CN106770208A - A kind of method that ferrous ion is detected based on gold nanorods - Google Patents
A kind of method that ferrous ion is detected based on gold nanorods Download PDFInfo
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- CN106770208A CN106770208A CN201611137867.7A CN201611137867A CN106770208A CN 106770208 A CN106770208 A CN 106770208A CN 201611137867 A CN201611137867 A CN 201611137867A CN 106770208 A CN106770208 A CN 106770208A
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Abstract
The invention discloses a kind of method that ferrous ion is detected based on gold nanorods, belong to ion analysis detection field, realized by following steps：The standard liquid of the ferrous ion of various concentrations is added to the mixed solution of hydrogen peroxide, potassium rhodanide, hydrochloric acid and gold nanorods solution, fully reaction, gold nanorods after reaction are utilized into ultraviolet-visible spectrophotometry, determine that it absorbs peak position, linear change according to absworption peak shift value draws standard working curve, linear equation with one unknown is obtained, the sample concentration value being calculated in the linear equation with one unknown that the absorption spectral peak shift value of testing sample is brought into standard working curve.Gold nanorods prepared by the present invention, process is simple and convenient, asepsis environment-protecting, size and pattern are homogeneous, good stability, the concentration and reaction condition by controlling ferrous ion solution of the invention so that gold nanorods and ferrous ion fast reaction in aqueous environments, the ferrous ion in water environment is rapidly detected, the specificity with height.
Description
Technical field
The present invention relates to the detection method of ferrous ion, and in particular to one kind detects ferrous ion based on gold nanorods
Method, belong to ion analysis detection field.
Background technology
Detecting the conventional method of ferrous ion has fluorescence method, electrochemical process and gas chromatography etc..These methods show
The advantages of detection sensitivity is high, reproducible and detects accurate, but at the same time there is instrument that is cumbersome and needing costliness
The deficiencies such as device equipment.Current colorimetric determination is a kind of more novel detection method of analytical chemistry field, it can overcome with
It is not enough so as to rapid sensitive is tested and analyzed to object exactly that upper detection method is present.Gold nanocrystals are in colorimetric detection
Field is widely used, and under normal circumstances to being added as the gold nano grain of detection probe in system to be detected, treats
Detectable substance directly makes gold nano grain reunite so as to complete to detect work, when making to be detected in this way with indirectly effect
Gold nano grain can occur from reunion so as to produce false positive effect and then detection work is had a huge impact.In order to overcome
The deficiency of " reunion colorimetric method ", colorimetric inspection is carried out there has been proposed detectable substance is treated using the method for oxide etch gold nanocrystals
Survey.This method is not usually required to carry out surface ligand modification to gold nanocrystals, easy to operate, detects sensitive directly perceived, however, Au
(I) with oxidation-reduction potential higher, this method is only limitted to mesh of the oxidation-reduction potential higher than Au (I)/Au (0) to/Au (0)
Mark thing.So, the colorimetric detection method of oxide etch gold nanocrystals is restricted in actual application, to being at present
Only, there is not yet low concentration ferrous ion is detected using the method.
The content of the invention
In order to the colorimetric detection method for overcoming the shortcomings of existing oxide etch gold nanocrystals is present, the invention provides one kind
The method that ferrous ion is detected based on gold nanorods, the method has very strong specificity, only sensitive to ferrous ion, detection
During do not need buffer solution, hence in so that operation is simple, and the preparation process of gold nanorods is simple, and yield is big, the party
Method can rapidly and sensitively detect the ferrous ion in serum solution.
