet is scattered in ultrapure water
30 min of ultrasound, centrifuging and taking supernatant is spare, NH in supernatant2The concentration of-BDC-MOF nanometer sheet is 200 μ g/mL；
3) it takes uricase to be dissolved in three (methylol) aminomethane-hydrochloride buffers and uricase solution is made, be protected from light
Be stored in 4 DEG C it is spare；
4) it takes o-phenylenediamine to be dissolved in three (methylol) aminomethane-hydrochloride buffers and o-phenylenediamine solution is made,
Stored protected from light is spare at 4 DEG C；
5) NH for the 200 μ g/mL for taking step 2 to prepare respectively250 μ L of-BDC-MOF nanometer sheet solution, step 3) are prepared
The 10 μ L of uricase solution and step 4) of 0.1U/mL prepare the 50 μ L of o-phenylenediamine solution of 2 mM and add after three is shaken mixing
Enter 90 μ L Tris-HCl (50 mM pH 7.4) buffer supplement volume to 200 μ L, places 30 minutes, detect glimmering at 37 DEG C
Optical signal；
6) NH for the 200 μ g/mL for taking step 2 to prepare250 μ L of-BDC-MOF nanometer sheet solution, step 3) prepare 0.1
The uric acid solution of the 10 μ L of uricase solution of U/mL and 50 μ L various concentration same volumes add the neighbour that step 4) prepares 2 mM
50 μ L of phenylenediamine solution is added 40 μ L Tris-HCl (50 mM pH 7.4) buffer and supplements body after four concussion mixing
Product is incubated for 30 minutes at 37 DEG C to 200 μ L, detects the fluorescence signal in the presence of various concentration uric acid；
7) according to the fluorescence signal of various concentration uric acid, fluorescence signal-concentration working curve is constructed.
Two-dimensional metallic organic framework material NH described in step 22The preparation method of-BDC-MOF nanometer sheet, including it is following
Step:
(1) 1.0-3.0 mg neighbour's amino terephthalic acid (TPA) is dissolved in the N that 2.0-5.0 mL volume ratio is 2:1, N- diformazan
The in the mixed solvent of base formamide and acetonitrile；
(2) 2.0-4.0 mg Gerhardite is dissolved in the N that 2.0-5.0 mL volume ratio is 1:2, N- dimethyl methyl
The in the mixed solvent of amide and acetonitrile；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 1.0-3.0 mL volume ratio is 1:1 is prepared as company
Connect liquid；
(4) adjacent amino terephthalic acid solution is charged first to the examination that diameter is 1.0-2.0 cm, capacity is 10-30 mL
Bottom of the tube adds the connection liquid of 1.0-3.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 30-50 DEG C of water-bath in test tube, is reacted 24-48 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, the 60-100 in vacuum drying oven
Two-dimensional metallic organic framework material NH is made in DEG C drying2- BDC-MOF nanometer sheet.
Preferably, two-dimensional metallic organic framework material NH described in step 22The preparation method of-BDC-MOF nanometer sheet, packet
Include following steps:
(1) 1.5 mg neighbour's amino terephthalic acid (TPA)s are dissolved in the n,N-Dimethylformamide that 3.0 mL volume ratios are 2:1
With the in the mixed solvent of acetonitrile；
(2) 3.0 mg Gerhardites are dissolved in the n,N-Dimethylformamide and second that 3.0 mL volume ratios are 1:2
The in the mixed solvent of nitrile；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 2.0 mL volume ratios are 1:1 is prepared as connection
Liquid；
(4) adjacent amino terephthalic acid solution is charged first to the test tube bottom that diameter is 1.5 cm, capacity is 25 mL,
The connection liquid for adding 2.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 40 DEG C of water-baths in test tube, is reacted 24 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, is done for 80 DEG C in vacuum drying oven
It is dry, two-dimensional metallic organic framework material NH is made2- BDC-MOF nanometer sheet.
A kind of fluorescent optical sensor of preparation method as described above detection uric acid obtained.
A kind of application method of fluorescent optical sensor as described above, comprising the following steps:
1) NH is taken2- BDC-MOF nanometer sheet solution, uricase solution and o-phenylenediamine solution, after three is shaken mixing,
It is placed 30 minutes at 37 DEG C, detects fluorescence signal；
2) sample solution is added into step 1), is incubated for 30 minutes at 37 DEG C, detects fluorescence signal；
3) fluorescence signal is substituted into fluorescence signal-concentration working curve, obtains uric acid content in sample.
