CN107607508A - A kind of method of water soluble fluorescence compound test tervalence gold ion - Google Patents
A kind of method of water soluble fluorescence compound test tervalence gold ion Download PDFInfo
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- CN107607508A CN107607508A CN201710814257.4A CN201710814257A CN107607508A CN 107607508 A CN107607508 A CN 107607508A CN 201710814257 A CN201710814257 A CN 201710814257A CN 107607508 A CN107607508 A CN 107607508A
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- gold ion
- tpcana
- tervalence gold
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Abstract
A kind of method of water soluble fluorescence compound test tervalence gold ion, the tervalence gold ion of various concentrations is detected using the TPCANa aqueous solution, obtains corresponding fluorescence curve；Using tervalence gold ion concentration as abscissa, relative intensity of fluorescence (F0‑F)/F0For ordinate, the standard curve of TPCANa detection tervalence gold ion concentration is obtained；Obtained according to standard curve, in the range of 40~175 μm of ol/L, equation of linear regression is：(F0‑F)/F0=0.00688C 0.28209, when detecting the sample containing tervalence gold ion, the TPCANa aqueous solution detects different fluorescence intensities to the tervalence gold ion of various concentrations, substitutes into equation of linear regression, obtains tervalence gold ion concentration.Identification of the salt that the present invention synthesizes to tervalence gold ion has good selectivity, and the range of linearity is wide, and high sensitivity, synthetic method is simple, while has the advantages that excellent water solubility.
Description
Technical field
The present invention relates to Au3+A kind of detection and analysis technology, and in particular to water soluble fluorescence compound test tervalence gold ion
Method.
Background technology
Gold be used as a kind of noble metal, its numerous areas such as be catalyzed, selective oxidation, nanometer diagnosis and detection have
It is widely applied, while mainly exists in water body in the form of Au (III).Golden simple substance shows as inertia, but in gold salt
Gold ion can be interacted with enzyme and DNA, have potential toxicity to human body, can be to liver, kidney and nervus peripheralis system
System produces infringement, and therefore, high selectivity and the highly sensitive detection method for building tervalence gold ion are extremely important.However, mesh
Preceding existing tervalence gold ion detection method is mainly based upon organic molecule fluorescence probe, and probe building-up process is cumbersome is difficult to for these
A large amount of productions, and most of this kind of probe needs to carry out in organic phase or half aqueous phase, limits it and is examined in tervalence gold ion
Application in survey.
The content of the invention
For deficiency of the prior art, object of the present invention is to provide a kind of water soluble fluorescence compound test three
The method of valency gold ion.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of method of water soluble fluorescence compound test tervalence gold ion, using the TPCANa aqueous solution to various concentrations
Tervalence gold ion is detected, and obtains corresponding fluorescence curve, then, using tervalence gold ion concentration as abscissa, relative fluorescence
Intensity (F0-F)/F0For ordinate, the standard curve of TPCANa detection tervalence gold ion concentration is obtained；Obtained according to standard curve,
In the range of 40~175 μm of ol/L, equation of linear regression is：(F0-F)/F0=0.00688C-0.28209, wherein, C is trivalent
Gold ion concentration, F0For 50 μm of ol/L aqueous solution TPCANa blank control group fluorescence intensities, F is that 50 μm of ol/L TPCANa are water-soluble
Liquid detects the Au of various concentrations3+Fluorescence intensity；
When detecting the sample containing tervalence gold ion, the TPCANa aqueous solution detects not to the tervalence gold ion of various concentrations
Same fluorescence intensity, equation of linear regression is substituted into, obtains tervalence gold ion concentration.
Further improve of the invention is that TPCANa is prepared by the following method：TPCA is added in NaOH solution and obtained
To the TPCANa aqueous solution, the aqueous solution is added in absolute ethyl alcohol, separates out precipitation, is filtered, drying obtains TPCANa.
Further improve of the invention is that the concentration of sodium hydroxide solution is 0.5mol/L~1.0mol/L.
Further improve of the invention is that the volume ratio of the aqueous solution and absolute ethyl alcohol is 1:10.
Further improve of the invention is that TPCA and NaOH mol ratio are 1:1~5.
