CN109307668A - Application of the porous metals organic coordination compound as probe in fluorescence detection aluminium ion - Google Patents
Application of the porous metals organic coordination compound as probe in fluorescence detection aluminium ion Download PDFInfo
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- 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
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- 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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- 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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Abstract
A kind of application the invention discloses porous metals organic coordination compound as probe in fluorescence detection aluminium ion, the structural unit of the complex are [(CH3)2NH2][Mg3(OH)(DHBDC)3(PTP)], DHBDC represents 2,5-Dihydroxyterephthalic acid dianion, and PTP represents 4 '-(4- pyridine) -4,2 ': 6 ', 4 "-terpyridyls.The complex is within the scope of 0~1.2 μm of ol/L, fluorescence intensity increases with aluminium ion concentration and is weakened, the state of fluorescent quenching is presented, increase fluorescence intensity with aluminium ion concentration within the scope of 4.2~15 μm of ol/L to gradually increase, the state of fluorescence enhancement is presented, aluminium ion is detected, fluorescence " on/off " effect is presented, detection limit can achieve 28nmol/L.The complex is made into test paper, aluminum ions presence, the test paper after recycling detection aluminium ion can be obviously distinguished under ultraviolet lamp, with N, after N- dimethyl acetamide is impregnated, the fluorescence spectrum of the test paper and the color under ultraviolet lamp revert to initial spectrum and color, have fine recycling.
Description
Technical field
The invention belongs to aluminum ions detection technique fields, and in particular to a kind of to use the conduct of porous metals organic coordination compound
Application of the probe in fluorescence detection aluminium ion.
Background technique
Aluminium is the third element that content is only second to oxygen, silicon in the earth's crust.Aluminum metal and its alloy are due to corrosion-resistant, close
Spending the advantages that small, thermal conductivity is good and ductility is good is widely used in every profession and trade.Minute quantity Al3+Human body will not be caused
Harm, but excessive Al3+It is larger to the harm of human body.Though the harm of the ion known to most people, is not affected by foot
Enough attention.Al3+Can be in conjunction with protein, coup injury central nervous system, aluminium accumulate in brain can cause it is cerebral neural
It degenerates, memory loss, intelligence and personality also will receive influence, or even senile dementia is presented.Therefore, to aluminum ions detection
In terms of environmental protection and human health, tool has very important significance.The World Health Organization studies have shown that human body per kilogram body
Weight allows the aluminium taken in no more than 1mg daily.
Currently, Al3+Detection method mainly include atomic absorption spectrography (AAS), atom luminescence spectroscopy, electrochemical method and
Chromatography etc., these methods usually have good sensitivity and repeatability, but there is also expensive equipment, detection it is time-consuming,
The disadvantages of cumbersome.Fluorescent spectrometry has the good, high sensitivity of selectivity, accuracy high and does not destroy biological sample etc. because of it
Advantage and be concerned.But since aluminium ion is as a kind of hard acid, coordination ability relatively transition metal Zn and Cd is weak very much,
So that it is hardly formed certain spectral signature, and this also affects fluorescence to Al3+The development of detection technique.
And coordination polymer is as a kind of most promising crystalline material, can by reasonably select metal from
Son and organic ligand, regulate and control the influence factor of reaction, reach the coordination of prediction and design some properties and structure
Polymer.In particular, some functional groups present in some open pore structures can pass through electrostatic, Lewis Acids and Bases effect, hydrogen
The sensing capabilities of such material of the reinforcement such as key.
Summary of the invention
The purpose of the present invention is provide a kind of new application for porous metals organic coordination compound.
Application of the porous metals organic coordination compound of the present invention as probe in fluorescence detection aluminium ion, wherein described porous
The structural unit of metal organic complex is [(CH3)2NH2][Mg3(OH)(DHBDC)3(PTP)], DHBDC representative sloughs two in formula
The 2,5-Dihydroxyterephthalic acid dianion of the upper hydrogen atom of a-COOH, PTP represent 4'- (4- pyridine) -4,2':6',
4 "-terpyridyl；The complex belongs to hexagonal crystal system, P6 (3)/mmc space group, and cell parameter isα=90 °, β=90 °, γ=120 °；The complex is according to announcement
Number for CN 108570062A application for a patent for invention disclosed in method be prepared.
