CN106568773B - Manganese ion colorimetric detection kit and detection method thereof - Google Patents
Manganese ion colorimetric detection kit and detection method thereof Download PDFInfo
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- 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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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention relates to the technical field of environmental and biological analysis, in particular to a manganese ion colorimetric detection kit and a detection method thereof. The kit comprises an acetic acid-sodium acetate buffer solution, a potassium periodate solution, an aminotriacetic acid solution, a gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), a standard colorimetric card C and a colorimetric tube; in the gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), the concentration of the nanorods is 0.5-10nM, and the concentration of the CTAB is 0.01-100 mM. The method for detecting the manganese ions has the advantages of high sensitivity, good selectivity, simplicity in operation, easiness in observation by naked eyes and the like, and can realize the detection of the manganese ions in the environmental sample under the debugging of the experimental conditions of the system.
Description
Technical Field
The invention relates to the technical field of environmental and biological analysis, in particular to a manganese ion colorimetric detection kit and a detection method thereof.
Background
Manganese is one of the essential trace elements of the human body, plays an important role in the composition of many enzymes, and is also an essential component of normal bone structure. Manganese deficiency can cause neurasthenia, and even lead to a decrease in insulin and synthesis and secretion; excessive manganese can cause poisoning, occupational manganese poisoning is caused by long-term inhalation of manganese smoke and manganese dust containing high manganese depth, and particularly workers in ferromanganese smelting, manufacturing and electric welding of welding electrodes, mining, crushing or dry battery production of manganese ores and the like can cause neurological symptoms like Parkinson's disease or Wilson's disease and the like after long-term manganese contact. Therefore, the detection of manganese ions in environmental and biological samples is very important.
In a water body environment, because manganese ions can not be decomposed, the manganese ions have biological enrichment and biological amplification effects in organisms, so that the content of the manganese ions in the organisms with higher food chains is also multiplied, and the harm to the organisms is larger. Human beings who are at the top of the food chain are also most harmed when eating these aquatic organisms containing heavy metal ions at high concentrations. Therefore, the detection of manganese ions in environmental and water body samples is very necessary.
At present, the detection means for manganese ions mainly include atomic absorption methods, catalytic photometry, fluorescence spectrophotometry, chemiluminescence methods, inductively coupled plasma mass spectrometry and other methods. However, these techniques require expensive large-scale instruments, or the detection means are too complicated to realize field detection and technical popularization. Compared with the detection technology, the colorimetric analysis method has the advantages that the visual observation is easy, the colorimetric analysis method is very suitable for the field real-time detection, the operation is simple, and the price is low. The gold nanoparticles have very large molar extinction coefficient due to surface plasmon resonance absorption, so that the gold nanoparticles have obvious advantages in colorimetric analysis.
Disclosure of Invention
The invention aims to provide a manganese ion colorimetric detection kit and a detection method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a manganese ion colorimetry detection kit comprises an acetic acid-sodium acetate buffer solution, a potassium periodate solution, an aminotriacetic acid solution, a gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), a standard colorimetric card C and a colorimetric tube;
in the gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), the concentration of the nanorods is 0.5-10nM, and the concentration of the CTAB is 0.01-100 mM.
The pH of the acetic acid-sodium acetate buffer solution is 3.6-5.8, and the solution concentration is 0.01-1M;
the concentration of the potassium periodate solution is 0.01-1M;
the concentration of the amino-triethyl acid solution is 0.01-1M.
Preferably, the pH of the acetic acid-sodium acetate buffer solution in the kit is 5.4, and the concentration is 50 mM; in gold nanorod solution containing cetyl ammonium bromide (CTAB), the concentration of the gold nanorods is 2.3nM, the length-diameter ratio is 2:1, and the concentration containing CTAB is 0.1M; the concentration of the potassium periodate solution is 0.02M; the concentration of the solution of the amino-triethyl acid was 0.01M.
The standard colorimetric card C is manganese standard color-scale solution with different concentrations of 0nM,5nM,10nM,15nM,20nM,25nM,30nM,40nM,50nM and 100nM respectively.
A method for detecting manganese ions by a manganese ion colorimetric detection kit comprises the steps of adding an acetic acid-sodium acetate buffer solution into a colorimetric tube, adding a sample to be detected, shaking and uniformly mixing, adding a gold nanorod solution containing CTAB after uniformly mixing, and shaking uniformly; sequentially adding a potassium periodate solution and an ammonia-troacetic acid solution, shaking and uniformly mixing; and then incubating for 10-30 minutes at the temperature of 20-40 ℃, carrying out color reaction, observing the color by naked eyes or an ultraviolet visible spectrometer, and comparing with a standard color comparison card C to determine the content of manganese ions.
