CN113324958A - Rapid detection capillary tube for visually detecting heavy metal mercury and preparation method and application thereof - Google Patents
Rapid detection capillary tube for visually detecting heavy metal mercury and preparation method and application thereof Download PDFInfo
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- CN113324958A CN113324958A CN202110546853.5A CN202110546853A CN113324958A CN 113324958 A CN113324958 A CN 113324958A CN 202110546853 A CN202110546853 A CN 202110546853A CN 113324958 A CN113324958 A CN 113324958A
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- capillary tube
- capillary
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- phycocyanin
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/286—Phases chemically bonded to a substrate, e.g. to silica or to polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
Abstract
The invention discloses a quick detection capillary tube for visually detecting heavy metal mercury as well as a preparation method and application thereof, and belongs to the technical field of mercury ion detection. The capillary tube is used as a carrier of phycocyanin and is subjected to surface amino silanization modification, so that the phycocyanin and the glass carrier are firmly combined, and the quick detection capillary tube for visually detecting heavy metal mercury is prepared. The quick detection capillary tube is used for detecting Hg in a liquid sample2+The rapid detection is realized without using any complex nano material or probe system or expensive processing equipment, so that the processing cost is saved; has obvious phenomenon in detection, has the advantages of high sensitivity, good selectivity, simple operation and the like, and is used in real samplesIt is also suitable for use.
Description
Technical Field
The invention relates to a quick detection capillary tube for visually detecting heavy metal mercury as well as a preparation method and application thereof, belonging to the technical field of mercury ion detection.
Background
Heavy metals are a major environmental pollutant with a potential risk of causing serious toxic effects in the human body. The aqueous environment, which refers to groundwater and drinking water, is the main source of accumulation of heavy metals, where the metals become part of the food chain through absorption. Food products such as fish, leafy vegetables and rice are often contaminated with heavy metals. Heavy metals are not biodegradable in nature, so they can accumulate in water and in animals and cause toxicity to humans. Mercury is a heavy metal known for its toxicity at low concentrations. Mercury ion (Hg)2+) Its presence in water and food is very common. Therefore, there is a need to develop an advanced Hg2+Rapid detection method, in particular for Hg in aqueous environments2+And (6) detecting.
At present, an atomic absorption method, a differential potential dissolution method, an electrode method, a gas chromatography method, a spectrophotometry method and the like are used for detecting heavy metals, although the methods are sensitive and accurate, the methods generally have the defects of complicated pretreatment, expensive required instruments and equipment, long detection time and high detection technical requirement, and are difficult to be applied to the field rapid detection of environmental samples such as food, water samples and the like.
The rapid detection products in the current market are mostly test strip products, including colloidal gold test strips and fluorescent test strips. The fluorescence method has higher detection sensitivity than the colloidal gold test strip in the detection principle, but needs to be assisted by a fluorescence reading device, the synthesis of a probe is more complicated and the like, and the fluorescent test strip products in the market are fewer. Therefore, a fluorescent fast-detection product which is more convenient to manufacture and use is to be developed. In addition, the test paper strip manufacturing process needs to use expensive equipment such as a film cutting machine and a strip cutting machine. Therefore, the development of a quick-detection product prepared at low cost has practical significance.
Therefore, the development of an environment-friendly, simple, sensitive, practical and visual carrier is realized for rapidly detecting Hg2+The key of the method is. The capillary has the advantages of high light transmittance, flexible surface functional group fixing mode and the like, and is a product form with market potential by combining fluorescent protein to develop a fluorescent quick detection product based on the capillary.
Disclosure of Invention
To solve the above problems, we developed a detection device using Phycocyanin (PC) as a protein sensor and capillary as a carrier, which is environment-friendly and easily available, for detecting Hg in a liquid sample2+The content is subjected to ultra-sensitive and selective detection, and the visualization of the detection result can be realized without using any complex nano material or probe system and expensive processing equipment. At present, no report of using phycocyanin to detect mercury ions by taking a capillary tube as a carrier exists.
The invention provides a quick-detection capillary tube for visually detecting heavy metal mercury, which is prepared by the following steps:
(1) soaking the capillary tube in a solution containing a silane coupling agent, taking out, washing and drying after the soaking is finished; then placing the capillary tube in a Glutaraldehyde (GA) aqueous solution for soaking, taking out after the soaking is finished, washing and drying to obtain a modified capillary tube;
(2) diluting phycocyanin by using a buffer solution to prepare a phycocyanin solution; and then immersing the modified capillary tube into phycocyanin solution, and obtaining the quick-detection capillary tube after immobilization treatment.
In one embodiment of the invention, the method further comprises pre-treating the capillary: and cleaning the glass substrate by using a cleaning agent to remove surface dirt.
In one embodiment of the invention, the pretreatment is to wash the capillary with a 25% NaOH solution by mass fraction.
In one embodiment of the present invention, the solution containing a silane coupling agent is a 3 mass% solution of 3-Aminopropyltriethoxysilane (ATPES).
