CN103323450B - Rapid determination method of iodide ion by using nano-gold as logic gate developing probe - Google Patents
Rapid determination method of iodide ion by using nano-gold as logic gate developing probe Download PDFInfo
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- CN103323450B CN103323450B CN201310215000.9A CN201310215000A CN103323450B CN 103323450 B CN103323450 B CN 103323450B CN 201310215000 A CN201310215000 A CN 201310215000A CN 103323450 B CN103323450 B CN 103323450B
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- iodide ion
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Abstract
The invention discloses a rapid determination method of iodide ion by using nano-gold as a logic gate developing probe. Thiocyanate can prevent aggregation of nano-gold in an acidic solution and make the acidic solution maintain claret-red, and iodide ion can specifically inhibit thiocyanate from protecting nano-gold so as to perform changes of solution color and ultraviolet absorption spectrum characteristic. Detection limit under visual observation is 0.8 micromol/L. Linearity range measured by absorbance ratio is 0.2-1.6micromol/L, and detection limit is 0.05micromol/L. After simple pretreatment of a water sample, the method can be adopted to rapidly determine the content of iodide ion therein. In addition, the nano-gold used in the invention is directly obtained by reducing chloroauric acid by sodium citrate without further modification. The preparation process is simple and rapid.
Description
Technical field
The present invention relates to nm of gold the quick content assaying method of the iodide ion being logic gate colour developing probe, belong to analytical chemistry and field of nanometer technology.
Background technology
Along with the development of nanometer technology, the nano material of numerous species, such as, metal nano material, oxide-based nanomaterial, semiconductor nano material and electrical-conductive nanometer polymkeric substance etc. are extensively applied to chemistry and field of biosensors.In all nano materials, golden nanometer particle (Gold nanoparticles, GNPs) is easy to prepare due to it and the spectral characteristic of biological functional, excellent biological stability and uniqueness receives the concern of researchers most.Typical gold colloidal nanaparticles is claret, and their aggregation then presents purple or blueness, and this is caused by the surface plasma absorption band of nm of gold moves to long wavelength.Nm of gold makes it be very suitable for logic gate Color Appearance System by being distributed to the quick change of color in state of aggregation process.In recent years, use the methods such as DNAzyme method, aptamer method, ligands method, established many logic gate color development system based on nm of gold and be successfully applied to the analysis of some metallic ions and small-molecule substance.
Iodine is one of trace element of needed by human, can participate in the synthesis of thyroid hormone, the g and D of regulation and control human body.Research shows, may cause Thyroid Gland Swell, nanism, miscarriage, amentia, myasthenia etc. during iodine uptake quantity not sufficient; The thyroid gland generation enlargement of some specific crowd may be caused when iodine uptake amount is excessive.Therefore, the Nutritive evaluation of the content of iodine in biological, the environment of Accurate Determining and food to human health status analysis, environmental assessment and food has very important practical significance.Establish the analytical approach of some iodine at present both at home and abroad, comprise photometry, electrochemical process, chromatography, neutron activation method and atomic spectroscopy etc.But the determination step of these methods is comparatively loaded down with trivial details, and need some specific instruments to assist, be therefore difficult to be applied in detection in real time.
The present invention is with thiocyanate (SCN
-) and iodide ion (I
-) two kinds of negative ion as input signal, using the standby nm of gold of reduction of sodium citrate legal system as colour developing probe, construct one and have the logic gate of " containing " behavior, i.e. " OR NOT gate ", and be applied to the mensuration of Trace Iodine.
Summary of the invention
The object of the invention is to develop the color probe for logic gate with the standby nm of gold of reduction of sodium citrate legal system, provide a kind of quick, easy, sensitive iodide ion new detecting method.