To achieve the above object, the technical solution adopted in the present invention is：
The invention provides a kind of method that ferrous ion is detected based on gold nanorods, comprise the following steps：
（1）Gold nanorods are scattered in cetyl trimethylammonium bromide solution, gold nanorods probe solution is obtained；
（2）Fitting operations curve：By potassium thiocyanate solution, hydrogenperoxide steam generator and 200 μ L gold nanorods probe solutions mix
Uniformly, detection architecture pH value is changed by using HCl or NaOH, be then added thereto to a series of various concentrations it is ferrous from
The substandard aqueous solution to the cumulative volume of reaction system is 2mL, fully after reaction, by the UV, visible light spectrophotometric of solution after reaction
Method is tested, and according to the relation drawing curve of the spectrum peak shift value and ferrous ion concentration for accordingly obtaining, obtains one
First linear function；
（3）Sample determination：By potassium thiocyanate solution, hydrogenperoxide steam generator, well mixed mixed solution is simultaneously adjusted with hydrochloric acid solution
Section pH value, the concentration of potassium rhodanide is 0.75 mM in mixed solution, and the concentration of hydrogen peroxide is 100 μM, and concentration of hydrochloric acid is 25
MM, is subsequently adding 200 μ L gold nanorods probe solutions and is well mixed, and is added thereto to a series of ferrous ion of various concentrations
4% hyclone solution, reaction total system volume is 2 mL, fully after reaction, then by step（2）Described correlation method enters
Row spectrum test, brings sample spectra peak shift value into step（2）In the linear equation with one unknown for obtaining, in the sample being calculated
The concentration value of ferrous ion.
Further, step（1）In, the gold nanorods for being used are prepared from using following methods：
（1）Prepare gold nanorods solution：Take cetyl trimethylammonium bromide solution and 30 μ L concentration that 5 mL concentration are 0.1M
For the aqueous solution of chloraurate of 50 mM is sufficiently mixed stirring, the fresh configurations of 0.3 mL are then rapidly joined under condition of ice bath
0.01 M sodium borohydride solutions, are sufficiently stirred for 2 minutes, obtain nm of gold seed-solution after still aging 2 h at room temperature stand-by；
（2）By the cetyl trimethylammonium bromide solution that 40 mL concentration are 0.1 M and the chlorine gold that 600 μ L concentration are 50 mM
Aqueous acid, the concentration of 96.5 μ L is that the silver nitrate solution of 50 mM is sufficiently mixed stirring 1 minute, in mixed solution dropwise plus
Enter the ascorbic acid that 500 μ L concentration are 0.08 M, stir 10 seconds, obtain the water white transparency aqueous solution；
（3）80 μ L nm of gold seed-solutions are added to the water white transparency aqueous solution, by solution in standing at 25 DEG C after stirring 10 minutes
12 hours, gold nanorods solution is obtained, supernatant is then removed in 15 minutes with the centrifugation of 8500 r/min rotating speeds, obtained final product filemot
Gold nanorods.
Gold nanorods draw ratio prepared by the present invention is 2.5:1.
Further, in detection process, step（1）The concentration of the cetyl trimethylammonium bromide solution be 0 ~
300mM；The concentration of the gold nanorods probe solution is 1.5 nM.
Further, the detection architecture pH value that changes adds 500 μ L concentration dense for the NaOH of 1M by detection architecture
The HCl for 0,1,10,100,1000 mM is spent to realize.
Further, step（2）With（3）In, the concentration of the potassium rhodanide is 0 ~ 25 mM, and addition volume is 15 μ L；Institute
It is 0 ~ 10000 μM to state the concentration of hydrogen peroxide, and addition volume is 20 μ L.
Further, the potassium rhodanide concentration is 0.75 mM；Concentration of hydrogen peroxide is 100 μM.
Further, step（2）With（3）In, the condition of the reaction is：0 ~ 12 min is reacted at 25-85 DEG C；It is optimal
The reaction condition of change be 65 DEG C at react 8min.
Further, step（2）With（3）In, the concentration of the ferrous ion standard aqueous solution is 0 ~ 2.5 μM.
Further, step（2）With（3）In, the condition of scanning of the ultraviolet-visible spectrophotometry is：Dual-beam swashs
Hair, light source：Deuterium lamp, scanning wavelength scope is 300-800 nm.
All variables can carry out ferrous ion detection in the range of preferred value, but there is optimal value so that detection range most
Greatly, i.e.,：PH is regulated and controled by adding concentration for the hydrochloric acid solution of 1M, and cetyl trimethylammonium bromide concentration is 50 mM, sulphur cyanogen
Sour potassium concn is 0.75 mM, and concentration of hydrogen peroxide is 100 μM, and the reaction time is 8 min, and reaction temperature is 65 DEG C.
