CN107219218B - A kind of bivalent nickel ion colorimetric detection method of simple and sensitive - Google Patents
A kind of bivalent nickel ion colorimetric detection method of simple and sensitive Download PDFInfo
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- CN107219218B CN107219218B CN201710394055.9A CN201710394055A CN107219218B CN 107219218 B CN107219218 B CN 107219218B CN 201710394055 A CN201710394055 A CN 201710394055A CN 107219218 B CN107219218 B CN 107219218B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 229910001453 nickel ion Inorganic materials 0.000 title claims abstract description 16
- 239000010931 gold Substances 0.000 claims abstract description 21
- 229910052737 gold Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 17
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims abstract description 15
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 13
- 230000004520 agglutination Effects 0.000 claims abstract description 7
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 40
- 239000012488 sample solution Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000004451 qualitative analysis Methods 0.000 claims description 3
- 238000012764 semi-quantitative analysis Methods 0.000 claims description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 11
- 239000012491 analyte Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 3
- 238000003745 diagnosis Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 230000036647 reaction Effects 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 15
- 238000012360 testing method Methods 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000000523 sample Substances 0.000 description 6
- 239000012496 blank sample Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910001112 rose gold Inorganic materials 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 102000005606 Activins Human genes 0.000 description 1
- 108010059616 Activins Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NMWONDKHBZEDMY-UHFFFAOYSA-H [Au](Cl)(Cl)Cl.C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[Na+].[Na+].[Na+] Chemical compound [Au](Cl)(Cl)Cl.C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-].[Na+].[Na+].[Na+] NMWONDKHBZEDMY-UHFFFAOYSA-H 0.000 description 1
- LLERHZKCRWPOFT-UHFFFAOYSA-L [Cl+].C(CC(O)(C(=O)O)CC(=O)[O-])(=O)[O-].[Na+] Chemical compound [Cl+].C(CC(O)(C(=O)O)CC(=O)[O-])(=O)[O-].[Na+] LLERHZKCRWPOFT-UHFFFAOYSA-L 0.000 description 1
- 239000000488 activin Substances 0.000 description 1
- 230000004523 agglutinating effect Effects 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000002384 drinking water standard Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 231100001224 moderate toxicity Toxicity 0.000 description 1
- 238000012123 point-of-care testing Methods 0.000 description 1
- 230000002685 pulmonary effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of bivalent nickel ion colorimetric detection methods of simple and sensitive.This method effectively can mediate gold nano grain to be aggregated using low concentration Phen, and the color change for causing reaction solution to occur from red to blue reacts.And a small amount of Ni2+Can Phen-Ni efficiently, specifically be generated with Phen2+Complex, to inhibit the metachromasia of above-mentioned solution.The degree that gold nano grain agglutination causes reaction solution that color change occurs is inversely proportional to Ni in sample2+Concentration.Therefore, Ni can be realized in the color change for observing by the naked eye reaction solution2+Simple and sensitive is qualitative or half-quantitative detection.The accurate quantitative analysis detection of target metal ions analyte can be further realized if by photometer.The method of the present invention can directly be applied in the numerous areas such as medical diagnosis, environmental monitoring, food safety Ni in all types of samples2+Simple, economic, quick, sensitive, the special analysis detection of analyte.
Description
Technical field
The invention belongs to nanochemistry field of sensing technologies, and in particular to a kind of bivalent nickel ion colorimetric inspection of simple and sensitive
Survey method.
Background technique
Bivalent nickel ion (Ni2+) belong to transition element, it is one of biological element needed by human, it can be in human activin
Various enzymes, participate in metabolism.However, Ni2+With moderate toxicity, human body large dosage absorbs or Long Term Contact can cause sternly
Weight disease, such as skin disease, pulmonary infection, malignant tumour.China's drinking water standard provides Ni in water2+Limit value is 0.02
mg/L.For ensure human health and other biological life security, to the trace Ni in food, water and environment2+Carry out sensitive inspection
It surveys significant.Existing Ni2+Detection technique mainly include spectrophotometry, atomic absorption method, atomic emission spectrometry, etc.
Gas ions mass spectrography, electrochemical methods and liquid chromatography etc..However, these methods or complex for operation step time-consuming, no
It can be used for field assay and real-time test (Point-of-Care Testing) or detection sensitivity is limited.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of bivalent nickel ion colorimetric detections of simple and sensitive
Method.
Thinking of the invention: the low concentration Phen containing N atom can be reacted by N-Au mediates gold nano grain hair
Raw agglutination, the color change for causing reaction solution to occur from red to blue react.And a small amount of Ni2+Can by with N Atomic coordinate,
Efficiently, Phen-Ni specifically is generated with Phen molecule2+Complex, so that above-mentioned solution changes color be inhibited to react.Jenner
The degree that rice grain agglutination causes reaction solution that color change occurs is inversely proportional to Ni in sample2+Concentration.Therefore, it observes by the naked eye
Ni can be realized in the color change of reaction solution2+Simple and sensitive is qualitative or half-quantitative detection.If being divided light by UV, visible light
Degree meter can then further realize the accurate quantitative analysis detection of target metal ions analyte.