In one embodiment of the invention, the aqueous Glutaraldehyde (GA) solution has a mass fraction of 25%.
In one embodiment of the invention, the buffer is Tris buffer; wherein the pH value of the Tris buffer solution is 6.
In one embodiment of the present invention, the concentration of phycocyanin in the phycocyanin solution is 0.5-0.8 mg/mL.
In one embodiment of the present invention, the phycocyanin solution is preferably obtained by diluting 200. mu.L of a phycocyanin aqueous solution having a concentration of 2.5mg/mL with 700. mu.L of Tris buffer (tris).
In an embodiment of the present invention, the phycocyanin solution may be prepared by mixing 1mg phycocyanin and 500 μ L deionized water.
In one embodiment of the invention, the temperature condition of the immobilization is 30 ℃, the rotating speed is 160r/min, and the time of immobilization is 2 h.
In one embodiment of the present invention, the drying in step (1) is performed at 100-120 ℃ for 1-3 h. Furthermore, the drying can be controlled to be fully performed in a nitrogen environment.
Another object of the present invention is to provide a method for detecting mercury ions, the method comprising the steps of:
and immersing a section of tube opening of the quick detection capillary tube into the sample liquid, placing the capillary tube under an ultraviolet lamp of 365nm after the capillary tube sucks the sample, and observing whether red fluorescence is presented or not.
In one embodiment of the invention, when there is no significant red fluorescence, then mercury ions are present at a level above 60 nM; when the fluorescence is obviously red, the content of mercury ions is lower than 60 nM.
In one embodiment of the invention, the capillary suction sample has an adsorption height of 20. + -.5 mm and a fixed protein content of 0.18-0.28 mg.
Has the advantages that:
the invention uses a visual capillary as a carrier of phycocyanin, and uses surface amino silanization modification to firmly combine protein and glass carrier for Hg in a liquid sample2+The rapid detection of the method does not need to use any complex nano material or probe system, does not need expensive processing equipment, and saves the processing cost. The method has the advantages of obvious phenomenon, high sensitivity, good selectivity, simple operation and the like, and is also applicable to real samples.
Drawings
FIG. 1 is a graph comparing contact angles before and after treatment with a 3% ATPES solution.
FIG. 2 is a graph showing the results of the capillary tube with the sample adsorbed thereon under an ultraviolet lamp.
FIG. 3 is a graph showing the relationship between the contact angle and the concentration of the silane coupling agent.
Detailed Description
Example 1 a fast detection capillary for detecting mercury was prepared:
and cleaning the glass substrate by using a cleaning agent to remove surface dirt. Preparing a NaOH solution with the mass fraction of 25%; soaking a capillary tube with the specification of 100mm, the inner diameter of 1.8mm and the outer diameter of 2.2mm in a 25% NaOH solution for reaction for 30 min.
Placing the pretreated capillary tube into 3% ATPES solution, soaking for 30min, taking out, thoroughly cleaning with anhydrous ethanol, and drying in a 120 deg.C drying oven for 1.5 h. As in fig. 1, it can be seen that the degree of capillary contact angle change is significant in the 3% ATPES solution.
The capillary was completely immersed in an aqueous solution of Glutaraldehyde (GA) having a mass fraction of 25% overnight, then thoroughly washed with ultrapure water and thoroughly dried with nitrogen GAs. Preparing phycocyanin solution (2mg/mL) according to the proportion of 1mg phycocyanin to 500 mu L deionized water, immersing the treated capillary into the phycocyanin solution, and placing the capillary on a shaking bed for immobilization for 2h (the temperature is 30 ℃, and the rotating speed is 160r/min), thus obtaining the capillary detection tube. And placing the prepared capillary detection tube into a drying agent for sealing and standby.
Example 2 detection of mercury ions using a mercury detection capillary:
the detection capillary mouth obtained in example 1 is contacted with a liquid sample to be detected, the capillary is used for sucking the sample to the adsorption height of 20mm (the fixed protein content is 0.18-0.28mg), and the sucked sample (No. 1-6 samples contain Hg)2+0nM, 30nM, 40nM, 50nM, 60nM, 70nM) respectively) was observed to exhibit red fluorescence under a 365nM ultraviolet lamp. If the red fluorescence intensity of sample tube No. 1 in FIG. 2 is high, Hg is not contained2+And the No. 2-6 sample tubes have low red fluorescence intensity and gradually reduced fluorescence intensity, the detection limit of the capillary tube is 25-30nM, and the detection process only needs a few minutes.
Example 3 Effect of different concentrations of pretreatment solution and silane coupling agent on the contact angle of capillary surface after treatment
Referring to example 1, the mass fraction of NaOH in the pretreatment solution NaOH solution was changed, and the results of the specific detection performances were not changed, as shown in Table 1 below. It can be seen that the capillary contact angle is the smallest in a 25% NaOH solution. Therefore, this condition is used as the optimum pretreatment condition.
TABLE 1 contact angle test results after treatment of NaOH solutions of different concentrations
Note: the smaller the contact angle, the more wetting the liquid on the capillary glass surface, and the easier the phycocyanin is adsorbed.
