CN104655578A - Colorimetric method for detecting lead ions - Google Patents
Colorimetric method for detecting lead ions Download PDFInfo
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- CN104655578A CN104655578A CN201510078869.2A CN201510078869A CN104655578A CN 104655578 A CN104655578 A CN 104655578A CN 201510078869 A CN201510078869 A CN 201510078869A CN 104655578 A CN104655578 A CN 104655578A
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Abstract
The invention discloses a colorimetric method for detecting lead ions, and specifically relates to a method for detecting lead ions by taking gold nanoparticles as a colorimetric probe. AuNPs(Cys-AuNPs) is modified by l-cysteine, and Cys can capture Pb<2+> by the binding function of a chelating ligand under the induction of Pb<2+>, so that Cys-AuNPs is aggregated, and thus the color of a solution changes, and the change in position and intensity of an AuNPs characteristic peak is caused. The colorimetric method has a detection range of 0.02- 5 microns, and detection limit of 0.02 microns, has the advantages of simplicity, economy, good selectivity (potassium thiocyanate as a screening agent) and the like, and can be used for detecting Pb<2+>.
Description
Technical field
The invention belongs to the method detecting heavy metal ion, be specifically related to a kind of method adopting colorimetric determination lead ion, specifically a kind of golden nanometer particle detects the method for lead ion as colorimetric probe.
Background technology
Toxic metal ions can cause serious impact to the health of environment and the mankind, especially lead ion, also can there is strong toxic action to human nerve, blood, digestion and kidney when a small amount of contact, affect the behavior of people, brain development and MNCV.New edition " drinking water sanitary standard " (GB5749-2006) regulation of Ministry of Public Health's promulgation in 2006, the content of daily Pb in Drinking Water must not higher than 0.01mg/L (being equivalent to 0.05 μM).Therefore, the plumbous detection method setting up a kind of accurate quick has important using value and practical significance.
The detection method of traditional lead comprises atomic absorption method (AAS) [Bednar A J, KirganR A, Jones W T.Analytica chimica acta, 2009,632 (1): 27-34.], spectrophotometric method [Narin I, Soylak M.Analytica Chimica Acta, 2003,493 (2): 205-212.], inductively coupled plasma mass spectrometry (ICP – MS) [
k, Ruzik R, Lipiec E.Talanta, 2007,72 (4): 1564-1572], x ray fluorescence spectrometry [Elzinga E J, Rouff A A, Reeder RJ.Geochimica et cosmochimica acta, 2006,70 (11): 2715-2725.] and electrochemical process [Yi Peng, Lidong Lin, Biosensors and Bioelectronics, 2014,59:314-320], but these methods all need complicated experimental technique usually, length consuming time, apparatus expensive, makes it be difficult to promote, is generally only applicable to lab analysis.
Compared to other detection methods, colourimetry has unique advantage, and the general naked eyes of its result are visible, without the need to complex instrument, cost is low and be very suitable for on-site measurement.Golden nanometer particle (AuNPs) has very strong surface plasma resonance (Surface plasmon resonance, SPR) performance, cause its ultraviolet-visible absorption spectroscopy can produce a sharp-pointed surface plasma resonance peak near 520nm, and the position at this peak can change with the change of AuNPs particle diameter and interparticle distance.In recent years, colorimetric determination Pb is used
2+research more [Huang K W, Yu C J, Tseng W L.Biosensors and Bioelectronics, 2010,25 (5): 984-989; Chai F, Wang C, Wang T, et al.ACS applied materials & interfaces, 2010,, but these method majorities can not meet cheap and simple, highly sensitive and selectivity these 3 requirements good simultaneously, are difficult to be applied to on-the-spot in situ detection 2 (5): 1466-1470].The present invention is used as colorimetric probe the AuNPs of Cys (L-cys) functionalization and detects Pb
2+.This method is simple, sensitive, selectivity is good, and detectability is low reaches 0.02 μM, lower than 0.05 μM (0.01mg/L) of national regulations, is expected to be applied in on-the-spot in situ detection.
Summary of the invention
The object of this invention is to provide a kind of method adopting colorimetric determination lead ion
Principle of the present invention: Cys contains-COOH and-a NH freely
2group, these 2 groups can provide a hydrophilic interface for reacting with heavy metal ion further.Work as Pb
2+when existing, Cys catches Pb by cheland combination
2+, cause Cys – AuNPs to assemble.When Cys – AuNPs occurs to assemble, the position of AuNPs characteristic peak and intensity can be caused to change, AuNPs solution colour also can be caused to be changed to indigo plant by red.