Porous metals organic coordination compound of the present invention has good sensing capabilities to aluminium ion, can be used as probe for fluorescence
Detect aluminium ion, the method for qualitative detection are as follows: porous metals organic coordination compound is dispersed in n,N-dimethylacetamide
In, compound concentration is the complex suspension of 1~4mg/mL, then impregnates 1~2 minute filter paper in gained suspension, takes
Filter paper is put 40 DEG C of drying, filter paper in a vacuum drying oven and is placed in dark compartment out, testing sample solution is sprayed on filter paper, if filter paper
Color becomes sapphirine, illustrates to contain aluminium ion in testing sample solution.
Application of the porous metals organic coordination compound of the present invention as probe in fluorescence detection aluminium ion, quantitative detection side
Method are as follows:
1, porous metals organic coordination compound is dispersed in n,N-dimethylacetamide, compound concentration is 1~4mg/
Then various concentration aluminium ion standard sample is added, using fluorescence spectrophotometer light in the complex suspension of mL into gained suspension
Degree meter detection various concentration aluminium ion corresponds to the fluorescence spectrum of system；When aluminium ion concentration is not more than 1.2 μm of ol/L, aluminium is drawn
Ion concentration is with I/I0The standard curve of variation, wherein I0It is that fluorescence intensity of the system at 505nm, I are when not adding aluminium ion
Corresponding body ties up to the fluorescence intensity at 505nm after adding the aluminium ion of various concentration；When aluminium ion concentration is 4.2~15 μm of ol/L
When, aluminium ion concentration is drawn with I'/I4.2The standard curve of variation, wherein I4.2It is corresponding when be aluminium ion concentration being 4.2 μm of ol/L
Fluorescence intensity of the system at 460nm, I' are that the fluorescence that ties up at 460nm of corresponding body is strong after the aluminium ion for adding various concentration
Degree.
2, the fluorescence spectrum of aluminium ion sample to be measured is measured with Fluorescence Spectrometer according to the method for step 1, if its maximum is glimmering
Light intensity peak is at 505nm, in conjunction with aluminium ion concentration in step 1 with I/I0The linear equation of the standard curve of variation calculates to be measured
Aluminum ions concentration in sample；If its maximum fluorescence intensity peak is at 460nm, in conjunction with aluminium ion concentration in step 1 with I'/I4.2
The linear equation of the standard curve of variation calculates aluminum ions concentration in sample to be tested.
Beneficial effects of the present invention are as follows:
1, porous metals organic coordination compound selection of the present invention has redox and is capable of intramolecular generation proton translocation
2,5-Dihydroxyterephthalic acid chooses the 4'- (4- pyridine) -4,2' with big conjugation as major ligand:
6', 4 "-terpyridyl is inserted into as second of ligand, is made in gained complex hole with-OH and with excited state molecule proton
Transfer performance, since-OH is strong lewis base, and Al3+As strong lewis acid, according to coordination principle, in complex hole
- OH and aluminium ion have good coordination ability, and then to aluminium ion have good selective enumeration method ability.
2, porous metals organic coordination compound of the present invention has the characteristics that " on-off " to aluminium ion fluorescence detection, can visually sentence
Break aluminum ions concentration range, and in numerous metal ions, there is selectivity well to aluminium ion, have to aluminium ion
Very low detection limit and apparent color change, detection limit can achieve 28nmol/L, be a kind of detection aluminium ions well
Probe.
3, porous metals organic coordination compound of the present invention can be made test paper, can obviously distinguish in the UV lamp aluminum ions
In the presence of effect of the more convenient realization scene to aluminium ion response.It will test the test paper recycling after aluminium ion, be used in combination
After n,N-dimethylacetamide is impregnated, the fluorescence spectrum of the test paper recycled and the color under ultraviolet lamp revert to initial
Spectrum and color can be used as test paper again, have fine recycling.
