CN103884701A - Mercury ion detection method - Google Patents

Mercury ion detection method Download PDF

Info

Publication number
CN103884701A
CN103884701A CN201410140977.3A CN201410140977A CN103884701A CN 103884701 A CN103884701 A CN 103884701A CN 201410140977 A CN201410140977 A CN 201410140977A CN 103884701 A CN103884701 A CN 103884701A
Authority
CN
China
Prior art keywords
mercury ion
solution
gold nanoclusters
detection method
gold
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410140977.3A
Other languages
Chinese (zh)
Inventor
刘萍萍
周会娜
陈千思
翟妞
金立锋
陈霞
郑庆霞
林福呈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhengzhou Tobacco Research Institute of CNTC
Original Assignee
Zhengzhou Tobacco Research Institute of CNTC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhengzhou Tobacco Research Institute of CNTC filed Critical Zhengzhou Tobacco Research Institute of CNTC
Priority to CN201410140977.3A priority Critical patent/CN103884701A/en
Publication of CN103884701A publication Critical patent/CN103884701A/en
Pending legal-status Critical Current

Links

Images

Abstract

The invention discloses a mercury ion detection method which is characterized by comprising the following steps: (1) mixing a standard mercury ion solution and a gold nanocluster solution, and establishing a standard curve for detecting the fluorescence signal quenching of nanocluster and the mercury ion quantity; and (2) mixing a sample solution with the gold nanocluster solution, substituting the quenching intensity of the fluorescence signal of the nanocluster into the standard curve, thereby obtaining the content of the mercury ion in the sample. The method has the advantages that the sensitivity is high, the interference of other ions on detection of the mercury ion is slight, and selective detection of the mercury ion can be realized, so that the aim of rapidly detecting the mercury ion concentration is achieved. The method has wide application prospects in mercury ion detection.