Further improve of the invention is that TPCA and NaOH mol ratio are 1:3.
Compared with prior art, beneficial effects of the present invention：The present invention is by using the TPCANa aqueous solution to various concentrations
Tervalence gold ion detected, obtain corresponding fluorescence curve, it is then, relatively glimmering using tervalence gold ion concentration as abscissa
Luminous intensity (F0-F)/F0For ordinate, the standard curve of TPCANa detection tervalence gold ion concentration is obtained；Obtained according to standard curve
Arrive, in the range of 40-175 μm of ol/L, equation of linear regression is：(F0-F)/F0=0.00688C-0.28209, wherein, C tri-
Valency gold ion concentration, F0For 50 μm of ol/L aqueous solution TPCANa blank control group fluorescence intensities, F is 50 μm of ol/L TPCANa water
Solution detects the Au of various concentrations3+Fluorescence intensity；When detection contains tervalence gold ion sample, TPCANa fluorescence probes
(the TPCANa aqueous solution) detects to obtain different fluorescence intensities to the tervalence gold ion of various concentrations, substitutes into equation of linear regression,
Obtain tervalence gold ion concentration.Using salt compound as probe in the present invention, the identification to tervalence gold ion has selection well
Property, the range of linearity is wide.Fluorescence probe of the present invention can directly detect Au in aqueous phase3+, without being carried out in organic phase.
Further, TPCANa synthetic method is simple, is reacted in water and then is precipitated in ethanol by TPCA and NaOH
Go out product, products therefrom has excellent water solubility, and synthetic method is nontoxic, cost is low, and fluorescent yield is high, the easily stored fortune of product
It is defeated.
Brief description of the drawings
Fig. 1 is synthetic material TPCANa of the present invention excitation/emission spectrogram.
Fig. 2 is synthetic material TPCANa of the present invention luminescence generated by light figure.
Fig. 3 is synthetic material TPCANa of the present invention and the fluorescent emission figure of tervalence gold ion effect.
Fig. 4 is synthetic material TPCANa of the present invention and various cation sites fluorescence block diagram.
Fig. 5 is fluorescence intensities of the synthetic material TPCANa of the present invention under different pH.
Fig. 6 is the linearity curve that the present invention obtains.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
The present invention prepares TPCANa：TPCA is added in sodium hydrate aqueous solution and reacted, obtains salting liquid, will be molten
Salt solution, which is transferred in the organic solvent under ice-water bath to separate out to precipitate, to be come, and is dried to obtain after filtering at 95-105 DEG C, final salt
Product, i.e. TPCANa, wherein, TPCA and NaOH mol ratio are 1:1~5, preferably 1:3, the concentration of sodium hydrate aqueous solution is
0.5mol/L~1.0mol/L, organic solvent are absolute ethyl alcohol.The aqueous solution of salt compound and the volume ratio of organic solvent are 1:
10.The structural formula of the salt product is as follows：
The method that tervalence gold ion detection is carried out using TPCANa, is comprised the following steps：
A, tervalence gold ion is detected：The 250mL 0.5mmol/L TPCANa aqueous solution is prepared, is diluted to 0-200 μ
Mol/L solution carries out fluoremetry.Specifically the concentration after dilution is：(10μmol/L、20μmol/L、30μmol/L、40μ
Mol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L), this is visited for determination fluorescence
Pin work optium concentration；With the concentration increase of salt compound solution, fluorescence intensity gradually increases, but not linear increase,
There is Fluorescence-quenching.
So the TPCANa aqueous solution that selected concentration is 0.5mmol/L is measured：By the 100 μ L TPCANa aqueous solution
Constant volume is hatched 1h under conditions of 60 DEG C, carried out glimmering to 10mL after (0.5mmol/L) mixes with the tervalence gold ion of various concentrations
Light measurement, as tervalence gold ion concentration increases, the fluorescence intensity at 420nm gradually weakens；Using tervalence gold ion concentration as horizontal stroke
Coordinate, relative intensity of fluorescence (F0–F)/F0For ordinate, the working curve of tervalence gold ion concentration is obtained, in 40~175 μm of ol/
In the range of L, equation of linear regression is：(F0-F)/F0=0.00688C-0.28209, C are tervalence gold ion concentration, unit μ
mol/L。
B, environmental screening：The salt compound aqueous solution, tervalence gold ion is added at different conditions, carry out conditional filtering.
