CN101892043A - Method for preparing gold nano particles and application of particles in detection of cyhalothrin - Google Patents
Method for preparing gold nano particles and application of particles in detection of cyhalothrin Download PDFInfo
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- CN101892043A CN101892043A CN2010101286883A CN201010128688A CN101892043A CN 101892043 A CN101892043 A CN 101892043A CN 2010101286883 A CN2010101286883 A CN 2010101286883A CN 201010128688 A CN201010128688 A CN 201010128688A CN 101892043 A CN101892043 A CN 101892043A
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- cyhalothrin
- mercaptoethylamine
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Abstract
The invention provides a method for preparing gold nano particles. The method particularly comprises the following steps of: at room temperature, adding perchloric acid gold into distilled water to obtain 10<-2>mol/L aqueous solution of the perchloric acid gold; adding sodium citrate and sodium borohydride while stirring the aqueous solution; continuously stirring the mixed solution for 0.5 to 2 hours; and adding 3*10<-5>mol/L aqueous solution of mercaptoethylamine to obtain mercaptoethylamine-modified gold nano particles, wherein the weight ratio of the distilled water, the aqueous solution of the perchloric acid gold, the sodium citrate, the sodium borohydride to the aqueous solution of the mercaptoethylamine is 1:(0.008-0.01): (0.032-0.04):(0.04-0.12):(0.005-0.05). The method is simple and has high operability; and by the change of visible color of the gold nano particles prepared by the method, cyhalothrin in esbiothrin pesticides can be quickly identified and detected, and the detection limit reaches national standard value.
Description
Technical field
The present invention relates to the nanocomposite optical field,, make mercaptoethylamine modify golden nanometer particle and be used as probe, be widely used in analyzing and testing work by gold nano special optical character.
Background technology
Pyrethrin, because of its characteristic with wide spectrum, low toxicity, efficient and biological degradation etc. is widely used, but in farm crop, soil, water body, all have residual, and since such agricultural chemicals certain property accumulated is arranged, the part kind has teratogenesis, mutagenesis to the people.Therefore, the residual and detection of pyrethroid pesticide in environment is the problem that people relatively pay close attention to always.But all concentrate on the chromatographic process about the residual detection report of pyrethroid in the environmental sample in the existing document.Chromatographic technique is considered to classical, the most the most frequently used Detecting Pesticide technology, and as gas-chromatography, liquid chromatography, gas chromatography mass spectrometry, LC-MS isochromatic spectrum technology, yet chromatographic technique detection time is long, cost is high, complicated operation.Therefore be subjected to very big restriction in the application that detects at the scene.
Summary of the invention
Technical problem to be solved by this invention is: a kind of Jenner's grain of rice (abbreviation gold nano) with finishing mercaptoethylamine of excellent performance is provided, the simple and feasible preparation method of this gold nano also is provided, provides this this gold nano to be used for the method for quick and maneuverable detection cyhalothrin simultaneously.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of golden nanometer particle provided by the invention, be with the source of perchloric acid gold as gold, Trisodium Citrate is as stablizer, distilled water is as reaction solvent, mercaptoethylamine is as ion and anion receptor additives, and one pot reaction makes, and concrete preparation method is: under the room temperature, add the perchloric acid gold in distilled water, forming concentration is 10
-2Perchloric acid Jinsui River solution of mol/L adds Trisodium Citrate after stirring 1～5 minute, under agitation add sodium borohydride then, continues to stir 0.5～2 hour, and adding concentration then is 3 * 10
-5The mercaptoethylamine aqueous solution of mol/L obtains the mercaptoethylamine gold nano-particles modified; Each composition weight proportioning is a distilled water: perchloric acid Jinsui River solution: Trisodium Citrate: sodium borohydride: the mercaptoethylamine aqueous solution=1: (0.008～0.01): (0.032～0.04): (0.04～0.12): (0.005～0.05).
Described each composition weight proportioning can be distilled water: perchloric acid Jinsui River solution: Trisodium Citrate: sodium borohydride: the mercaptoethylamine aqueous solution=1: 0.01: 0.04: 0.12: 0.05.
Prepared golden nanometer particle has monodispersity preferably in water, its resonance absorption peak position is at 510～520nm, and solution colour is a burgundy, and particle diameter is 5～20nm.
Above-mentioned golden nanometer particle provided by the invention utilizes the interaction of hydrogen bond of trifluoromethyl in this Jenner's grain of rice surface amino groups and the cyhalothrin, obtains the colorimetric sensor of cyhalothrin.Because described interaction can make Jenner's grain of rice assemble, thus the variation of the color of showing and uv-absorbing, so be used as the probe that detects cyhalothrin.
Adopt following method during the detection of described probe cyhalothrin in: get Jenner's grain of rice solution that the 1.50mL mercaptoethylamine is modified respectively, add 0.25mL 5 * 10 to the aqueous solution
-5～10
-8The mol/L cyhalothrin mixes, and leaves standstill to observe the colour-change of respectively organizing mixing solutions after for some time, carries out the uv-visible absorption spectra analysis; Then, by comparison, the color generation obvious variation of the gold nano that the mercaptoethylamine of adding cyhalothrin is modified, and increase along with cyhalothrin concentration, color is deepened successively, solution colour becomes hyacinthine so that atropurpureus from burgundy, and tangible red shift takes place ultraviolet absorption peak, and its colorimetric detection is limited to 4.5 * 10
-8Mol/L～5.5 * 10
-8Mol/L, preferred value is 5 * 10
-8Mol/L.