Content of the present invention:
Adopt a method for colorimetric determination lead ion, it is characterized in that: it uses golden nanometer particle as signal element, use Cys as the specific recognition element of lead ion, and be screener with potassium rhodanate;
The steps include:
One, 13nmAuNPs preparation:
13nm AuNPs adopts reduction of sodium citrate HAuCl according to literature method
4method is synthesized; 97.5mL ultrapure water and 2.5mL mass concentration 0.412% (10mM) chlorauric acid solution is added in the there-necked flask of cleaning, stir and be heated to boiling, 2mL mass concentration 1% citric acid three sodium solution is added after 7-8min, solution from colourless become redness after, stop heating, continue to stir 15min;
Two, Cys modifies the preparation of AuNPs solution:
After the centrifugal 20min of 1mL AuNPs solution 12000 turns/min, be resuspended in after sucking supernatant in 900 μ L ultrapure waters, add the freshly prepd Cys solution of 10 μ L 5 μMs, after concussion, leave standstill hatching 0.5h;
Three, new Pb
2+the configuration of standard solution:
Get 1mL variable concentrations 0,0.2,0.5,1,2,5,10,20, the standard P b of 50,100 μMs
2+solution, adds 20 μ L10mM potassium rhodanate solution, is configured to new Pb
2+standard solution;
Four, Pb
2+measure:
0 is added respectively, 0.02,0.05,0.1,0.2,0.5,1,2,5,10 μMs of new Pb in the Cys – AuNPs solution of preparation in above-mentioned 900 μ L steps (two)
2+standard solution, after hatching 30 minutes, obtains spectrum with ultraviolet/visible spectrophotometer scanning, spectrogram in record 400-800nm wavelength coverage; With Pb
2+the logarithm of concentration is horizontal ordinate, with 520nm place absorbance for ordinate drawing standard curve.
The present invention is when detecting actual sample, and adding 2 μMs of potassium rhodanates is screener.
Add Cys again after being redissolved by AuNPs, the amount adding Cys is 50nM.
Add new Pb
2+the amount of standard solution is 0,0.02,0.05,0.1,0.2,0.5,1,2,5,10 μMs.
Tool of the present invention has the following advantages: 1, detector probe provided by the invention is highly sensitive, selectivity good, and detectability is low; 2, do not need large-scale instrument, by naked eye or uv-vis spectra, get final product recognition detection result; 3, the inventive method is simple, quick, easy to operate, can carry out on-the-spot original position and detect fast.
Accompanying drawing explanation
Fig. 1 is (A) AuNPs, (B) Cys-AuNPs and (C) Pb
2+the transmission electron microscope photo of-Cys – AuNPs.
Fig. 2 .1 adds variable concentrations Pb for (A)
2+ultraviolet-visible spectral curve.
Fig. 2 .2 is ((B) Pb
2+standard spectral curves.
Fig. 3 adds in ultraviolet-visible absorption spectroscopy that the different heavy metal ion of same concentrations obtains
Difference (the i.e. Δ A of 520nm place blank group and experimental group absorbance
520=A
blank-A) histogram that obtains for ordinate.
Embodiment
Adopt a method for colorimetric determination lead ion, it uses golden nanometer particle as signal element, uses Cys as the specific recognition element of lead ion, and is screener with potassium rhodanate;
The steps include:
One, 13nmAuNPs preparation
13nm AuNPs adopts reduction of sodium citrate HAuCl according to literature method
4method is synthesized.97.5mL ultrapure water and 2.5mL mass concentration 0.412% (10mM) chlorauric acid solution is added in the there-necked flask of cleaning, stir and be heated to boiling, 2mL mass concentration 1% citric acid three sodium solution is added after 7-8min, solution from colourless become redness after, stop heating, continue to stir 15min.Can see that freshly prepd AuNPs is uniformly dispersed in accompanying drawing 1 (A), mean grain size is about 13nm.
Two, Cys modifies the preparation of AuNPs solution
After the centrifugal 20min of 1mL AuNPs solution 12000 turns/min, be resuspended in after sucking supernatant in 900 μ L ultrapure waters, add the freshly prepd Cys solution of 10 μ L 5 μMs, after concussion, leave standstill hatching 0.5h.Fig. 1 (B) can illustrate that Cys is modified to AuNPs surface, and Cys – AuNPs still exists in solution with single dispersing form.