Specific steps are as follows:
Step 1, by Ni2+Sample solution is mixed with Phen solution, generates Phen-Ni2+Complex is made anti-
Answer solution.
Gold nano grain solution is added into reaction solution made from step 1 for step 2, and mixed solution is made, and mixes molten
Remaining Phen will mediate gold nano grain agglutination, the agglutination degree and Ni of gold nano grain in liquid2+Ni in sample solution2 +Concentration be in inverse ratio, the color change of the naked-eye observation mixed solution carries out qualitative or semi-quantitative analysis, or using photometer into
The Ni of simple and sensitive is realized in row quantitative analysis2+Colorimetric detection.
The color of the gold nano grain solution is red.
The luminosity is calculated as one of bench photometer and Portable photometer.
With existing Ni2+Detection method is compared, and of the invention has the prominent advantages that:
1) entire Ni2+Operation in analytic process is extremely simple, and the operator without professional skill training can also carry out
Experiment；2) by cooperateing with Phen effectively to mediate gold nano grain agglutinating reaction and Ni2+Efficiently, specifically with Phen molecule
Generate Phen-Ni2+Complex reaction, significantly improves the detection sensitivity of method；3) naked-eye observation solution colour is only needed
Change, Ni can be realized2+Sensitive qualitative or semi-quantitative analysis, or can be by further realizing analysis by Portable photometer
The accurate quantitative analysis of object detects, and can be used for Ni while greatly reducing analysis cost2+The field assay of sample and immediately detection；
4) present invention can directly be applied in the numerous areas such as medical diagnosis, environmental monitoring, food safety Ni in all types of samples2+
Simple, economic, quick, sensitive, the special qualitative and quantitative detection of analyte.
Detailed description of the invention
Fig. 1 is that the principle of the bivalent nickel ion colorimetric detection method of simple and sensitive in Example 1 and Example 2 of the present invention is shown
It is intended to.
Marked in the figure: the colourless ultrapure water of 1-1-；1-2-Phen；2-test tubes；The colourless ultrapure water of 3-1-；3-
2—Ni2+；4-Phen-Ni2+Complex；5-1-red solution；5-2-gold nano grain；6-naked eyes；7-is portable
Spectrophotometer.
Fig. 2 is to detect (A) 2 respectively using the bivalent nickel ion colorimetric detection method of simple and sensitive in the embodiment of the present invention 1
μM Ni2+Sample solution is compared with (B) blank sample (ultrapure water) gained Colorimetric results.
Fig. 3 is to analyze a series of contain using the bivalent nickel ion colorimetric detection method of simple and sensitive in the embodiment of the present invention 2
There is various concentration Ni2+Sample solution when absorption intensity value (A730) at the 730 nm and absorption intensity value at 520 nm
(A520) ratio (A730/A520) and Ni2+Concentration value between working curve.
Specific embodiment
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1:
2 μM of Ni are detected respectively using the bivalent nickel ion colorimetric detection method of simple and sensitive2+Sample solution and blank sample
(ultrapure water).
As shown in Figure 1, the specific steps of the present embodiment are as follows: step 1 is added in the plastics test tubes of 1 1.5 mL
The Phen solution (being prepared by the ultrapure water that resistivity is 18.2 M Ω cm) of 150 2 μM of μ L, then into the solution
The Ni of 2 μM of 150 μ L is added dropwise2+(nickel chloride prepared by the ultrapure water that resistivity is 18.2 M Ω cm is molten for sample solution
Liquid), and shaking test tube is uniformly mixed two kinds of solution, generates Phen-Ni2+Reaction solution is made in complex；Step 2,
300 μ L red gold nano grain solution (about 13 nm of partial size, by reduction of sodium citrate chlorine are continuously added in above-mentioned reaction solution
Auric acid is made), and shake test tube and make solution after mixing, the color change of naked-eye observation solution.
According to identical step, analysis margin sample, i.e. ultrapure water (resistivity is 18.2 M Ω cm), and naked-eye observation is molten
The color change of liquid.Figure it is seen that blank sample obtains is blue solution for detection, and detect 2 μM of Ni2+Analyte
Resulting is red solution.This is because the Phen molecule containing N atom can be reacted by N-Au when detection blank sample
It mediates gold nano grain to be aggregated, leads to the color change of reaction solution generation from red to blue.And when there are Ni in sample2+
When, Ni2+By with N Atomic coordinate, efficiently, specifically with Phen molecule generate Phen-Ni2+Complex product.By
Gold nano grain cannot be caused to be aggregated in the product, entire reaction solution still keeps the original red of gold nano grain solution
Color.Contrast and experiment in Fig. 2 shows the Ni of simple and sensitive of the invention2+Colorimetric detection method is practical.