In the gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), the concentration of the nanorods is 0.5-10nM, and the concentration of the CTAB is 0.01-100 mM.
The pH of the acetic acid-sodium acetate buffer solution is 3.6-5.8, and the solution concentration is 0.01-1M;
the concentration of the potassium periodate solution is 0.01-1M;
the concentration of the amino-triethyl acid solution is 0.01-1M.
The pH value of the acetic acid-sodium acetate buffer solution in the kit is 5.4, and the concentration is 50 mM; in gold nanorod solution containing cetyl ammonium bromide (CTAB), the concentration of the gold nanorods is 2.3nM, the length-diameter ratio is 2:1, and the concentration containing CTAB is 0.1M; the concentration of the potassium periodate solution is 0.02M; the concentration of the solution of the amino-triethyl acid was 0.01M.
The standard colorimetric card C is manganese standard color-scale solution with different concentrations of 0nM,5nM,10nM,15nM,20nM,25nM,30nM,40nM,50nM and 100nM respectively.
The preparation of the standard colorimetric card C comprises the steps of putting 0-100nM manganese standard color-scale solutions with different concentrations into a colorimetric tube respectively, adding an acetic acid-sodium acetate buffer solution, shaking and mixing uniformly, adding a gold nanorod solution containing CTAB after mixing uniformly, and shaking uniformly; sequentially adding a potassium periodate solution and an ammonia-troacetic acid solution, shaking and uniformly mixing; and then incubating for 10-30 minutes at the temperature of 20-40 ℃ for color reaction, recording the color development result by using a professional camera, and collecting pictures to form a manganese ion standard color comparison card C by using pictures with color gradients.
The principle of the invention (shown in figure 1) is that in an acid solution, nitrilotriacetic acid is used as an activator, manganese ions catalyze potassium periodate to oxidize gold nanorods to generate trivalent manganese ions, and the trivalent manganese ions are reduced to manganese ions, so that the gold nanorods are etched in a circulating catalytic manner, the absorption spectrum of the gold nanorods is changed (shown in figure 3) and is accompanied by obvious morphological change (shown in figure 2) and color change (shown in figure 4), and the change is in a linear relation with the concentration of the manganese ions (shown in figure 5).
The invention has the advantages that:
the method for detecting the manganese ions by using the manganese ion catalytic etching gold nanorod colorimetric method has the advantages of high sensitivity (detection limit of 10nM), good selectivity, simplicity in operation, high speed, easiness in observation by naked eyes, suitability for field real-time detection and the like.
Drawings
FIG. 1 shows the principle of manganese ion catalytic etching of gold nanorods.
FIG. 2 is a transmission electron microscope image before and after manganese ion catalytic etching of gold nanorods, according to an embodiment of the present invention; wherein, the gold nanorods are arranged before (left) and after (middle is low concentration, right is high concentration) manganese ion catalytic etching.
Fig. 3 is an absorption spectrum of gold nanorods catalytically etched by manganese ions (with a concentration from low to high) according to an embodiment of the present invention.
Fig. 4 is a manganese ion standard color comparison card C provided in the embodiment of the present invention.
FIG. 5 is a standard curve for detecting manganese ions according to the present invention.
Fig. 6 is a graph showing the results of a selective experiment (fig. 6A) and a corresponding photograph (fig. 6B) for detecting manganese ions according to an embodiment of the present invention.
Fig. 7 is a flowchart for detecting the flow of manganese ions according to an embodiment of the present invention.
Detailed Description
The present invention is further illustrated in detail by the following examples. The invention is in no way limited thereto.
The kit adopts weak acid acetic acid with pH of 3.6-5.8 and concentration of 0.01-1M to enable potassium periodate oxidation reaction catalyzed by manganese to be in a weak acid condition, and the gold nanorods are modified by CTAB, wherein CTAB has sensitization effect as a surfactant and nitrilotriacetic acid with catalysis assistance effect, the gold nanorods are blue under a normal state in the reaction process, after being oxidized and etched by potassium periodate, the shape of the gold nanorods is changed from a rod shape to a sphere shape, the color of the gold nanorods is changed from blue to red, the change and the concentration change of manganese ions added as a catalyst present a certain linear relation, and the detection of the manganese ions is carried out according to the linear relation.