Three, new Pb
2+the configuration of standard solution
Get 1mL variable concentrations 0,0.2,0.5,1,2,5,10,20, the Pb of 50,100 μMs
2+standard solution, adds 20 μ L10mM potassium rhodanate solution, is configured to new Pb
2+standard solution.
Four, Pb
2+measure
1. detection sensitivity
0 is added respectively, 0.02,0.05,0.1,0.2,0.5,1,2,5,10 μMs of standard P b in above-mentioned 900 μ L Cys – AuNPs solution
2+solution, after hatching 30 minutes, obtains spectrum with ultraviolet/visible spectrophotometer scanning, spectrogram in record 400-800nm wavelength coverage.With Pb
2+the logarithm of concentration is horizontal ordinate, with 520nm place absorbance for ordinate drawing standard curve, as shown in Figure 2.As seen from the figure, the sensing range of this colourimetry is 0.02 ~ 5 μM, detects and is limited to 0.02 μM (<0.05 μM).In addition, in experimentation when adding Pb
2+when concentration is to 1 μM, solution colour can become purple from claret.Continue to increase Pb
2+when concentration is more than 10 μMs, after leaving standstill, solution can produce precipitation, and these can be arrived by naked eye.
2. method choice
10 μ L 200 μ g/ml standard C d are added respectively in 1mLCys – AuNPs solution
2+, Cu
2+, Hg
2+, Zn
2+, Co
2+, Ni
2+, Pb
2+, As
2+solution (containing 2 μMs of potassium rhodanates), after hatching 30 minutes, spectrogram in scanning record 400-800nm wavelength coverage, result as shown in Figure 3.As seen from the figure, other heavy metal ion are to Pb
2+interference less (potassium rhodanate shield effectiveness is better), illustrate that this colourimetry is to Pb
2+there is good selectivity.
Embodiment 1:
13nm AuNPs adopts reduction of sodium citrate HAuCl according to literature method
4method is synthesized.In the AuNPs solution that 900 μ L redissolve, add the freshly prepd Cys solution of 10 μ L 5 μMs, concussion leaves standstill hatching 0.5h.Get 1mL potable water, add 10 μ L100 μM Pb
2+standard solution and 2 μ L10mM potassium rhodanate solution.The above-mentioned solution of 100 μ L is added in 0.9mLCys – AuNPs solution, after hatching 30 minutes, spectrogram in scanning record 400-800nm wavelength coverage.Found that, the standard deviation measured for 3 times is 0.56%, and average recovery rate is 95.7%, and this shows that this system can be used for Pb in potable water
2+detection.
Embodiment 2:
Get 1mL potable water, add 10 μ L1mM standard P b
2+solution and 2 μ L10mM potassium rhodanate solution.The above-mentioned solution of 100 μ L is added in 0.9mLCys – AuNPs solution, after hatching 30 minutes, spectrogram in scanning record 400-800nm wavelength coverage.The standard deviation measured for 3 times is 0.346%, and average recovery rate is 102.4%, and this shows that this system can be used for Pb in potable water
2+detection.
Claims (4)
1. adopt a method for colorimetric determination lead ion, it is characterized in that: it uses golden nanometer particle as signal element, use Cys as the specific recognition element of lead ion, and be screener with potassium rhodanate; It is characterized in that the steps include:
One, 13nmAuNPs preparation:
13nm AuNPs adopts reduction of sodium citrate HAuCl according to literature method
4method is synthesized; 97.5mL ultrapure water and 2.5mL mass concentration 0.412% (10mM) chlorauric acid solution is added in the there-necked flask of cleaning, stir and be heated to boiling, 2mL mass concentration 1% citric acid three sodium solution is added after 7-8min, solution from colourless become redness after, stop heating, continue to stir 15min;
Two, Cys modifies the preparation of AuNPs solution:
After the centrifugal 20min of 1mL AuNPs solution 12000 turns/min, be resuspended in after sucking supernatant in 900 μ L ultrapure waters, add the freshly prepd Cys solution of 10 μ L 5 μMs, after concussion, leave standstill hatching 0.5h;
Three, new Pb
2+the configuration of standard solution:
Get 1mL variable concentrations 0,0.2,0.5,1,2,5,10,20, the Pb of 50,100 μMs
2+standard solution, adds 20 μ L10mM potassium rhodanate solution, is configured to new Pb
2+standard solution;
Four, Pb
2+measure:
1,0 is added respectively, 0.02,0.05,0.1,0.2,0.5,1,2,5,10 μMs of new Pb in the Cys – AuNPs solution prepared in above-mentioned 900 μ L steps (two)
2+standard solution, after hatching 30 minutes, obtains spectrum with ultraviolet/visible spectrophotometer scanning, spectrogram in record 400-800nm wavelength coverage; With Pb
2+the logarithm of concentration is horizontal ordinate, with 520nm place absorbance for ordinate drawing standard curve.