Beneficial effects of the present invention are：
（1）The preparation process of gold nanorods is simple and convenient, environment-protecting asepsis, and the gold nanorods size prepared with seeded growth method is equal
Even, pattern is homogeneous, and good stability, yield is big.
（2）Detection process is carried out in sour environment, and testing result has high degree of specificity, can quantitatively to ferrous ion
Detected, be quick on the draw, detection time is short.
Brief description of the drawings
Fig. 1 is the transmission electron microscope of the gold nanorods prepared by embodiment 1（TEM）Figure；
Fig. 2 is the gold nanorods of embodiment 1 and the reacted TEM figures of ferrous ion that concentration is 1mM；
The specially selective experimental result of the detection ferrous ion that Fig. 3 is provided for the present invention；
Fig. 4 is that the peak shift value of gold nanorods detection various concentrations ferrous ion in the embodiment of the present invention 1 is linear with ferrous ion
Graph of a relation.
Specific embodiment
With reference to embodiment, the present invention is further described, and the description of specific embodiment is substantially only example, without
It is to present disclosure and its application or using limiting.
4% hyclone solution used in the present invention is purchased from Hangzhou Sijiqing Biological Engineering Material Co., Ltd..
Embodiment 1
1.1 take the cetyl trimethylammonium bromide solution that 5 mL concentration are 0.1M with the gold chloride that 30 μ L concentration are 50 mM
The aqueous solution is sufficiently mixed stirring, and the 0.01 M sodium borohydrides that the fresh configurations of 0.3 mL are then rapidly joined under condition of ice bath are molten
Liquid, is sufficiently stirred for 2 minutes, obtains nm of gold seed-solution after still aging 2 h at room temperature stand-by；
By the cetyl trimethylammonium bromide solution that 40 mL concentration are 0.1 M and the gold chloride water that 600 μ L concentration are 50 mM
Solution, the concentration of 96.5 μ L is that the silver nitrate solution of 50 mM is sufficiently mixed stirring 1 minute, to being added dropwise over 500 in mixed solution
μ L concentration is the ascorbic acid of 0.08 M, stir about after 10 seconds solution gradually become clear, colorless；
Finally, the previously prepared nm of gold seed-solutions of 80 μ L are added to the water white transparency aqueous solution, by solution after stirring 10 minutes
Standing 12 hours in 25 DEG C of environment can prepare gold nanorods solution；
1.2 by step（1）Prepared gold nanorods solution, supernatant is removed in 15 minutes with the centrifugation of 8500 r/min rotating speeds,
Tan precipitate, as gold nanorods, will precipitation to be dispersed in the cetyl trimethylammonium bromide that concentration is 50 mM again molten
In liquid, gold nanorods probe solution is obtained；
The gold nanorods of preparation are shown in Fig. 1, from figure 1 it appears that the gold nanorods size uniform for preparing, pattern is homogeneous；
1.3 fitting operations curves：By 50 μ L, the HCl solution of 0.1 M, 15 μ L, 0.75 mM potassium thiocyanate solutions, 20 μ L,
10 mM hydrogenperoxide steam generators and 200 μ L gold nanorods probe solutions are well mixed, and 0 ~ 2.5 μM is then separately added into thereto
Ferrous ion standard aqueous solution add to overall reaction system for 2mL, reacted 8 minutes at 65 DEG C, by solution after reaction with ultraviolet
Visible spectrophotometry is tested, and the reacted gold nanorods of reaction system that concentration is 1 mM are added to ferrous ion
Carry out TEM signs (see Fig. 2).Relation drawing according to the spectrum peak shift value and ferrous ion concentration for accordingly obtaining is bent
Line, obtains linear equation with one unknown for y=0.09093x-6.7394, linearly dependent coefficient R2=0.9751, range of linearity 75-1000
NM (see Fig. 4), secondary detection method specific selectivity is good（See Fig. 3）
1.4 take 4% serum solution containing ferrous ion as sample, are added thereto to 100 μ L, and 100 mM HCl solutions will
Potassium thiocyanate solution, hydrogenperoxide steam generator and 200 μ L gold nanorods probe solutions are well mixed, potassium thiocyanate solution concentration
It is 0.75 mM, concentration of hydrogen peroxide is 100 μM.Reaction system cumulative volume is 2 mL, is reacted 8 minutes at 65 DEG C；By purple