In the present invention, to the NH of synthesis2- BDC-MOF nanometer sheet is scanned Electronic Speculum (SEM) and atomic force microscope
(AFM) it characterizes using the material for proving synthesis as two-dimensional slice structure (SEM is as shown in Fig. 2, AFM is as shown in Figure 3), while utilizing glimmering
Photothermal spectroscopic analyzer is characterized (such as Fig. 4) to the fluorescent characteristic of material.When, there are when uric acid, uric acid and uricase occur instead in system
Hydrogen peroxide should be generated, due to the two-dimensional metallic organic framework material NH of above-mentioned synthesis2- BDC-MOF nanometer sheet has analogue enztme
Activity, the hydrogen peroxide that can be catalyzed generation decompose production hydroxyl radical free radical (OH), since hydroxyl radical free radical has Strong oxdiative
Property, can the o-phenylenediamine in oxidation system become 2,3- diaminophenol piperazine, 2,3- diaminophenol piperazines and NH2- BDC-MOF nanometers
Piece can generate fluorescence resonance energy transfer to make NH2The fluorescence signal of-BDC-MOF nanometer sheet is compared to that there is no targets
It is low when object uric acid, the analysis detection to uric acid is realized accordingly.Testing principle is as shown in Figure 1.
In a kind of method of above-mentioned fluorescent optical sensor detection uric acid, the two-dimensional metallic organic framework material NH2-BDC-
MOF nanometer sheet can not only emit fluorescence, and material has horseradish peroxidase activity, being capable of catalyzing hydrogen peroxide decomposition
Generate hydroxyl radical free radical.
The method of fluorescent optical sensor detection uric acid of the present invention based on two-dimensional metallic organic framework material nanometer sheet
It is not limited in NH obtained in above-mentioned steps2- BDC-MOF nanometer sheet also includes other two-dimensional metallic organic framework materials, together
When, for that can generate the substance of hydrogen peroxide such as: glucose, hypoxanthine, acetylcholine conceive model in the technology of the present invention
The biomolecule that two-dimensional metallic organic framework material in enclosing and capable of reacting generates hydrogen peroxide belongs to guarantor of the invention
Protect range.
The beneficial technical effect of the present invention lies in:
The present invention utilizes analysis detection of the material building biosensor of synthesis for uric acid；Existing uric acid is overcome to detect
The deficiencies of interference of technology co-existence substance is big, sensitivity is low, cumbersome, has using synthesized two-dimensional metallic organic framework material
There are fluorescence and analogue enztme characteristic, in conjunction with the specific recognition capability of uricase, the detection method is quickly, efficiently.
Detailed description of the invention
Fig. 1 is based on NH2The schematic diagram of the fluorescent optical sensor detection uric acid of-BDC-MOF nanometer sheet building；
Fig. 2 NH2Scanning electron microscope (SEM) figure of-BDC-MOF nanometer sheet；
Fig. 3 NH2Atomic force microscope (AFM) phenogram of-BDC-MOF nanometer sheet；
Fig. 4 NH2The fluorescent characteristic figure of-BDC-MOF nanometer sheet；
Fig. 5 is based on NH2The fluorescence spectrum of the fluorescent optical sensor detection various concentration uric acid of-BDC-MOF nanometer sheet building
Scheme (A), the working curve diagram (B) of sensor detection uric acid and the working curve diagram of sensor detection uric acid seek uric acid concentration
The matched curve (C) that logarithm is done.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
A kind of preparation method for the fluorescent optical sensor detecting uric acid, including the following steps:
1) the uric acid solution of various concentration unit is prepared；
2) by the two-dimensional metallic organic framework material NH with fluorescent characteristic2- BDC-MOF nanometer sheet is scattered in ultrapure water
30 min of ultrasound, centrifuging and taking supernatant is spare, NH in supernatant2The concentration of-BDC-MOF nanometer sheet is 200 μ g/mL；