Description

A kind of detection method of mercury ion
 
Technical field
The present invention relates to harmful ion and detect, specifically a kind of detection method of mercury ion.
Background technology
The detection of mercury ion is significant to environment and human health.
At present, the detection method of mercury mainly contains Atomic absorption/emission spectrum, X diffraction fluorescence spectrum, inductively coupled plasma mass spectrometry and the cold steam atomic fluorescence spectrophotometry of selectivity etc., has the drawback of required instrument costliness.
Therefore, develop efficient, cheap, mercury detection technique becomes important in recent years research topic easily and efficiently.
goal of the invention
The detection method of a kind of mercury ion that object of the present invention provides based on above-mentioned prior art situation just, utilizes the method can realize the fast detecting of ion concentration of mercury.
The object of the invention is to be achieved through the following technical solutions:
A detection method for mercury ion, comprises the steps:
1) standard mercury ion solution and gold nanoclusters solution are mixed, set up the typical curve between fluorescence signal cancellation and the mercury ion amount that detects nano-cluster;
2) unknown concentration mercury ion sample solution and gold nanoclusters solution are mixed, bring the fluorescence signal cancellation intensity that detects nano-cluster into typical curve, obtain the content of mercury ion in sample.
The series concentration scope of described standard mercury ion solution is: 12499.2-24.425 nM(nanomole).
Described gold nanoclusters solution is formulated by the following method: gold nanoclusters is dissolved in PBS, regulates pH value to 3-4.5, obtain gold nanoclusters solution; The concentration of gold nanoclusters in solution is calculated as 0.5-2 mM with gold ion concentration.
In the preparation of gold nanoclusters solution, be to regulate pH value by the aqueous solution of phosphoric acid or sodium dihydrogen phosphate.
The structure of described gold nanoclusters is as follows: described gold nanoclusters is modified by human albumin HSA parcel, and decorative layer is HSA, and the particle diameter of described gold nanoclusters is 3-5 nm; The emission wavelength of gold nanoclusters is 725 nm; The excitation wavelength of gold nanoclusters is 500-550nm.
Described gold nanoclusters is also that quantum dot is prepared as follows:
1) in 0.5mL 10 mM gold chlorides, add 0.5 mL 50 mg/mL human albumin HSA, magnetic stirs,
2) above-mentioned solution is regulated to pH=12 with NaOH;
3) microwave is synthetic, and 300w, the time of 100s, obtains described gold nanoclusters.
While detecting fluorescence, instrument is Fluorescence spectrophotometer.
The invention has the advantages that: highly sensitive, other ion pair mercury ion detecting are disturbed little, can realize the selectivity detection to mercury ion, thereby reach the object of fast detecting ion concentration of mercury.This invention has broad application prospects in the detection of mercury ion.
Brief description of the drawings
Fig. 1 is the phenogram of the present invention's quantum dot used, and wherein: A is quantum dot transmission electron microscope picture, B is fluorescent exciting spectrogram.
Fig. 2 is the interference test that gold nanoclusters detects mercury ion, wherein: A is that each metallic ion adds fluorogram after nano-cluster.B is fluorescence intensity level figure.
Fig. 3 is that different ion concentration of mercury detect the fluorescence emission spectrogram in solution at gold nanoclusters.
Fig. 4 is ion concentration of mercury and gold nanoclusters fluorescence intensity graph of a relation and range of linearity figure, wherein: A is ion concentration of mercury and nano-cluster fluorescence intensity cancellation graph of a relation.B is range of linearity figure.
Embodiment
The present invention is described further below in conjunction with accompanying drawing:
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
Intermediate water described in literary composition (conductivity 18.2 M Ω) is ultrapure water.
A detection method for mercury ion, comprises the steps:
1) standard mercury ion solution and gold nanoclusters solution are mixed, set up the typical curve between fluorescence signal cancellation and the mercury ion amount that detects nano-cluster;
2) sample solution and gold nanoclusters solution are mixed, bring the fluorescence signal cancellation intensity that detects nano-cluster into typical curve, obtain the content of mercury ion in sample.
The series concentration of described standard mercury ion solution is respectively: 24.425,48.83,97065,195.3,390.6,781.2,1562.4,3124.8, and 6249.6,12499.2 nM .
Described gold nanoclusters solution is formulated by the following method: gold nanoclusters is dissolved in PBS, to 3-4.5, obtains gold nanoclusters solution by the aqueous solution adjusting pH value of phosphoric acid or sodium dihydrogen phosphate; The concentration of gold nanoclusters in solution is calculated as 0.5-2 mM with gold ion concentration.
Described gold nanoclusters is also that quantum dot is prepared as follows:
1) in 0.5mL 10 mM gold chlorides, add 0.5 mL 50 mg/mL human albumin HSA, magnetic stirs,
2) above-mentioned solution is regulated to pH=12 with NaOH;
3) microwave is synthetic, and 300w, the time of 100s, obtains described gold nanoclusters.
The gold nanoclusters goods that obtain are light brown clear solution, have good water-soluble.
The structure of described gold nanoclusters is as follows: described gold nanoclusters is modified by human albumin HSA parcel, and decorative layer is HSA, and the particle diameter of described gold nanoclusters is 3-5 nm; The emission wavelength of gold nanoclusters is 725 nm; The excitation wavelength of gold nanoclusters is 500-550nm.
Characterize: transmission electron microscope carries out scanner uni excitation spectrum and emission spectrum to above-mentioned quantum-dot structure, and result as shown in Figure 1.Transmission electron microscope picture shows, the quantum dot of synthesized is spherical in shape, and particle diameter is evenly distributed.
Method: use luminoscope to carry out fluorometric assay, first fixed transmission wavelength is 700 nm, scanning fluorescence excitation spectrum, obtains maximum excitation wavelength 525 nm; Taking 525 nm as excitation wavelength, scan quantum dot fluorescence emission spectrum again.
Result: fluorescence excitation spectrum shows that this quantum dot has wider excitation wavelength range, from 500 nm to 550 nm; Fluorescent emission wavelength is in 725 nm left and right.
Example
1) standard mercury ion solution and gold nanoclusters solution are mixed, set up the typical curve between fluorescence signal cancellation and the mercury ion amount that detects nano-cluster;
2) unknown concentration mercury ion solution and gold nanoclusters solution are mixed, bring the fluorescence signal cancellation intensity that detects nano-cluster into typical curve, obtaining mercury ion fluorescent intensity in sample is 160, by I/I 0be worth 0.727 substitution standard equation, obtaining ion concentration of mercury is 1019.5 nM.