Detailed description of the invention
Fig. 1 is that different metal ions are added in complex and the suspension that DMAC N,N' dimethyl acetamide is formed is corresponding glimmering
Light spectrogram.
Fig. 2 is that different metal ions are added in complex and the suspension that DMAC N,N' dimethyl acetamide is formed is corresponding glimmering
Intensity ratio.
Fig. 3 is that the ultraviolet light irradiation of different metal ions is added in complex and the suspension of DMAC N,N' dimethyl acetamide formation
Under corresponding color diagram.
Fig. 4 is that complex is corresponding with the aluminium ion of various concentration is added in the suspension that DMAC N,N' dimethyl acetamide is formed
Fluorescence spectra.
Fig. 5 is in complex CIE coordinate corresponding with the suspension that DMAC N,N' dimethyl acetamide is formed and addition aluminium ion
Color change figure.
Fig. 6 is that complex is corresponding with the aluminium ion of various concentration is added in the suspension that DMAC N,N' dimethyl acetamide is formed
Fluorescence maximum emission peak strength straight line fitted figure.
Fig. 7 is purple after the suspension that complex and DMAC N,N' dimethyl acetamide are formed and the aluminium ion that various concentration is added
Corresponding color change figure under outer light irradiation.
Fig. 8 is corresponding color change figure under ultraviolet light irradiation after being sprayed into different metal ions on complex test paper.
Fig. 9 is that corresponding color becomes under complex solid spray aluminium ion solution and the ultraviolet light irradiation for being repeated 3 times sprinkling
Change figure.
Figure 10 is complex solid spray aluminium ion solution and is repeated 3 times later X-ray diffraction comparison chart.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1, test of the complex to aluminium ion selection performance
By the finely ground rear ultrasonic disperse of 50mg porous metals organic coordination compound mortar in 50mL DMAC N,N' dimethyl acetamide
In, it is configured to the complex suspension that concentration is 1mg/mL, the suspension is under the excitation of maximum excitation wavelength 362nm, most
Big emission peak is at 505nm.
It takes the complex suspension of 3mL 1mg/mL to be added in 4mL cuvette, 30 μ L is added into cuvette respectively
0.001mol/L Li(NO3)、Mn(NO3)2、Zn(NO3)2、Cd(NO3)2、Co(NO3)2、Ni(NO3)2、Cu(NO3)2、Pb(NO3)2、
Al(NO3)3、Cr(NO3)3、Ga(NO3)3、In(NO3)3、Fe(NO3)3、Nd(NO3)3、Er(NO3)3、Y(NO3)3N, N- dimethyl
Acetamide solution uses sepectrophotofluorometer in the case where excitation wavelength is 362nm, and fixed slit width is 3nm, tests different gold
Belong to the fluorescence spectrum that ion pair answers system.By Fig. 1 and 2 as it can be seen that the complex to aluminum ions fluorescent effect obviously with others
Metal ion is different, and aluminium ion has the phenomenon that apparent blue shift and fluorescence enhancement, illustrates that the complex has very aluminium ion
Good selectivity；It takes pictures in the UV lamp to it, it can also be seen that different colors is presented in different metal ions (see Fig. 3).
2, complex is to aluminum ions quantitative test
The Al of various concentration is added in the complex suspension that concentration is 1mg/mL3+(0、0.3、0.6、0.9、1.2、
1.5,1.8,3,4.2,5.4,6.6,7.8,9,10.2,11.4,12.6,13.8 and 15 μm of ol/L), using sepectrophotofluorometer
In the case where excitation wavelength is 362nm, fixed slit width is 3nm, and test various concentration aluminium ion corresponds to the fluorescence spectrum of system.By
Fig. 4 is as it can be seen that in 0~1.2 μm of ol/L concentration range, with Al3+The increase of concentration, fluorescence maximum emission peak is with concentration
Increase and gradually decrease, the state of fluorescent quenching is presented, and works as Al3+Concentration when reaching 1.2 μm of ol/L, maximum emission peak
Offset takes place in position, and in 1.2~4.2 μm of ol/L concentration ranges, the position of maximum emission peak and intensity are with Al3+Concentration
Change less stable, works as Al3+Concentration to 4.2 μm of ol/L after, maximum emission peak is displaced at 460nm, and later with
Al3+The increase of concentration, fluorescence intensity are also gradually increasing, and the state of fluorescence enhancement is presented.Pass through matching for test 1mg/mL
The transmitting peak data of object suspension is closed, and Al is added3+The emission peak that blue shift occurs afterwards, which is brought on CIE chromaticity coordinates, to be calculated, can
To see apparent color change (see Fig. 5), while to the Al that various concentration is added3+Solution is taken pictures in the UV lamp, can also be with
It is clearly visible fluorescence gradual quenching at green light 505nm, and gradually increasing at blue light 460nm.