3) it takes uricase to be dissolved in three (methylol) aminomethane-hydrochloride buffers and uricase solution is made, be protected from light
Be stored in 4 DEG C it is spare；
4) it takes o-phenylenediamine to be dissolved in three (methylol) aminomethane-hydrochloride buffers and o-phenylenediamine solution is made,
Stored protected from light is spare at 4 DEG C；
5) NH for the 200 μ g/mL for taking step 2 to prepare respectively250 μ L of-BDC-MOF nanometer sheet solution, step 3) are prepared
The 10 μ L of uricase solution and step 4) of 0.1U/mL prepare the 50 μ L of o-phenylenediamine solution of 2 mM and add after three is shaken mixing
Enter 90 μ L Tris-HCl (50 mM pH 7.4) buffer supplement volume to 200 μ L, places 30 minutes, detect glimmering at 37 DEG C
Optical signal；
6) NH for the 200 μ g/mL for taking step 2 to prepare250 μ L of-BDC-MOF nanometer sheet solution, step 3) prepare 0.1
The uric acid solution of the 10 μ L of uricase solution of U/mL and 50 μ L various concentration same volumes add the neighbour that step 4) prepares 2 mM
50 μ L of phenylenediamine solution is added 40 μ L Tris-HCl (50 mM pH 7.4) buffer and supplements body after four concussion mixing
Product is incubated for 30 minutes at 37 DEG C to 200 μ L, detects the fluorescence signal in the presence of various concentration uric acid；
7) according to the fluorescence signal of various concentration uric acid, fluorescence signal-concentration working curve is constructed.
Two-dimensional metallic organic framework material NH described in step 22The preparation method of-BDC-MOF nanometer sheet, including it is following
Step:
(1) 1.0-3.0 mg neighbour's amino terephthalic acid (TPA) is dissolved in the N that 2.0-5.0 mL volume ratio is 2:1, N- diformazan
The in the mixed solvent of base formamide and acetonitrile；
(2) 2.0-4.0 mg Gerhardite is dissolved in the N that 2.0-5.0 mL volume ratio is 1:2, N- dimethyl methyl
The in the mixed solvent of amide and acetonitrile；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 1.0-3.0 mL volume ratio is 1:1 is prepared as company
Connect liquid；
(4) adjacent amino terephthalic acid solution is charged first to the examination that diameter is 1.0-2.0 cm, capacity is 10-30 mL
Bottom of the tube adds the connection liquid of 1.0-3.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 30-50 DEG C of water-bath in test tube, is reacted 24-48 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, the 60-100 in vacuum drying oven
Two-dimensional metallic organic framework material NH is made in DEG C drying2- BDC-MOF nanometer sheet.
Preferably, two-dimensional metallic organic framework material NH described in step 22The preparation method of-BDC-MOF nanometer sheet, packet
Include following steps:
(1) 1.5 mg neighbour's amino terephthalic acid (TPA)s are dissolved in the n,N-Dimethylformamide that 3.0 mL volume ratios are 2:1
With the in the mixed solvent of acetonitrile；
(2) 3.0 mg Gerhardites are dissolved in the n,N-Dimethylformamide and second that 3.0 mL volume ratios are 1:2
The in the mixed solvent of nitrile；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 2.0 mL volume ratios are 1:1 is prepared as connection
Liquid；
(4) adjacent amino terephthalic acid solution is charged first to the test tube bottom that diameter is 1.5 cm, capacity is 25 mL,
The connection liquid for adding 2.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 40 DEG C of water-baths in test tube, is reacted 24 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, is done for 80 DEG C in vacuum drying oven
It is dry, two-dimensional metallic organic framework material NH is made2- BDC-MOF nanometer sheet.
A kind of fluorescent optical sensor of preparation method as described above detection uric acid obtained.
A kind of application method of fluorescent optical sensor as described above, comprising the following steps:
1) NH is taken2- BDC-MOF nanometer sheet solution, uricase solution and o-phenylenediamine solution, after three is shaken mixing,
It is placed 30 minutes at 37 DEG C, detects fluorescence signal；
2) sample solution is added into step 1), is incubated for 30 minutes at 37 DEG C, detects fluorescence signal；
3) fluorescence signal is substituted into fluorescence signal-concentration working curve, obtains uric acid content in sample.