Claims (7)

1. a detection method for mercury ion, is characterized in that: comprise the steps:
1) standard mercury ion solution and gold nanoclusters solution are mixed, set up the typical curve between fluorescence signal cancellation and the mercury ion amount that detects nano-cluster;
2) unknown concentration mercury ion sample solution and gold nanoclusters solution are mixed, bring the fluorescence signal cancellation intensity that detects nano-cluster into typical curve, obtain the content of mercury ion in sample.
2. the detection method of mercury ion according to claim 1, is characterized in that: the series concentration scope of described standard mercury ion solution is: 12499.2-24.425 nM.
3. the detection method of mercury ion according to claim 1, is characterized in that: described gold nanoclusters solution is formulated by the following method: gold nanoclusters is dissolved in PBS, regulates pH value to 4.5, obtain gold nanoclusters solution; The concentration of gold nanoclusters in solution is calculated as 1 mM with gold ion concentration.
4. the detection method of mercury ion according to claim 3, is characterized in that: in the preparation of gold nanoclusters solution, be to regulate pH value by the aqueous solution of phosphoric acid or sodium dihydrogen phosphate.
5. the detection method of mercury ion according to claim 1, is characterized in that: the structure of described gold nanoclusters is as follows: described gold nanoclusters is modified by human albumin HSA parcel, and decorative layer is HSA, and the particle diameter of described gold nanoclusters is 3-5 nm; The emission wavelength of gold nanoclusters is 725 nm; The excitation wavelength of gold nanoclusters is 540nm.
6. the detection method of mercury ion according to claim 5, is characterized in that: described gold nanoclusters is also that quantum dot is prepared as follows:
1) in 0.5mL 10 mM gold chlorides, add 0.5 mL 50 mg/mL human albumin HSA, magnetic stirs,
2) above-mentioned solution is regulated to pH=12 with NaOH;
3) microwave is synthetic, the time of 300W 100s, obtains described gold nanoclusters.
7. the detection method of mercury ion according to claim 1, is characterized in that: while detecting fluorescence, instrument is Fluorescence spectrophotometer.
CN201410140977.3A 2014-04-10 2014-04-10 Mercury ion detection method Pending CN103884701A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410140977.3A CN103884701A (en) 2014-04-10 2014-04-10 Mercury ion detection method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410140977.3A CN103884701A (en) 2014-04-10 2014-04-10 Mercury ion detection method

Publications (1)

Publication Number Publication Date
CN103884701A true CN103884701A (en) 2014-06-25

Family

ID=50953715

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410140977.3A Pending CN103884701A (en) 2014-04-10 2014-04-10 Mercury ion detection method

Country Status (1)

Country Link
CN (1) CN103884701A (en)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104215760A (en) * 2014-09-13 2014-12-17 福建医科大学 Urease inhibitor determination method based on fluorescence gold nano cluster
CN104745194A (en) * 2015-03-24 2015-07-01 南昌大学 Preparation method of quantum dot@Cu nano-cluster ratiometric fluorescent sensor and application thereof in Cu<2+> detection
CN104801722A (en) * 2015-03-13 2015-07-29 武汉理工大学 Preparation method of human serum albumin gold nanoclusters
CN105572087A (en) * 2016-01-11 2016-05-11 东北师范大学 Mercury ion colorimetric detection test paper capable of being cyclically used and application method thereof
CN105675519A (en) * 2016-04-01 2016-06-15 江南大学 Mercury ion detection method
CN106198474A (en) * 2016-07-20 2016-12-07 郑州大学 A kind of mercury ion test paper and using method thereof
CN106908427A (en) * 2017-03-01 2017-06-30 哈尔滨师范大学 Gold nanoclusters and carbon quantum dot composite fluorescence probe and its application
CN107024463A (en) * 2017-06-14 2017-08-08 江南大学 Selective Sensitive Detection mercury ion is used for based on gold nanoclusters ratio fluorescent test strip
CN108303401A (en) * 2017-12-18 2018-07-20 中国烟草总公司郑州烟草研究院 A kind of fluorescence nano composite material and its application in metal ion detection
CN111227799A (en) * 2020-01-21 2020-06-05 中国农业大学 In-vivo detection method for brain tissue methylmercury
CN111375783A (en) * 2020-04-17 2020-07-07 广东医科大学 Multifunctional HSA-cadmium nanocluster, preparation method and application thereof
CN111879747A (en) * 2020-08-21 2020-11-03 中国医学科学院生物医学工程研究所 Mercury ion and copper ion synchronous detection method
CN112170859A (en) * 2020-10-09 2021-01-05 深圳技术大学 Preparation method of gold nanocluster