Embodiment 2:
Bivalent nickel ion colorimetric detection method analytical concentration range using simple and sensitive is the Ni of 465 nM ~ 2 μM2+Sample
This solution.Specific implementation process is as follows:
As shown in Figure 1, each Ni in the present embodiment2+The specific steps of sample solution analysis are as follows: step 1, at 1 1.5
The Phen solution that 2 μM of 150 μ L is added in the plastics test tubes of mL (is the ultrapure of 18.2 M Ω cm by resistivity
Water is prepared), a certain concentration Ni of 150 μ L is then added dropwise into the solution2+Sample solution (is 18.2 M Ω cm's by resistivity
The nickel chloride solution that ultrapure water is prepared), and shaking test tube is uniformly mixed two kinds of solution, generates Phen-Ni2+Complex,
Reaction solution is made；Step 2 continuously adds 300 μ L red gold nano grain solution (partial sizes about 13 in above-mentioned reaction solution
Nm is made by reduction of sodium citrate gold chloride), and shake test tube and make solution after mixing, the color of naked-eye observation solution becomes
Change, and measures absorption intensity value (A520 of the solution at 520 and 730 nm using Portable UV-Vis Spectrophotometer
And A730).By the ratio (A730/A520) of the absorption intensity value at the two wavelength of all samples to Ni2+Concentration value mapping
(Fig. 3), can be obtained Ni2+Quantitative determination working curve.
From the figure 3, it may be seen that with Ni2+The increase of concentration, corresponding A730/A520 ratio gradually decrease.This is because working as sample
Ni in this2+When concentration is larger, analyte efficiently, specifically can generate Phen-Ni with more Phen molecule2+
Complex product.It mediates gold nano grain to be aggregated at this point, remaining Phen molecule is not enough to react by N-Au, contains
There is absorption intensity value of the corresponding mixed solution of the more gold nano grain freely dispersed at 730 nm, i.e. A730 value is smaller；
And its absorption intensity value at 520 nm, i.e. A520 value are then larger.In addition, Fig. 3 is shown, new method measures all nickel ion samples
This gained A730/A520 ratio and Ni2+Good linear relationship is presented in 465 nM ~ 2 μM of concentration range in concentration.
Claims (1)
1. a kind of bivalent nickel ion colorimetric detection method of simple and sensitive, it is characterised in that specific steps are as follows:
Step 1 mixes nickel ion sample solution with Phen solution, generates Phen-Ni2+Reaction is made in complex
Solution；
Gold nano grain solution is added into reaction solution made from step 1 for step 2, mixed solution is made, in mixed solution
Remaining Phen will mediate gold nano grain agglutination, Ni in the agglutination degree and nickel ion sample solution of gold nano grain2+
Concentration be in inverse ratio, the color change of the naked-eye observation mixed solution carries out qualitative or semi-quantitative analysis, or using photometer into
The bivalent nickel ion colorimetric detection of simple and sensitive is realized in row quantitative analysis；
The color of the gold nano grain solution is red；
The luminosity is calculated as one of bench photometer and Portable photometer.
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| CN113310973B (en) * | 2021-04-15 | 2023-04-25 | 中国工程物理研究院材料研究所 | Preparation method of nano-gold colorimetric sensor and application of nano-gold colorimetric sensor in divalent nickel ion detection |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841061A (en) * | 2012-09-14 | 2012-12-26 | 中国科学院宁波材料技术与工程研究所 | Method for detecting nickelous ions |
| CN104193678A (en) * | 2014-03-06 | 2014-12-10 | 西北师范大学 | A nickel ion acceptor compound, synthesis thereof and applications of the compound |
| CN106442514A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Simple ultrasensitive colorimetric detection method for bivalent copper ions |
| CN106442513A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Instrument-free bivalent copper ion detection method based on timing strategy |
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2017
- 2017-05-28 CN CN201710394055.9A patent/CN107219218B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841061A (en) * | 2012-09-14 | 2012-12-26 | 中国科学院宁波材料技术与工程研究所 | Method for detecting nickelous ions |
| CN104193678A (en) * | 2014-03-06 | 2014-12-10 | 西北师范大学 | A nickel ion acceptor compound, synthesis thereof and applications of the compound |
| CN106442514A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Simple ultrasensitive colorimetric detection method for bivalent copper ions |
| CN106442513A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Instrument-free bivalent copper ion detection method based on timing strategy |
Non-Patent Citations (1)
| Title |
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| 铜、锌、钴、镍-邻菲罗啉体系中稀土元素与偶氮氯膦Ⅲ显色反应的研究;虞光禹;《分析化学》;19861231;第14卷(第9期);第646-649页 * |
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Application publication date: 20170929 Assignee: Guilin Qiyun New Materials Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044906 Denomination of invention: A simple and sensitive colorimetric detection method for divalent nickel ions Granted publication date: 20191126 License type: Common License Record date: 20231101 |