Embodiment 1(the method for the present invention detects uric acid)
1, NH is first synthesized2- BDC-MOF nanometer sheet, process are as follows:
1) by 1.5 mg neighbour's amino terephthalic acid (TPA)s be dissolved in 3 mL volume ratios be 2:1 n,N-Dimethylformamide and
The in the mixed solvent of acetonitrile；
2) 3.0 mg Gerhardites are dissolved in the n,N-Dimethylformamide and acetonitrile that 3 mL volume ratios are 1:2
In the mixed solvent；
3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 2 mL volume ratios are 1:1 is prepared as bridging agent；
4) reaction carries out in the test tube of 1.5 cm diameter, 25 mL, and adjacent amino terephthalic acid solution is charged first to test tube
Bottom adds the bridging agent of 2 mL, is eventually adding the solution that upper layer is dissolved with copper nitrate；
5) adjacent amino terephthaldehyde acid layer is heated in 40 DEG C of water-baths, reacts 24 hours；
6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile, 80 DEG C of dryings in vacuum drying oven using centrifugation；
2, the two-dimensional metallic organic framework material NH by above-mentioned with fluorescent characteristic2- BDC-MOF nanometer sheet is scattered in ultrapure
30 min of ultrasound in water, centrifuging and taking supernatant (200 μ g/mL) are spare；
3, it takes uricase to be dissolved in three (methylol) aminomethane-hydrochloride buffers and uricase solution is made, be protected from light storage
It is spare there are 4 DEG C；
4, it takes o-phenylenediamine to be dissolved in three (methylol) aminomethane-hydrochloride buffers and o-phenylenediamine solution is made, keep away
Light be stored in 4 DEG C it is spare；
5) NH for the 200 μ g/mL for taking step 2 to prepare respectively250 μ L of-BDC-MOF nanometer sheet solution, step 3) are prepared
The 10 μ L of uricase solution and step 4) of 0.1U/mL prepare the 50 μ L of o-phenylenediamine solution of 2 mM and add after three is shaken mixing
Enter 90 μ L Tris-HCl (50 mM pH 7.4) buffer supplement volume to 200 μ L, places 30 minutes, detect glimmering at 37 DEG C
Optical signal；
6) NH for the 200 μ g/mL for taking step 2 to prepare250 μ L of-BDC-MOF nanometer sheet solution, step 3) prepare 0.1
The uric acid solution of the 10 μ L of uricase solution of U/mL and 50 μ L various concentration same volumes add the neighbour that step 4) prepares 2 mM
50 μ L of phenylenediamine solution is added 40 μ L Tris-HCl (50 mM pH 7.4) buffer and supplements body after four concussion mixing
Product is incubated for 30 minutes at 37 DEG C to 200 μ L, detects the fluorescence signal in the presence of various concentration uric acid, and building fluorescence signal-is dense
The working curve of degree；
7, quantitative analysis is carried out to uric acid in sample according to the fluorescence signal of detection uric acid and working curve.
The results show that system fluorescence intensity is linearly closed with concentration when uric acid concentration is in 0.01 ~ 10 mM concentration range
It is (FL=1699.7-777.61LgCUA, R2=0.993), detection limit is up to 4 μM, as shown in Figure 5.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of preparation method for the fluorescent optical sensor for detecting uric acid, it is characterised in that: include the following steps:
1) the uric acid solution of various concentration unit is prepared；
2) by the two-dimensional metallic organic framework material NH with fluorescent characteristic2- BDC-MOF nanometer sheet is scattered in ultrapure water ultrasonic
30 min, centrifuging and taking supernatant is spare, NH in supernatant2The concentration of-BDC-MOF nanometer sheet is 200 μ g/mL；
3) it takes uricase to be dissolved in three (methylol) aminomethane-hydrochloride buffers and uricase solution is made, stored protected from light
It is spare at 4 DEG C；
4) it takes o-phenylenediamine to be dissolved in three (methylol) aminomethane-hydrochloride buffers and o-phenylenediamine solution is made, be protected from light
Be stored in 4 DEG C it is spare；
5) NH for the 200 μ g/mL for taking step 2 to prepare respectively250 μ L of-BDC-MOF nanometer sheet solution, step 3) prepare 0.1
The 10 μ L of uricase solution and step 4) of U/mL prepare the 50 μ L of o-phenylenediamine solution of 2 mM and add after three is shaken mixing
Enter the Tris-HCl buffer supplement volume of 90 μ L, 50 mM, pH 7.4 to 200 μ L, places 30 minutes, detect at 37 DEG C
Fluorescence signal；
6) NH for the 200 μ g/mL for taking step 2 to prepare250 μ L of-BDC-MOF nanometer sheet solution, step 3) prepare 0.1 U/mL
10 μ L of uricase solution and 50 μ L various concentration same volumes uric acid solution, add step 4) prepare 2 mM adjacent benzene
After four concussion mixing 40 μ L are added, the Tris-HCl buffer of 50 mM pH 7.4 supplements body in 50 μ L of diamine solution
Product is incubated for 30 minutes at 37 DEG C to 200 μ L, detects the fluorescence signal in the presence of various concentration uric acid；
7) according to the fluorescence signal of various concentration uric acid, fluorescence signal-concentration working curve is constructed.