Examples manganese ion (spiked) detection in Drinking Water
The kit comprises an acetic acid-sodium acetate buffer solution, a potassium periodate solution, an aminotriacetic acid solution, a gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), a standard colorimetric card C and a colorimetric tube;
the acetic acid-sodium acetate buffer solution is prepared by using analytically pure sodium acetate and glacial acetic acid and using secondary deionized water, and the pH value of the prepared buffer solution is 5.4, and the concentration is 50 mM.
The concentration of the potassium periodate solution is 0.02M, and the potassium periodate solution is obtained by dissolving analytically pure potassium periodate in secondary deionized water;
the concentration of the aminotriacetic acid solution is 0.01M, and the aminotriacetic acid solution is obtained by dissolving analytically pure aminotriacetic acid in secondary deionized water;
gold nanorod solutions containing cetyltrimethylammonium bromide (CTAB) were prepared as follows:
1) synthesizing a gold seed solution: adding 50 mu L of chloroauric acid solution (50mM) into 7.7mL of 0.1M hexadecyltrimethylammonium bromide (CTAB) solution, stirring and shaking uniformly, adding 600 mu L of sodium borohydride (0.01M) solution for accelerated shaking for a few minutes, stopping when the color of the mixed solution is changed from bright yellow to purple gray, and standing for 2 hours at 26 ℃ for later use.
2) And (3) nanorod synthesis: adding 1200 mu L of chloroauric acid (50mM) solution into 100mL of 0.1M hexadecyltrimethylammonium bromide (CTAB) solution, uniformly stirring, adding 300 mu L of silver nitrate (0.01M) solution, uniformly mixing, adding 960 mu L of ascorbic acid (0.1M) solution, stirring and adding 200 mu L of the synthesized gold seed solution to the solution when the solution is colorless from yellow brown, continuously stirring until the color of the solution is gradually changed from colorless to blue green, stopping stirring, and standing for 20 hours to obtain the gold nanorods. From the transmission mirror, the length-diameter ratio of the gold nanorods is about 2:1 (see figure 2 (left)), the radial absorption peak of the ultraviolet-visible absorption spectrogram is 660nM-670nM (see figure 3 absorption spectrogram), and the concentration of the nanorods is estimated to be 2.3nM according to the Lambert beer law.
Standard color card C was prepared by preparing 10. mu.L of a manganese standard gradation solution at a concentration of 0nM,5nM,10nM,15nM,20nM,25nM,30nM,40nM,50nM,100 nM.
Namely a kit:
acetic acid-sodium acetate buffer solution, pH 5.4, concentration 50 mM;
potassium periodate solution with concentration of 0.02M;
a solution of glycine and acetic acid, at a concentration of 0.01M;
2mL of colorimetric tube;
a glass graduated straw;
manganese standard color-scale solution;
manganese standard colorimetric card.
The detection method comprises the following steps: respectively adding the gold nanorods into colorimetric tubes filled with 1mL of acetic acid-sodium acetate buffer solution, shaking and uniformly mixing, adding the gold nanorods containing CTAB, and shaking uniformly; then respectively adding potassium periodate solution and aminotriacetic acid solution, shaking and uniformly mixing; after mixing evenly, adding gold nanorod solution containing CTAB, and shaking evenly; and then incubating for 10-30 minutes at the temperature of 20-40 ℃, carrying out color reaction, recording a color development result by using a professional camera, collecting pictures, forming a manganese standard color comparison card C (shown in figure 4) by using the pictures with color gradients, simultaneously collecting corresponding ultraviolet-visible absorption spectrograms, and preparing a standard curve according to peak displacement (shown in figure 5).
Specifically, detecting manganese ions (labeled) in drinking water:
(1) taking 2.0mL of colorimetric tubes, adding 1mL of acetic acid-sodium acetate buffer solution into each colorimetric tube, respectively adding 10 mu L of a manganese ion labeling sample containing three different concentrations, uniformly shaking, labeling No. 1, No. 2 and No. 3, respectively adding gold nanorods containing CTAB, and uniformly shaking;
(2) sequentially adding a potassium periodate solution and a nitrilotriacetic acid solution, and uniformly mixing by shaking;
(3) incubating at 20-40 deg.C for 10-30 min,
(3) observing the color change, comparing the colorimetric tube with a standard colorimetric card C to determine the concentration range of the manganese ions in the drinking water added standard sample, and showing that the concentration of the manganese ions is correspondingly consistent with that of the colorimetric card; meanwhile, peak shift can be obtained through an external visible spectrogram, the determined content of the manganese ions is determined according to a standard curve, the standard recovery rate of the detection result of the method is 85-103% (see table 1), and the reliability of the practical application of the method is illustrated.