To achieve these goals, the present invention is by the following technical solutions:
of the present invention take nm of gold as the rapid assay methods of iodide ion of logic gate colour developing probeit is characterized in that nm of gold being stoped to produce gathering in an acidic solution based on thiocyanate, make it keep claret, and the specific suppression thiocyanate of iodide ion energy is to the protective effect of nm of gold; thus show the change of solution colour and ultra-violet absorption spectrum feature, come
measure iodide ion concentration.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that utilizing visualization solution colour feature to judge the concentration of iodide ion.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that utilizing absorbance ratio A
700/ A
520to judge the concentration of iodide ion.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that used nm of gold adopts the method preparation of reduction of sodium citrate gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliters of 0.1g/L, reaction solution becomes claret from light yellow, continue backflow after 15 minutes, reaction solution is slowly cooled to room temperature and forms nm of gold.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that 5:4 is by nano-Au solution with containing the mixing of variable concentrations iodide ion solution by volume, adding 0.05 ml concn is 8 ~ 10 mmol/L sulfuric acid solutions, containing the thiocyanate of 2.5 ~ 3 μm of ol/L in 8 ~ 10 described mmol/L sulfuric acid solutions, react 3 ~ 5 minutes at 30 DEG C, visualization color characteristic or mensuration absorbance ratio A
700/ A
520, when visualization color characteristic along with the increase of iodide ion concentration, the color of nm of gold becomes aubergine-purple-pewter from redness gradually, and the detection of visualization is limited to 0.8 μm of ol/L; As mensuration absorbance ratio A
700/ A
520time, the absorbance ratio A along with the increase of iodide ion concentration
700/ A
520increase gradually, A within the scope of 0.2 ~ 1.6 μm of ol/L
700/ A
520linear with iodide ion concentration, detect and be limited to 0.05 μm of ol/L.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.1 nmol/L.
Described
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that 5:4 is by nano-Au solution with containing the mixing of variable concentrations iodide ion solution by volume, add 0.05 milliliter of 8 mmol/L sulfuric acid solution, containing the thiocyanate of 2.5 μm of ol/L in 8 described mmol/L sulfuric acid solutions, react 3 minutes at 30 DEG C, visualization color characteristic or mensuration absorbance ratio A
700/ A
520to judge the concentration of iodide ion; Nano-Au solution and be respectively 0.25 milliliter and 0.20 milliliter containing the volume of variable concentrations iodide ion solution.
the iodide ion method taking nm of gold as logic gate and develop the color in probe Fast Measurement water sample of the present invention, comprise the steps: in the water sample of 10 milliliters, to add the ethylenediamine tetraacetic acid that final concentration is 0.5 mmol/L, after 0.22 μm of membrane filtration, obtain sample solution; 0.20 milliliter of above-mentioned sample solution and 0.05 milliliter of 8 mmol/L sulfuric acid is added in 0.25 milliliter of nm of gold, containing the thiocyanate of 2.5 μm of ol/L in 8 described mmol/L sulfuric acid solutions, react 3 minutes at 30 DEG C, the change of then visualization color or mensuration absorbance ratio A
700/ A
520, according to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve, obtain
the content of the iodide ion in water sample.
Described
take nm of gold as the iodide ion method in logic gate colour developing probe Fast Measurement water sampleit is characterized in that used nm of gold adopts the method preparation of reduction of sodium citrate gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliter of 0.1 g/L, reaction solution becomes claret from light yellow, continue backflow after 15 minutes, reaction solution is slowly cooled to room temperature and forms nm of gold.
Described
take nm of gold as the iodide ion method in logic gate colour developing probe Fast Measurement water sample, it is characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.1 nmol/L.
The present invention is concrete by the following technical solutions:
(1) preparation of nm of gold
The all glasswares used in following process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.The preparation of nm of gold: the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliter of 0.1 g/L, reaction solution becomes claret by from light yellow, continues backflow after 15 minutes, reaction solution is slowly cooled to room temperature.The nm of gold particle diameter of gained is 13 nm, and concentration is about 3.1 nmol/L, 4 DEG C of preservations.
(2) mensuration of iodide ion
Nano-Au solution prepared by 0.25 milliliter of step () is added in 0.20 milliliter of iodide ion sample solution, then 0. 05 milliliter of 8 mmol/L(final concentration is added, lower same) sulfuric acid (being the thiocyanate of 2.5 μm of ol/L containing final concentration), 30 DEG C of reactions 5 minutes after mixing, the change of visualization color or the absorbance ratio (A at mensuration 700 nm and 520 nm wavelength places
700/ A
520).According to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve.The detection of visualization is limited to 0.8 μm of ol/L, and the detection of dulling luminosity ratio pH-value determination pH is limited to 0.05 μm of ol/L.