As seen from Figure 6, in 0~1.2 μm of ol/L and 4.2~15 μm of ol/L concentration range, aluminium ion concentration and fluorescence are strong
Degree has good linear relationship, carries out linear fit to it, meets linear equation in 0~1.2 μm of ol/L concentration range: I/
I0=0.98992-0.2422 [Al3+], linear fit constant R2=0.99, meet in 4.2~15 μm of ol/L concentration ranges straight
Line equation: I/I4.2=-0.47028+0.36685 [Al3+], linear fit constant R2=0.99, wherein I is the aluminium of various concentration
Ion pair answers the fluorescence intensity of system, I0It is the corresponding fluorescence intensity of system, I when aluminium ion is not added4.2It is that aluminium ion concentration is
The fluorescence intensity of system, [Al are corresponded to when 4.2 μm of ol/L3+] refer to aluminum ions concentration.
Meanwhile acquired solution after the complex suspension of 1mg/mL and addition various concentration aluminium ion being put into dark compartment and is used
Ultraviolet light irradiation, it can be seen that apparent color change, such as Fig. 7 has occurred in it.
3, test of the complex test paper to aluminium ion selectivity and reusability
Filter paper is impregnated into 1~2min in the complex suspension of 1mg/mL, taking-up is placed in a vacuum drying oven 40 DEG C of bakings
It is dry, filter paper is placed in dark compartment later, the Li (NO that will be prepared using n,N-dimethylacetamide as solvent3)、Mn(NO3)2、Zn
(NO3)2、Cd(NO3)2、Co(NO3)2、Ni(NO3)2、Pb(NO3)2、Al(NO3)3、Cr(NO3)3、Ga(NO3)3、In(NO3)3、Fe
(NO3)3、Nd(NO3)3、Er(NO3)3、Y(NO3)3Solution is sprayed above respectively, it can be seen that the color of filter paper changes, and aluminium
Ion is obviously different from other metal ions, is more bright blue (such as Fig. 8), this also with above test 1 test result phase
Meet.
Al (NO is directly sprayed to solid porous metals organic coordination compound sample3)3Solution, under ultraviolet lamp it can also be seen that
Solid sample is sprayed Al (NO to probe into whether it has reusability by the difference of color before and after solid sample3)3Solution
Afterwards, it then is immersed in n,N-dimethylacetamide and exchanges 3~5 times, later again dry up sample, it is seen that the organic cooperation of porous metals
Object can restore its original color sample, if spraying Al (NO again3)3Color change can occur again, be repeated in three for solution
Secondary sample is all unaffected (such as Fig. 9), and powder-X-ray diffractometer test curve, which also illustrates the complex still, has good knot
Crystalline substance (such as Figure 10) illustrates that the complex has good reusability.
Claims (3)
1. application of the porous metals organic coordination compound as probe in fluorescence detection aluminium ion, it is characterised in that: described is more
The structural unit of mesoporous metal organic coordination compound is [(CH3)2NH2][Mg3(OH)(DHBDC)3(PTP)], DHBDC representative is sloughed in formula
The 2,5-Dihydroxyterephthalic acid dianion of the upper hydrogen atom of two-COOH, PTP represent 4'- (4- pyridine) -4,2':6',
4 "-terpyridyl；The complex belongs to hexagonal crystal system, P6 (3)/mmc space group, and cell parameter isα=90 °, β=90 °, γ=120 °.