Different condition is：Different pH, other metal cations interference.Concrete operations are as follows：By 100 μ L TPCANa
(0.5mmol/L) is diluted to 10mL, and it is 2~13 to adjust its pH, measures the fluorescent emission intensity at 420nm；By 100 μ L's
TPCANa (0.5mmol/L) and different metal cation mixed diluting to 10mL, measure the fluorescence intensity at 420nm.
Embodiment 1
TPCANa preparation
1.5g TPCA are dissolved into the 20mL NaOH aqueous solution (1mol/L), until completely dissolved, the solution be added dropwise
Into the absolute ethyl alcohol of 200mL ice baths, there is white precipitate precipitation, white precipitate is TPCANa, uses saturated sodium carbonate solution
Precipitation is cleaned, removes remnants TPCA, the powder of gained is filtered, dries, obtains TPCANa.
The TPCANa obtained to embodiment is tested, and obtains excitation/emission spectrogram (Fig. 1), luminescence generated by light figure (figure
2), can be seen that the present invention from Fig. 1 and Fig. 2 and be successfully prepared TPCANa has fluorescence, can be used as fluorescence probe.
TPCANa reacts with gold ion
100 μ L TPCANa (0.5mmol/L) aqueous solution is added to the tervalence gold ion solution of different volumes
In (0.25mmol/L), 10mL is diluted to, carries out fluoremetry, as the increase of tervalence gold ion concentration (is increased to by 0 μm of ol/L
200 μm of ol/L, specific concentration are 0 μm of ol/L, 1 μm of ol/L, 2 μm of ol/L, 4 μm of ol/L, 6 μm of ol/L, 8 μm of ol/L, 10 μm of ol/
L、20μmol/L、40μmol/L、60μmol/L、80μmol/L、100μmol/L、125μmol/L、150μmol/L、175μmol/
L, 200 μm of ol/L), the fluorescent emission intensity at 420nm gradually weakens, and fluorescent emission is shown in Fig. 3.
TPCANa pH response ranges
100 μ L TPCANa (0.5mmol/L) aqueous solution is diluted to 10mL, it is 2~13 to adjust its pH value, is measured
Fluorescent emission intensity at 420nm；It is 2 to 13 to be diluted to 10mL and adjust pH 100 μ L TPCANa (0.5mmol/L), tool
Body, pH value is：2nd, under 3,4,5,6,7,8,9,11,11,12,13, the fluorescence intensity at 420nm is measured, sees Fig. 4.
TPCANa sensitivity detection
By 100 μ L TPCANa (0.5mmol/L) aqueous solution and different metal cation (Ag+、Fe2+(500μmol/
L)、Ca2+、Cu2+、Zn2+、Mg2+、Al3+、Na+、Ba2+、K+、Cd2+、In3+、Sn4+(500μM)、Ce3+(500μM)、Fe3+(500μ
mol/L)、Au3+(100 μm of ol/L), remaining metal cation concentration is 1mmol/L) mixed diluting to 10mL, determines different gold
Belong to the fluorescence intensity block diagram at 420nm corresponding to ion, referring to Fig. 5, experiment shows, other metal ions do not disturb TPCANa
To the measure of tervalence gold ion.
The acquisition of linearity curve
After 100 μ L TPCANa (0.5mmol/L) aqueous solution is mixed with the tervalence gold ion (0.25mM) of different volumes
Constant volume obtains 50 μM of TPCANa and a series of Au to 10mL3+Concentration is hatched (by 0 μM to 200 μM) under conditions of 60 DEG C
After 1h, fluoremetry is carried out, as tervalence gold ion concentration increases, the fluorescence intensity at 420nm gradually weakens；With trivalent gold from
Sub- concentration is abscissa, relative intensity of fluorescence (F0–F)/F0For ordinate, F0It is strong for 50 μM of TPCANa blank control group fluorescence
Degree, F are the Au of 50 μM of TPCANa aqueous assay various concentrations3+Fluorescence intensity, the work for obtaining tervalence gold ion concentration is bent
Line, in the range of 40~175 μm of ol/L, equation of linear regression is：(F0–F)/F0=0.00688C-0.28209, C are trivalent gold
Ion concentration, unit are μm ol/L, and linearity curve is shown in Fig. 6.