2. the method for employing colorimetric determination lead ion according to claim 1, is characterized in that: the present invention is when detecting actual sample, and adding 2 μMs of potassium rhodanates is screener.
3. the method for employing colorimetric determination lead ion according to claim 1, is characterized in that: add Cys again after being redissolved by AuNPs, the amount adding Cys is 50nM.
4. the method for employing colorimetric determination lead ion according to claim 1, is characterized in that: add new Pb
2+the amount of standard solution is 0,0.02,0.05,0.1,0.2,0.5,1,2,5,10 μMs.
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| CN105203521A (en) * | 2015-10-22 | 2015-12-30 | 南华大学 | O-phenylenediamine detection method based on nano-interface energy transferring |
| CN105403558A (en) * | 2015-11-18 | 2016-03-16 | 沈阳药科大学 | Method for on-line and quick detection of lead ions |
| CN105548130A (en) * | 2016-02-29 | 2016-05-04 | 福州大学 | Fluorescent sensor for cobalt ion detection and application method of fluorescent sensor |
| CN106442345A (en) * | 2016-09-08 | 2017-02-22 | 常熟理工学院 | Method of detecting lead ion based on CD spectrum detection technology |
| CN107677623A (en) * | 2017-08-28 | 2018-02-09 | 杨蕾 | A kind of method based on Ag@Au nano-particles detection lead ion |
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
| US10677790B2 (en) | 2016-07-20 | 2020-06-09 | City University Of Hong Kong | Optochemical detector and a method for fabricating an optochemical detector |
| CN114778461A (en) * | 2022-04-22 | 2022-07-22 | 南通大学 | Preparation method of intelligent gold nanoparticles and application of intelligent gold nanoparticles in beta-amyloid protein colorimetric analysis |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203521A (en) * | 2015-10-22 | 2015-12-30 | 南华大学 | O-phenylenediamine detection method based on nano-interface energy transferring |
| CN105203521B (en) * | 2015-10-22 | 2017-11-24 | 南华大学 | A kind of o-phenylenediamine detection method based on nano-interface energy transfer |
| CN105403558A (en) * | 2015-11-18 | 2016-03-16 | 沈阳药科大学 | Method for on-line and quick detection of lead ions |
| CN105403558B (en) * | 2015-11-18 | 2019-04-02 | 沈阳药科大学 | A kind of method of quick detection lead ion |
| CN105548130A (en) * | 2016-02-29 | 2016-05-04 | 福州大学 | Fluorescent sensor for cobalt ion detection and application method of fluorescent sensor |
| CN105548130B (en) * | 2016-02-29 | 2018-03-16 | 福州大学 | A kind of fluorescent optical sensor and its application process for cobalt ions detection |
| US10677790B2 (en) | 2016-07-20 | 2020-06-09 | City University Of Hong Kong | Optochemical detector and a method for fabricating an optochemical detector |
| CN106442345A (en) * | 2016-09-08 | 2017-02-22 | 常熟理工学院 | Method of detecting lead ion based on CD spectrum detection technology |
| CN106442345B (en) * | 2016-09-08 | 2019-03-15 | 常熟理工学院 | A kind of lead ion detection method based on CD spectrum detection technique |
| CN107677623A (en) * | 2017-08-28 | 2018-02-09 | 杨蕾 | A kind of method based on Ag@Au nano-particles detection lead ion |
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
| CN114778461A (en) * | 2022-04-22 | 2022-07-22 | 南通大学 | Preparation method of intelligent gold nanoparticles and application of intelligent gold nanoparticles in beta-amyloid protein colorimetric analysis |
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Application publication date: 20150527 |