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101713737A (en) * 2009-12-29 2010-05-26 东北师范大学 Fluorescent detection probe for mercury ions and application method thereof
CN102150034A (en) * 2008-08-05 2011-08-10 新加坡科技研究局 Methods, compositions, and articles comprising stabilized gold nanoclusters
CN103464780A (en) * 2013-09-06 2013-12-25 湖南科技大学 Preparation method of fluorescence gold nano clusters with stable chicken ovalbumin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102150034A (en) * 2008-08-05 2011-08-10 新加坡科技研究局 Methods, compositions, and articles comprising stabilized gold nanoclusters
CN101713737A (en) * 2009-12-29 2010-05-26 东北师范大学 Fluorescent detection probe for mercury ions and application method thereof
CN103464780A (en) * 2013-09-06 2013-12-25 湖南科技大学 Preparation method of fluorescence gold nano clusters with stable chicken ovalbumin

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LEI YAN 等: "Microwave-assisted synthesis of BSA-stabilized and HSA-protected gold nanoclusters with red emission", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 22, 11 November 2011 (2011-11-11), pages 1000 - 1005 *
PO-CHENG CHEN 等: "Synthesis of fluorescent BSA–Au NCs for the detection of Hg2+ ions", 《J NANOPART RES》, vol. 15, 24 December 2012 (2012-12-24), pages 1336 *
杜鹃: "金纳米粒子微波及水热反应合成研究及其在光谱分析中的应用", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, no. 02, 15 February 2014 (2014-02-15) *

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104215760B (en) * 2014-09-13 2016-06-29 福建医科大学 Urease inhibitor assay method based on fluorogold nanocluster
CN104215760A (en) * 2014-09-13 2014-12-17 福建医科大学 Urease inhibitor determination method based on fluorescence gold nano cluster
CN104801722A (en) * 2015-03-13 2015-07-29 武汉理工大学 Preparation method of human serum albumin gold nanoclusters
CN104745194A (en) * 2015-03-24 2015-07-01 南昌大学 Preparation method of quantum dot@Cu nano-cluster ratiometric fluorescent sensor and application thereof in Cu<2+> detection
CN105572087A (en) * 2016-01-11 2016-05-11 东北师范大学 Mercury ion colorimetric detection test paper capable of being cyclically used and application method thereof
CN105675519B (en) * 2016-04-01 2018-02-09 江南大学 A kind of mercury ion detecting method
CN105675519A (en) * 2016-04-01 2016-06-15 江南大学 Mercury ion detection method
CN106198474A (en) * 2016-07-20 2016-12-07 郑州大学 A kind of mercury ion test paper and using method thereof
CN106908427A (en) * 2017-03-01 2017-06-30 哈尔滨师范大学 Gold nanoclusters and carbon quantum dot composite fluorescence probe and its application
CN107024463A (en) * 2017-06-14 2017-08-08 江南大学 Selective Sensitive Detection mercury ion is used for based on gold nanoclusters ratio fluorescent test strip
CN108303401A (en) * 2017-12-18 2018-07-20 中国烟草总公司郑州烟草研究院 A kind of fluorescence nano composite material and its application in metal ion detection
CN111227799A (en) * 2020-01-21 2020-06-05 中国农业大学 In-vivo detection method for brain tissue methylmercury
CN111375783A (en) * 2020-04-17 2020-07-07 广东医科大学 Multifunctional HSA-cadmium nanocluster, preparation method and application thereof
CN111375783B (en) * 2020-04-17 2022-10-11 广东医科大学 Multifunctional HSA-cadmium nanocluster, preparation method and application thereof
CN111879747A (en) * 2020-08-21 2020-11-03 中国医学科学院生物医学工程研究所 Mercury ion and copper ion synchronous detection method
CN111879747B (en) * 2020-08-21 2023-08-22 中国医学科学院生物医学工程研究所 Synchronous detection method for mercury ions and copper ions
CN112170859A (en) * 2020-10-09 2021-01-05 深圳技术大学 Preparation method of gold nanocluster