Outward-visible absorption spectra peak shift value is brought into the linear equation with one unknown of standard working curve, be calculated in sample it is ferrous from
The concentration value of son is 355nM；
The condition of scanning of above-mentioned ultraviolet-visible spectrophotometry is：Dual beam excitation, light source：Deuterium lamp, scanning wavelength scope is
300-800 nm。
Embodiment 2
Standard curve is obtained by the methods described of embodiment 1, difference is that change reaction temperature is 45 DEG C, range of linearity 350-
1000 nM。
Embodiment 3
Standard curve is obtained by the methods described of embodiment 1, difference is that change reaction temperature is 85 DEG C, range of linearity 75-
650 nM。
Embodiment 4
Standard curve is obtained by the methods described of embodiment 1, difference is to change the reaction time for 6min., the range of linearity
650-1500 nM。
Embodiment 5
Standard curve is obtained by the methods described of embodiment 1, difference is to change the reaction time for 10min.The range of linearity
350-650 nM。
Embodiment 6
Standard curve is obtained by the methods described of embodiment 1, difference is that the concentration of hydrogen peroxide is 10 μM.The range of linearity
150-650 nM。
Embodiment 7
Standard curve is obtained by the methods described of embodiment 1, difference is that the concentration of hydrogen peroxide is 1 mM.The range of linearity
300-850 nM。
Embodiment 8
Standard curve is obtained by the methods described of embodiment 1, difference is that the concentration of potassium rhodanide is 0.55 mM.Linear model
Enclose 200-1200nM.
Embodiment 9
Standard curve is obtained by the methods described of embodiment 1, difference is that the concentration of potassium rhodanide is 1 mM.The range of linearity
65-550nM。
It can be seen from the results above that in hydrogen peroxide, the optimization concentration range of potassium rhodanide, and the optimization time,
In temperature range, the detection of ferrous ion can be carried out, but compared with Example 1, the range of linearity of detection narrows；In addition,
When the scope that hydrogen peroxide, potassium rhodanide etc. are provided beyond the present invention, poor specificity.
Above example is that explanation example effect is played to technology design of the invention, can not limit the present invention with this
Protection domain, those skilled in the art modify and are equal in the spirit and scope for not departing from technical solution of the present invention
Replace, all should fall within the scope and spirit of the invention.
Claims (10)
1. it is a kind of based on gold nanorods detect ferrous ion method, it is characterised in that comprise the following steps：
（1）Gold nanorods are scattered in cetyl trimethylammonium bromide solution, gold nanorods probe solution is obtained；
（2）Fitting operations curve：By potassium thiocyanate solution, hydrogenperoxide steam generator and 200 μ L gold nanorods probe solutions mix
Uniformly, detection architecture pH value is changed by using HCl or NaOH, be then added thereto to a series of various concentrations it is ferrous from
The substandard aqueous solution to the cumulative volume of reaction system is 2mL, fully after reaction, by the UV, visible light spectrophotometric of solution after reaction
Method is tested, and according to the relation drawing curve of the spectrum peak shift value and ferrous ion concentration for accordingly obtaining, obtains one
First linear function；
（3）Sample determination：By potassium thiocyanate solution, hydrogenperoxide steam generator, well mixed mixed solution is simultaneously adjusted with hydrochloric acid solution
Section pH value, the concentration of potassium rhodanide is 0.75 mM in mixed solution, and the concentration of hydrogen peroxide is 100 μM, and concentration of hydrochloric acid is 25
MM, is subsequently adding 200 μ L gold nanorods probe solutions and is well mixed, and is added thereto to a series of ferrous ion of various concentrations
4% hyclone solution, reaction total system volume is 2 mL, fully after reaction, then by step（2）Described correlation method enters
Row spectrum test, brings sample spectra peak shift value into step（2）In the linear equation with one unknown for obtaining, in the sample being calculated
The concentration value of ferrous ion.