When detection contains tervalence gold ion, the TPCANa aqueous solution (50 μm of ol/L) is carried out to the tervalence gold ion of various concentrations
Detection, by the fluorescence intensity detected (in the range of linearity of detection be possible), equation of linear regression is substituted into, obtains trivalent
Gold ion concentration.
Identification of the salt that the present invention synthesizes to tervalence gold ion has good selectivity, and the range of linearity is wide, high sensitivity,
Synthetic method is simple, while has the advantages that excellent water solubility.
Claims (6)
- A kind of 1. method of water soluble fluorescence compound test tervalence gold ion, it is characterised in that using the TPCANa aqueous solution pair The tervalence gold ion of various concentrations is detected, and obtains corresponding fluorescence curve, then, using tervalence gold ion concentration as horizontal seat Mark, relative intensity of fluorescence (F0-F)/F0For ordinate, the standard curve of TPCANa detection tervalence gold ion concentration is obtained；According to mark Directrix curve obtains, and in the range of 40~175 μm of ol/L, equation of linear regression is：(F0-F)/F0=0.00688C-0.28209, its In, C is tervalence gold ion concentration, F0For 50 μm of ol/L aqueous solution TPCANa blank control group fluorescence intensities, F is 50 μm of ol/ The Au of LTPCANa aqueous assay various concentrations3+Fluorescence intensity；When detecting the sample containing tervalence gold ion, the TPCANa aqueous solution detects to obtain difference to the tervalence gold ion of various concentrations Fluorescence intensity, substitute into equation of linear regression, obtain tervalence gold ion concentration.
- A kind of 2. method of water soluble fluorescence compound test tervalence gold ion according to claim 1, it is characterised in that TPCANa is prepared by the following method：TPCA is added in NaOH solution and obtains the TPCANa aqueous solution, the aqueous solution is added Into absolute ethyl alcohol, precipitation is separated out, is filtered, drying obtains TPCANa.
- A kind of 3. method of water soluble fluorescence compound test tervalence gold ion according to claim 2, it is characterised in that The concentration of sodium hydroxide solution is 0.5mol/L~1.0mol/L.
- A kind of 4. method of water soluble fluorescence compound test tervalence gold ion according to claim 2, it is characterised in that The volume ratio of the aqueous solution and absolute ethyl alcohol is 1:10.
- A kind of 5. method of water soluble fluorescence compound test tervalence gold ion according to claim 2, it is characterised in that TPCA and NaOH mol ratio is 1:1~5.
- A kind of 6. method of water soluble fluorescence compound test tervalence gold ion according to claim 5, it is characterised in that TPCA and NaOH mol ratio is 1:3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110305035A (en) * | 2019-07-03 | 2019-10-08 | 云南民族大学 | A kind of full nh 2 column [5] aromatic hydrocarbons and its synthetic method and the application in detection tervalence gold ion |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818016A (en) * | 2015-05-25 | 2015-08-05 | 西南大学 | Novel method for detecting trivalent gold ions |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818016A (en) * | 2015-05-25 | 2015-08-05 | 西南大学 | Novel method for detecting trivalent gold ions |
Non-Patent Citations (3)
| Title |
|---|
| LEI SHI ET AL: "Carbon dots with high fluorescent quantum yield: the fluorescence originates from organic fluorophores", 《NANOSCALE》 * |
| 刘通秀等: "金(III)离子荧光探针的研究进展", 《中国科学》 * |
| 蔡菲: "功能化石墨烯量子点的分析应用研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110305035A (en) * | 2019-07-03 | 2019-10-08 | 云南民族大学 | A kind of full nh 2 column [5] aromatic hydrocarbons and its synthetic method and the application in detection tervalence gold ion |
| CN110305035B (en) * | 2019-07-03 | 2022-06-17 | 云南民族大学 | Total amino column [5] arene, synthetic method thereof and application thereof in detection of trivalent gold ions |
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