Similar Documents

Publication Publication Date Title
CN103884701A (en) Mercury ion detection method
CN103264165B (en) A kind of method of synthesizing silver nanoclusters taking single stranded DNA as template
Miao et al. Self-assembly of manganese doped zinc sulfide quantum dots/CTAB nanohybrids for detection of rutin
Ma et al. A novel ascorbic acid sensor based on the Fe 3+/Fe 2+ modulated photoluminescence of CdTe quantum dots@ SiO 2 nanobeads
Ji et al. Label-free detection of Pb 2+ based on aggregation-induced emission enhancement of Au-nanoclusters
Khantaw et al. Selective turn-on fluorescence sensor for Ag+ using cysteamine capped CdS quantum dots: Determination of free Ag+ in silver nanoparticles solution
CN105352925A (en) Copper ions detection method based on nano-cluster
CN104267026A (en) Mercury-ion detection method simulating peroxidase based on nano platinum and kit
Sun et al. Development of a ZnCdS@ ZnS quantum dots–based label-free electrochemiluminescence immunosensor for sensitive determination of aflatoxin B 1 in lotus seed
Bi et al. Room-temperature phosphorescence sensor based on manganese doped zinc sulfide quantum dots for detection of urea
Huang et al. Fast synthesis of porous copper nanoclusters for fluorescence detection of iron ions in water samples
Wang et al. Carbon dot-and gold nanocluster-based three-channel fluorescence array sensor: Visual detection of multiple metal ions in complex samples
He et al. Ratiometric Fluorescent Paper‐Based Sensor Based on CdTe Quantum Dots and Graphite Carbon Nitride Hybrid for Visual and Rapid Determination of Cu2+ in Drinks
Hernández et al. Highly sensitive ratiometric quantification of cyanide in water with gold nanoparticles via Resonance Rayleigh Scattering
Gao et al. A novel nonenzymatic fluorescent sensor for glucose based on silica nanoparticles doped with europium coordination compound
Tian et al. Novel ratiometric probe based on the use of rare earth-carbon dots nanocomposite for the visual determination of doxycycline
Tang et al. A simple and sensitive resonance Rayleigh scattering method for determination of As (III) using aptamer‐modified nanogold as a probe
Ye et al. A simple label-free rhodamine 6G SERS probe for quantitative analysis of trace As 3+ in an aptamer–nanosol
Carolan et al. Germanium nanocrystals as luminescent probes for rapid, sensitive and label-free detection of Fe 3+ ions
Liu et al. A ratiometric fluorescence sensor based on carbon quantum dots realized the quantitative and visual detection of Hg2+
Hou et al. Water‐soluble AIE‐active Fluorescent Organic Nanoparticles: Design, Preparation and Application for Specific Detection of Cyanide in Water and Food Samples
Gao et al. Rapid and accurate detection of phosphate in complex biological fluids based on highly improved antenna sensitization of lanthanide luminescence
Deng et al. A novel electrochemiluminescence resonance energy transfer system for ultrasensitive detection of prostate-specific antigen
Chen et al. An aptasensor for ampicillin detection in milk by fluorescence resonance energy transfer between upconversion nanoparticles and Au nanoparticles
Sakao et al. Determination of trace elements in shellfish tissue samples by inductively coupled plasma mass spectrometry

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20140625