2. method according to claim 1, it is characterised in that step（1）In, the gold nanorods use following methods system
It is standby to form：
（1）Prepare gold nanorods solution：Take cetyl trimethylammonium bromide solution and 30 μ L concentration that 5 mL concentration are 0.1M
For the aqueous solution of chloraurate of 50 mM is sufficiently mixed stirring, the fresh configurations of 0.3 mL are then rapidly joined under condition of ice bath
0.01 M sodium borohydride solutions, are sufficiently stirred for 2 minutes, obtain nm of gold seed-solution after still aging 2 h at room temperature stand-by；
（2）By the cetyl trimethylammonium bromide solution that 40 mL concentration are 0.1 M and the chlorine gold that 600 μ L concentration are 50 mM
Aqueous acid, the concentration of 96.5 μ L is that the silver nitrate solution of 50 mM is sufficiently mixed stirring 1 minute, in mixed solution dropwise plus
Enter the ascorbic acid that 500 μ L concentration are 0.08 M, stir 10 seconds, obtain the water white transparency aqueous solution；
（3）80 μ L nm of gold seed-solutions are added to the water white transparency aqueous solution, by solution in standing at 25 DEG C after stirring 10 minutes
12 hours, gold nanorods solution is obtained, supernatant is then removed in 15 minutes with the centrifugation of 8500 r/min rotating speeds, obtained final product filemot
Gold nanorods.
3. method according to claim 2, it is characterised in that the gold nanorods draw ratio is 2.5:1.
4. method according to claim 1, it is characterised in that step（1）In, the cetyl trimethylammonium bromide is molten
The concentration of liquid is 0 ~ 300mM；The concentration of the gold nanorods probe solution is 1.5 nM.
5. method according to claim 1, it is characterised in that the change detection architecture pH value is by detection architecture
The NaOH concentration for adding 500 μ L concentration to be 1M is that the HCl of 0,1,10,100,1000 mM is realized.
6. method according to claim 1, it is characterised in that step（2）With（3）In, the concentration of the potassium rhodanide
It is 0 ~ 25 mM, addition volume is 15 μ L；The concentration of the hydrogen peroxide is 0 ~ 10000 μM, and addition volume is 20 μ L..
7. method according to claim 6, it is characterised in that the potassium rhodanide concentration is 0.75 mM；Hydrogen peroxide is dense
Spend is 100 μM.
8. method according to claim 1, it is characterised in that step（2）With（3）In, the condition of the reaction is：
0 ~ 12 min is reacted at 25-85 DEG C；The reaction condition of optimization be 65 DEG C at react 8min.
9. method according to claim 1, it is characterised in that step（2）With（3）In, the ferrous ion standard is water-soluble
The concentration of liquid is 0 ~ 2.5 μM.
10. method according to claim 1, it is characterised in that step（2）With（3）In, the UV, visible light light splitting light
The condition of scanning of degree method is：Dual beam excitation, light source：Deuterium lamp, scanning wavelength scope is 300-800 nm.
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Cited By (1)
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| CN107543924A (en) * | 2017-09-06 | 2018-01-05 | 重庆医科大学 | Biology sensor detection myeloperoxidase based on copper palladium platinum mesh nanometer material |
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| CN103411962A (en) * | 2013-05-15 | 2013-11-27 | 中国科学院烟台海岸带研究所 | Kit and method for detecting cobalt ions through colorimetric method |
Non-Patent Citations (3)
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| RENXIAN ZOU ET AL.: "Selective etching of gold nanorods by ferric chloride at room temperature", 《CRYSTENGCOMM》 * |
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| 杨春平 等主编: "《废水处理原理》", 31 December 2012, 湖南大学出版社 * |
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| CN107543924A (en) * | 2017-09-06 | 2018-01-05 | 重庆医科大学 | Biology sensor detection myeloperoxidase based on copper palladium platinum mesh nanometer material |
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Application publication date: 20170531 |