TABLE 1 manganese ion spiking test results
Claims (4)
1. A manganese ion colorimetric detection kit is characterized in that: the kit comprises an acetic acid-sodium acetate buffer solution, a potassium periodate solution, an aminotriacetic acid solution, a gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), a standard colorimetric card C and a colorimetric tube;
in the gold nanorod solution containing Cetyl Trimethyl Ammonium Bromide (CTAB), the concentration of the nanorods is 2.3nM, the length-diameter ratio is 2:1, and the CTAB concentration is 0.1M;
the pH of the acetic acid-sodium acetate buffer solution is 5.4, and the solution concentration is 50 mM;
the concentration of the potassium periodate solution is 0.02M;
the concentration of the amino-triethyl acid solution is 0.01M;
the standard colorimetric card C is manganese standard color-scale solution with different concentrations of 0nM,5nM,10nM,15nM,20nM,25nM,30nM,40nM,50nM and 100nM respectively.
2. The method for detecting manganese ions by using the manganese ion colorimetric detection kit according to claim 1, which is characterized in that: adding acetic acid-sodium acetate buffer solution into a colorimetric tube, adding a sample to be detected, uniformly mixing, adding a gold nanorod solution containing CTAB, and uniformly mixing; sequentially adding a potassium periodate solution and an ammonia-troacetic acid solution, shaking and uniformly mixing; and then incubating for 10-30 minutes at the temperature of 20-40 ℃, carrying out color reaction, observing the color by naked eyes or an ultraviolet visible spectrometer, and comparing with a standard color comparison card C to determine the content of manganese ions.
3. The method for detecting manganese ions by using the manganese ion colorimetric detection kit according to claim 2, wherein the method comprises the following steps: the pH value of the acetic acid-sodium acetate buffer solution in the kit is 5.4, and the concentration is 50 mM; in gold nanorod solution containing cetyl ammonium bromide (CTAB), the concentration of the gold nanorods is 2.3nM, the length-diameter ratio is 2:1, and the concentration containing CTAB is 0.1M; the concentration of the potassium periodate solution is 0.02M; the concentration of the solution of the amino-triethyl acid was 0.01M.
4. The method for detecting manganese ions by using the manganese ion colorimetric detection kit according to claim 3, wherein the method comprises the following steps: the standard colorimetric card C is manganese standard color-scale solution with different concentrations of 0nM,5nM,10nM,15nM,20nM,25nM,30nM,40nM,50nM and 100nM respectively.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078688A (en) * | 2007-05-31 | 2007-11-28 | 中国铝业股份有限公司 | Method for determining phosphor and manganese of ferro-phosphorus |
| CN101625312A (en) * | 2008-07-09 | 2010-01-13 | 苏州艾杰生物科技有限公司 | Manganese ion diagnostic/assay kit and method for assaying concentration of manganese ions |
| CN103278497A (en) * | 2013-05-15 | 2013-09-04 | 中国科学院烟台海岸带研究所 | Copper ion colorimetry detecting kit and detecting method thereof |
| 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 |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN104215595A (en) * | 2014-09-17 | 2014-12-17 | 陕西华陆化工环保有限公司 | Method for detecting trace manganese in environmental sample |
-
2016
- 2016-11-22 CN CN201611031910.1A patent/CN106568773B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078688A (en) * | 2007-05-31 | 2007-11-28 | 中国铝业股份有限公司 | Method for determining phosphor and manganese of ferro-phosphorus |
| CN101625312A (en) * | 2008-07-09 | 2010-01-13 | 苏州艾杰生物科技有限公司 | Manganese ion diagnostic/assay kit and method for assaying concentration of manganese ions |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN103278497A (en) * | 2013-05-15 | 2013-09-04 | 中国科学院烟台海岸带研究所 | Copper ion colorimetry detecting kit and detecting method thereof |
| 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 |
| CN104215595A (en) * | 2014-09-17 | 2014-12-17 | 陕西华陆化工环保有限公司 | Method for detecting trace manganese in environmental sample |
Non-Patent Citations (2)
| Title |
|---|
| Fenton-like Reaction-Mediated Etching of Gold Nanorods for Visual Detection of Co2+;Zhiyang Zhang et al.;《Langmuir》;20141208;第643？650页 * |
| 污水中锰的动力学分光光度法测定;王尊本等;《分析化学》;19860630;第14卷(第6期);第467-468页 * |
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