Advantage of the present invention:
(1) the present invention is based on thiocyanate can stop nm of gold to produce gathering in an acidic solution; it is made to keep claret; and the specific suppression thiocyanate of iodide ion energy is to the protective effect of nm of gold; thus show the change of solution colour and ultra-violet absorption spectrum feature, the content detection of iodide ion can be directly used in.
(2) nm of gold used in the present invention is directly obtained by reduction of sodium citrate gold chloride, and without the need to further modifying, preparation process is simple and quick.
(3) processing requirements of the present invention to sample is low, and anti-interference is good, only needs to add after ethylenediamine tetraacetic acid is sheltered to measure in water sample.
(4) detection speed of the present invention is fast, can complete pre-service and the detection of actual water sample in 3 minutes.
(5) detection sensitivity of the present invention is high, and the detection changed by visual color is limited to 0.8 μm of ol/L, and the detection of dulling luminosity ratio pH-value determination pH is limited to 0.05 μm of ol/L.
Accompanying drawing explanation
Fig. 1 is nm of gold absorbance ratio (A after varying input signal effect under 8 mmol/L sulfuric acid conditions
700/ A
520) change and respective color variation diagram (illustration).(0,0) represents not thiocyanate and iodide ion, and color is pewter; (0,1) represents thiocyanate, and not containing iodide ion, color is pewter; (1,0) represents containing iodide ion, not thiocyanate, and color is red; (1,1) represents thiocyanate and iodide ion, and color is pewter.Wherein thiocyanate concn is 2.5 μm of ol/L, and iodide ion concentration is 2 μm of ol/L.
Fig. 2 is the absorbance ratio figure under variable concentrations sulfuric acid condition after nm of gold and iodide ion effect.Wherein thiocyanate concn is 2.5 μm of ol/L.
Fig. 3 is the absorbance ratio figure under variable concentrations thiocyanate condition after nm of gold and iodide ion effect.Wherein sulfuric acid concentration is 8 mmol/L.
Fig. 4 is 8 mmol/L sulfuric acid, absorbance ratio under 2.5 μm of ol/L thiocyanate conditions after nm of gold and the effect of variable concentrations iodide ion is schemed over time.
Fig. 5 is the color variation diagram under 8 mmol/L sulfuric acid, 2.5 μm of ol/L thiocyanate conditions after nm of gold and the effect of variable concentrations iodide ion.Concrete color change is from left to right shown as, and when not containing iodide ion, solution is aobvious red; When iodide ion concentration is 0.8 μm of ol/L, solution displaing amaranth; When iodide ion concentration is 1.6 μm of ol/L, solution shows purple; When iodide ion concentration is 2.4 μm of ol/L, solution shows pewter.
Fig. 6 is the absorbance ratio variation diagram under 8 mmol/L sulfuric acid, 2.5 μm of ol/L thiocyanate conditions after nm of gold and the effect of variable concentrations iodide ion.
Fig. 7 is the absorbance ratio (A of nm of gold under 8 mmol/L sulfuric acid, 2.5 μm of ol/L thiocyanate conditions
700/ A
520) with the linear relationship chart of iodide ion concentration.
Embodiment
Embodiment 1:
The chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliter of 0.1 g/L, reaction solution becomes claret from light yellow, continues backflow after 15 minutes, reaction solution is slowly cooled to room temperature.The nm of gold particle diameter of gained is 13 nm, and concentration is about 3.1 nmol/L, 4 DEG C of preservations.The all glasswares used in above process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.
Embodiment 2:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.05 milliliter of 8 mmol/L sulfuric acid and 0.2 ml distilled water, 30 DEG C are reacted 5 minutes.When iodide ion and thiocyanate all do not contain, or only containing iodide ion, and iodide ion and thiocyanate all containing time, namely under (0,0), (0,1), (1,1) three kinds of states, nm of gold sedimentation, color becomes indigo plant, absorbance ratio A
700/ A
520greatly; When sulf onyl cyanate, namely under (1,0) state, there is not sedimentation in nm of gold, color remains unchanged, absorbance ratio A
700/ A
520little (see figure 1).