2. application of the porous metals organic coordination compound according to claim 1 as probe in fluorescence detection aluminium ion,
It is characterized in that specific detection method are as follows: porous metals organic coordination compound is dispersed in n,N-dimethylacetamide, is matched
Concentration processed is the complex suspension of 1~4mg/mL, then impregnates filter paper 1~2 minute in gained suspension, takes out filter paper
It is placed on after vacuum drying in dark compartment, testing sample solution is sprayed on filter paper, if filter paper color becomes sapphirine, illustrated to test sample
Contain aluminium ion in product solution.
3. application of the porous metals organic coordination compound according to claim 1 as probe in fluorescence detection aluminium ion,
It is characterized in that specific detection method are as follows:
(1) porous metals organic coordination compound is dispersed in n,N-dimethylacetamide, compound concentration is 1~4mg/mL's
Then various concentration aluminium ion standard sample is added, using sepectrophotofluorometer in complex suspension into gained suspension
Detection various concentration aluminium ion corresponds to the fluorescence spectrum of system；When aluminium ion concentration is not more than 1.2 μm of ol/L, aluminium ion is drawn
Concentration is with I/I0The standard curve of variation, wherein I0It is fluorescence intensity of the system at 505nm when not adding aluminium ion, I is addition
Corresponding body ties up to the fluorescence intensity at 505nm after the aluminium ion of various concentration；When aluminium ion concentration is 4.2~15 μm of ol/L,
Aluminium ion concentration is drawn with I'/I4.2The standard curve of variation, wherein I4.2Be aluminium ion concentration be 4.2 μm of ol/L when correspond to system
Fluorescence intensity at 460nm, I' are that corresponding body ties up to fluorescence intensity at 460nm after the aluminium ion for adding various concentration；
(2) fluorescence spectrum for measuring aluminium ion sample to be measured with Fluorescence Spectrometer according to the method for step (1), if its maximum fluorescence
Intensity peak is at 505nm, in conjunction with aluminium ion concentration in step (1) with I/I0The linear equation of the standard curve of variation calculates to be measured
Aluminum ions concentration in sample；If its maximum fluorescence intensity peak at 460nm, in conjunction with aluminium ion concentration in step (1) with I'/
I4.2The linear equation of the standard curve of variation calculates aluminum ions concentration in sample to be tested.
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| CN110044884A (en) * | 2019-04-11 | 2019-07-23 | 华南理工大学 | A kind of Test paper of divalent manganesetion and the preparation method and application thereof |
| CN110330660A (en) * | 2019-06-11 | 2019-10-15 | 河北科技大学 | A kind of preparation method and applications of the rare-earth europium hybrid luminescent materials with aluminium ion sensing capabilities |
| CN111253586A (en) * | 2020-03-09 | 2020-06-09 | 重庆师范大学 | Cadmium-based metal-organic framework material and preparation method and application thereof |
| CN113666822A (en) * | 2021-08-24 | 2021-11-19 | 桂林医学院 | Small molecule fluorescent probe for aluminum ion detection and cell imaging and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044884A (en) * | 2019-04-11 | 2019-07-23 | 华南理工大学 | A kind of Test paper of divalent manganesetion and the preparation method and application thereof |
| CN110330660A (en) * | 2019-06-11 | 2019-10-15 | 河北科技大学 | A kind of preparation method and applications of the rare-earth europium hybrid luminescent materials with aluminium ion sensing capabilities |
| CN110330660B (en) * | 2019-06-11 | 2021-07-20 | 河北科技大学 | Preparation method and application of rare earth europium hybrid luminescent material with aluminum ion sensing performance |
| CN111253586A (en) * | 2020-03-09 | 2020-06-09 | 重庆师范大学 | Cadmium-based metal-organic framework material and preparation method and application thereof |
| CN111253586B (en) * | 2020-03-09 | 2021-10-26 | 重庆师范大学 | Cadmium-based metal-organic framework material and preparation method and application thereof |
| CN113666822A (en) * | 2021-08-24 | 2021-11-19 | 桂林医学院 | Small molecule fluorescent probe for aluminum ion detection and cell imaging and application thereof |
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Application publication date: 20190205 |