Referring to example 1, only the concentration of the silane coupling agent was changed, and the other properties were not changed, and the results of the specific measurements are shown in FIG. 3 and Table 2. It can be seen that the capillary contact angle is the smallest in a 3% ATPES solution. Therefore, the solution under these conditions is used as the optimum silane coupling agent.
TABLE 2 contact Angle test results after treatment with different coupling agents
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A fast detection capillary tube for visually detecting heavy metal mercury is characterized in that a preparation method of the fast detection capillary tube comprises the following steps:
(1) soaking the capillary tube in a solution containing a silane coupling agent, taking out, washing and drying after the soaking is finished; then placing the capillary tube in a glutaraldehyde aqueous solution for soaking, taking out after the soaking is finished, washing and drying to obtain a modified capillary tube;
(2) diluting phycocyanin by using a buffer solution to prepare a phycocyanin solution; and then immersing the modified capillary tube into phycocyanin solution, and obtaining the quick-detection capillary tube after immobilization treatment.
2. The fast detection capillary according to claim 1, wherein the pretreatment is a washing of the capillary with a 25% NaOH solution by mass fraction.
3. The capillary for rapid detection according to claim 1, wherein the solution containing the silane coupling agent is a 3 mass% solution of 3-aminopropyltriethoxysilane.
4. The rapid detection capillary according to claim 1, wherein the glutaraldehyde aqueous solution has a mass fraction of 25%.
5. The capillary for rapid test according to claim 1, wherein the concentration of phycocyanin in the phycocyanin solution is 0.5-0.8 mg/mL.
6. The rapid detection capillary according to claim 1, wherein the temperature condition of immobilization is 30 ℃, the rotation speed is 160r/min, and the time of immobilization is 2 h.
7. The fast detection capillary according to any one of claims 1 to 7, wherein the method further comprises pre-treating the capillary: and cleaning the glass substrate by using a cleaning agent to remove surface dirt.
8. A method for visually and rapidly detecting mercury ions is characterized by comprising the following processes:
immersing the one-end nozzle of the rapid-detection capillary tube of any one of claims 1 to 7 in the sample liquid, and observing whether red fluorescence appears after the capillary tube sucks in the sample and placing under an ultraviolet lamp of 365 nm.
9. The method of claim 8, wherein in the absence of significant red fluorescence, mercury ions are present at a level of greater than 60 nM; when the fluorescence is obviously red, the content of mercury ions is lower than 60 nM.
10. The method of claim 8, wherein the capillary suction sample has an adsorption height of 20 ± 5mm and a fixed protein content of 0.18-0.28 mg.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110546853.5A CN113324958A (en) | 2021-05-19 | 2021-05-19 | Rapid detection capillary tube for visually detecting heavy metal mercury and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110546853.5A CN113324958A (en) | 2021-05-19 | 2021-05-19 | Rapid detection capillary tube for visually detecting heavy metal mercury and preparation method and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080166792A1 (en) * | 2007-01-05 | 2008-07-10 | Attar Amir J | Detection of analytes in materials liquids using capillary colorimetric detection |
| CN101713737A (en) * | 2009-12-29 | 2010-05-26 | 东北师范大学 | Fluorescent detection probe for mercury ions and application method thereof |
| US20140256573A1 (en) * | 2011-03-09 | 2014-09-11 | Abionic Sa | Rapid quantification of biomolecules in a selectively functionalized nanofluidic biosensor and method thereof |
| CN110947372A (en) * | 2019-12-16 | 2020-04-03 | 成都普利泰生物科技有限公司 | Capillary tube surface amination method |
-
2021
- 2021-05-19 CN CN202110546853.5A patent/CN113324958A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080166792A1 (en) * | 2007-01-05 | 2008-07-10 | Attar Amir J | Detection of analytes in materials liquids using capillary colorimetric detection |
| CN101713737A (en) * | 2009-12-29 | 2010-05-26 | 东北师范大学 | Fluorescent detection probe for mercury ions and application method thereof |
| US20140256573A1 (en) * | 2011-03-09 | 2014-09-11 | Abionic Sa | Rapid quantification of biomolecules in a selectively functionalized nanofluidic biosensor and method thereof |
| CN110947372A (en) * | 2019-12-16 | 2020-04-03 | 成都普利泰生物科技有限公司 | Capillary tube surface amination method |
Non-Patent Citations (5)
| Title |
|---|
| YUBIN ZHAO等: "A SERS-based capillary sensor for the detection of mercury ions in environmental water", 《SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY》 * |
| 张何等: "一种基于钝顶螺旋藻藻蓝蛋白荧光猝灭法的汞离子传感新方法", 《分析测试学报》 * |
| 徐开先等: "《传感器实用技术》", 31 December 2016, 国防工业出版社 * |
| 李永生等: "一种用于化学分析的新方法——荧光毛细分析法", 《光谱学与光谱分析》 * |
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Application publication date: 20210831 |