Embodiment 3:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 ml distilled water and 0.05 milliliter of variable concentrations (final concentration is 0 ~ 10 mmol/L) sulfuric acid (thiocyanates containing 2.5 μm of ol/L), 30 DEG C are reacted 5 minutes, measure absorbance ratio A
700/ A
520.As shown in Figure 2, Δ A
700/ A
520reach maximum when sulfuric acid final concentration is 8 mmol/L.
Embodiment 4:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 ml distilled water and 0.05 milliliter of 8 mmol/L sulfuric acid (being the thiocyanate of 0 ~ 3 μm of ol/L containing final concentration), 30 DEG C are reacted 5 minutes, measure absorbance ratio A
700/ A
520.As shown in Figure 3, Δ A
700/ A
520reach maximum when thiocyanate final concentration is 2.5 μm of ol/L.
Embodiment 5:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 ml distilled water and 0.05 milliliter of 8 mmol/L sulfuric acid (thiocyanates containing 2.5 μm of ol/L), 30 DEG C are reacted 0 ~ 5 minute, measure absorbance ratio A
700/ A
520.As shown in Figure 4, absorbance ratio A
700/ A
520reach maximum after 3 minutes.
Embodiment 6:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 ml distilled water and 0.05 milliliter of 8 mmol/L sulfuric acid (thiocyanates containing 2.5 μm of ol/L), 30 DEG C are reacted 3 minutes, and the change of visualization color, result as shown in Figure 5.When not containing iodide ion, solution is aobvious red; When iodide ion concentration is 0.8 μm of ol/L, solution displaing amaranth; When iodide ion concentration is 1.6 μm of ol/L, solution shows purple; When iodide ion concentration is 2.4 μm of ol/L, solution shows pewter.
Embodiment 7:
In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 ml distilled water and 0.05 milliliter of 8 mmol/L sulfuric acid (thiocyanates containing 2.5 μm of ol/L), 30 DEG C are reacted 3 minutes, measure absorbance ratio A
700/ A
520.As shown in Figure 6, absorbance ratio A
700/ A
520increase with the increase of iodide ion concentration, A within the scope of 0.2 ~ 1.6 μm of ol/L
700/ A
520(see figure 7) linear with iodide ion concentration, detects and is limited to 0.05 μm of ol/L.
Embodiment 8:
Add ethylenediamine tetraacetic acid (final concentration is 0.5 mmol/L) in the water sample of 10 milliliters, after 0.22 μm of membrane filtration, obtain sample solution.In the nm of gold that 0.25 milliliter of embodiment 1 is obtained, add 0.2 milliliter of above-mentioned sample solution and 0.05 milliliter of 8 mmol/L sulfuric acid (thiocyanates containing 2.5 μm of ol/L), 30 DEG C are reacted 3 minutes, the change of visualization color or mensuration absorbance ratio A
700/ A
520.7 content calculating iodide ion in water samples in conjunction with the embodiments, the sample tests recovery is 97.1% ~ 105.0%, and relative standard deviation is 1.4 ~ 2.2%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. one kind
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that nm of gold being stoped to produce gathering in an acidic solution based on thiocyanate, make it keep claret, and the specific suppression thiocyanate of iodide ion energy is to the protective effect of nm of gold; thus show the change of solution colour and ultra-violet absorption spectrum feature, come
measure iodide ion concentration.
2. according to claim 1
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that utilizing visualization solution colour feature to judge the concentration of iodide ion.
3. according to claim 1
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that utilizing absorbance ratio A
700/ A
520to judge the concentration of iodide ion.
4. according to claim 1 or 2 or 3
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that used nm of gold adopts the method preparation of reduction of sodium citrate gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliters of 0.1g/L, reaction solution becomes claret from light yellow, continue backflow after 15 minutes, reaction solution is slowly cooled to room temperature and forms nm of gold.