2. the preparation method of the fluorescent optical sensor of detection uric acid according to claim 1, it is characterised in that: described in step 2
Two-dimensional metallic organic framework material NH2The preparation method of-BDC-MOF nanometer sheet, comprising the following steps:
(1) 1.0-3.0 mg neighbour's amino terephthalic acid (TPA) is dissolved in the N that 2.0-5.0 mL volume ratio is 2:1, N- dimethyl methyl
The in the mixed solvent of amide and acetonitrile；
(2) 2.0-4.0 mg Gerhardite is dissolved in the n,N-Dimethylformamide that 2.0-5.0 mL volume ratio is 1:2
With the in the mixed solvent of acetonitrile；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 1.0-3.0 mL volume ratio is 1:1 is prepared as connection
Liquid；
(4) adjacent amino terephthalic acid solution is charged first to the test tube bottom that diameter is 1.0-2.0 cm, capacity is 10-30 mL
Portion adds the connection liquid of 1.0-3.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 30-50 DEG C of water-bath in test tube, is reacted 24-48 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, is done for 60-100 DEG C in vacuum drying oven
It is dry, two-dimensional metallic organic framework material NH is made2- BDC-MOF nanometer sheet.
3. the preparation method of the fluorescent optical sensor of detection uric acid according to claim 2, it is characterised in that: described in step 2
Two-dimensional metallic organic framework material NH2The preparation method of-BDC-MOF nanometer sheet, comprising the following steps:
(1) 1.5 mg neighbour's amino terephthalic acid (TPA)s are dissolved in the n,N-Dimethylformamide and second that 3.0 mL volume ratios are 2:1
The in the mixed solvent of nitrile；
(2) 3.0 mg Gerhardites are dissolved in the n,N-Dimethylformamide and acetonitrile that 3.0 mL volume ratios are 1:2
In the mixed solvent；
(3) mixed solvent of n,N-Dimethylformamide and acetonitrile that 2.0 mL volume ratios are 1:1 is prepared as connection liquid；
(4) adjacent amino terephthalic acid solution is charged first to the test tube bottom that diameter is 1.5 cm, capacity is 25 mL, then plus
The connection liquid for entering 2.0 mL, is eventually adding copper nitrate solution made from step 2；
(5) adjacent amino terephthaldehyde acid layer is heated in 40 DEG C of water-baths in test tube, is reacted 24 hours；
(6) gray product is obtained, washes away n,N-Dimethylformamide and acetonitrile using centrifugation, 80 DEG C of dryings in vacuum drying oven,
Two-dimensional metallic organic framework material NH is made2- BDC-MOF nanometer sheet.
4. a kind of fluorescent optical sensor of preparation method as described in any one of claims 1-3 detection uric acid obtained.
5. a kind of application method of fluorescent optical sensor as claimed in claim 4, it is characterised in that: the following steps are included:
1) NH is taken2- BDC-MOF nanometer sheet solution, uricase solution and o-phenylenediamine solution, after three is shaken mixing, in 37
It is placed 30 minutes at DEG C, detects fluorescence signal；
2) sample solution is added into step 1), is incubated for 30 minutes at 37 DEG C, detects fluorescence signal；
3) fluorescence signal is substituted into fluorescence signal-concentration working curve, obtains uric acid content in sample.
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| CN109507317B (en) * | 2018-11-19 | 2021-05-28 | 中国农业科学院农业质量标准与检测技术研究所 | Sensing application of gallium metal organic framework material in detecting endocrine disruptors |
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