5. according to claim 4
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that 5:4 is by nano-Au solution with containing the mixing of variable concentrations iodide ion solution by volume, adding 0.05 ml concn is 8 ~ 10 mmol/L sulfuric acid solutions, containing the thiocyanate of 2.5 ~ 3 μm of ol/L in 8 ~ 10 described mmol/L sulfuric acid solutions, react 3 ~ 5 minutes at 30 DEG C, visualization color characteristic or mensuration absorbance ratio A
700/ A
520, when visualization color characteristic along with the increase of iodide ion concentration, the color of nm of gold becomes aubergine-purple-pewter from redness gradually, and the detection of visualization is limited to 0.8 μm of ol/L; As mensuration absorbance ratio A
700/ A
520time, the absorbance ratio A along with the increase of iodide ion concentration
700/ A
520increase gradually, A within the scope of 0.2 ~ 1.6 μm of ol/L
700/ A
520linear with iodide ion concentration, detect and be limited to 0.05 μm of ol/L.
6. according to claim 4
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probe, it is characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.1 nmol/L.
7. according to claim 5
take nm of gold as the rapid assay methods of the iodide ion of logic gate colour developing probeit is characterized in that 5:4 is by nano-Au solution with containing the mixing of variable concentrations iodide ion solution by volume, add 0.05 milliliter of 8 mmol/L sulfuric acid solution, containing the thiocyanate of 2.5 μm of ol/L in 8 described mmol/L sulfuric acid solutions, react 3 minutes at 30 DEG C, visualization color characteristic or mensuration absorbance ratio A
700/ A
520to judge the concentration of iodide ion; Nano-Au solution and be respectively 0.25 milliliter and 0.20 milliliter containing the volume of variable concentrations iodide ion solution.
8. one kind
take nm of gold as the iodide ion method in logic gate colour developing probe Fast Measurement water sample, comprise the steps: in the water sample of 10 milliliters, to add the ethylenediamine tetraacetic acid that final concentration is 0.5 mmol/L, after 0.22 μm of membrane filtration, obtain sample solution; 0.20 milliliter of above-mentioned sample solution and 0.05 milliliter of 8 mmol/L sulfuric acid is added in 0.25 milliliter of nm of gold, containing the thiocyanate of 2.5 μm of ol/L in 8 described mmol/L sulfuric acid solutions, react 3 minutes at 30 DEG C, the change of then visualization color or mensuration absorbance ratio A
700/ A
520, according to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve, obtain
the content of the iodide ion in water sample.
9. according to claim 8
take nm of gold as the iodide ion method in logic gate colour developing probe Fast Measurement water sampleit is characterized in that used nm of gold adopts the method preparation of reduction of sodium citrate gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution adding rapidly 3 milliliter of 0.1 g/L, reaction solution becomes claret from light yellow, continue backflow after 15 minutes, reaction solution is slowly cooled to room temperature and forms nm of gold.
10. according to claim 9
take nm of gold as the iodide ion method in logic gate colour developing probe Fast Measurement water sample, it is characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.1 nmol/L.
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| CN105954957B (en) * | 2016-05-02 | 2018-10-23 | 福建医科大学 | NAND gate based on gold nano cluster solid-phase complex and its construction method |
| CN106404766A (en) * | 2016-08-30 | 2017-02-15 | 中南林业科技大学 | Preparation method of nanogold colorimetric probe and method for detecting iodide ions by using nanogold colorimetric probe |
| CN108508002A (en) * | 2018-02-08 | 2018-09-07 | 暨南大学 | A kind of NIMPLY+OR logic gates based on nanogold and the Visual retrieval applied to DNA |
| CN110646418B (en) * | 2019-10-24 | 2021-10-15 | 福建医科大学 | Scandium ion rapid determination method using nanogold as developing probe |
| CN113866100B (en) * | 2021-07-12 | 2024-04-30 | 中南民族大学 | Method for judging authenticity of white skill by utilizing nano silver deposition visual sensor |
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| CN102183516B (en) * | 2011-03-04 | 2013-01-16 | 南京工业大学 | Nano gold colorimetric method for simply and cheaply detecting mercury ions |
| KR101208659B1 (en) * | 2011-08-30 | 2012-12-05 | 한국기계연구원 | Detection method using colorimetric analysis |
| CN102706814B (en) * | 2012-05-11 | 2014-04-02 | 福建医科大学 | Rapid melamine determination method using bare gold nanoparticles as developing probe |
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