The detection of described probe cyhalothrin in for actual lake water is handled carrying out heating and filtering behind lake water and the yellow soda ash mixing earlier, detects by the following method: get Jenner's grain of rice solution that the 1.50mL mercaptoethylamine is modified respectively, add 0.25mL5 * 10 again
-5～10
-8The mol/L cyhalothrin mixes, and leaves standstill to observe the colour-change of respectively organizing mixing solutions after for some time, carries out the uv-visible absorption spectra analysis; Then, by comparison, the color generation obvious variation of the gold nano that the mercaptoethylamine of adding cyhalothrin is modified, and increase along with cyhalothrin concentration, color is deepened successively, and solution colour becomes bluish voilet so that atropurpureus from burgundy, and tangible red shift takes place ultraviolet absorption peak.
Experimental result shows that the mass ratio of cyhalothrin in lake water all can detect by visual colour-change or ultraviolet-visible spectrum in being not less than the scope of 0.1mg/L.
The present invention has the following advantages:
(1) simple and feasible, the stable process conditions of preparation method, favorable reproducibility, agents useful for same safety are easy to get, and just obtain surface-functionalized golden nanometer particle by simple one kettle way single step reaction.
(2) stable, good optical property: this gold nano monodispersity is good, uniform particles, and have satisfactory stability, deposit one month after, its performance not have change substantially.
(3) freedom from jamming is good: visual colour-change and optical change do not take place to cyhalothrin analogue and yin, yang ion that some are common in this gold nano, thereby have realized specific identification and check to cyhalothrin.Find out that by Fig. 2 and Fig. 3 only free chrysanthemum ester makes the ultraviolet absorption peak generation obvious variation of this gold nano, makes the color of solution become atropurpureus by burgundy simultaneously.
(4) be used to detect cyhalothrin: can discern cyhalothrin by the variation of obvious colour-change and ultraviolet-visible spectrum, this method is simple and efficient, easy handling.Studies show that: the solution colour of gold nano is relevant with its size and grain spacing, when the gold nano grain spacing is significantly less than particle diameter, just reunite easily, and color and a series of optical change take place, solution colour becomes hyacinthine or atropurpureus by burgundy on the macroscopic view.Utilize this character, in control gold nano particle diameter,, just can design diversified gold nano-probe, thereby realize quick, noiseless detection cyhalothrin in conjunction with various surface modifying methods.
In a word, method technology provided by the invention is easy, and operability is good, the common laboratory complete operation of all having ready conditions.Prepared golden nanometer particle can be by quick identification and the detection of visual colour-change realization to cyhalothrin, and its detectability can the value of being up to state standards.
Description of drawings
Fig. 1 modifies the uv-visible absorption spectra at gold nano 520nm place when the different number of days for mercaptoethylamine.
Fig. 2 modifies gold nano to the cyhalothrin of concentration and the uv-visible absorption spectra of analogue thereof for mercaptoethylamine.
Fig. 3 modifies column diagram after gold nano adds the yin, yang ion respectively for mercaptoethylamine.
Behind the cyhalothrin of Fig. 4 for the adding different concns, mercaptoethylamine is modified the uv-visible absorption spectra of gold nano.
Behind the lake water solution of Fig. 5 for the cyhalothrin of adding different concns, mercaptoethylamine is modified the uv-visible absorption spectra of gold nano.
Fig. 6 prepares the process flow sheet of the gold nano of mercaptoethylamine modification for the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment, but do not limit the present invention.
One. the preparation of the gold nano that mercaptoethylamine is modified
The present invention adopts the sodium borohydride reduction method, promptly with the source of perchloric acid gold as gold, mercaptoethylamine is as stablizer, redistilled water is as reaction solvent, one pot reaction makes the mercaptoethylamine gold nano-particles modified, and concrete preparation method is: referring to Fig. 6, under the room temperature, in 94mL water, add 1mL 10
-2Mol/L AuClO
4The aqueous solution, the 4mg Trisodium Citrate stirred 1～5 minute, added 4～12mg NaBH
4, continue to stir 0.5～2 hour, add 0.5～5mL 3 * 10
-5The mercaptoethylamine aqueous solution of mol/L gets final product.The maximum absorption peak position of this gold nano is at 520nm, the about 8nm of particle diameter, the character (see figure 1) that do not change in the one month scope.
As shown in Figure 2: with 0.25mL 10
-4The cyhalothrin of mol/L and cyhalothrin analogue solution join respectively in the gold nano solution of 1.5mL mercaptoethylamine modification, mix, and place ten minutes, carry out the uv-visible absorption spectra analysis.In the resulting uv-visible absorption spectra: 1. blank, 2. permethrin, 3. high permethrin, 4. cyhalothrin, 5. Cypermethrin, 6. Deltamethrin, 7. cyhalofop-butyl.
As shown in Figure 3: with 0.25mL 10
-4The K of mol/L
+(a1), Na
+(a2), Ca
2+(a3), Mg
2+(a4), Mn
2+(a5), Pb
2+(a6), Cd
2+(a7), H
2PO
4 -(a8), CO
3 2-(a9) solion, blank (a10) join respectively in the gold nano solution of 1.5mL mercaptoethylamine modification, mix, placed ten minutes, and carried out the uv-visible absorption spectra analysis, be illustrated as various zwitterions and add the ultraviolet absorption value of back in 520nm place gold nano.
By Fig. 2 and Fig. 3 as can be seen, cyhalothrin analogue and common yin, yang ion all can not produce the detection of cyhalothrin and disturb.
Two. the gold nano that mercaptoethylamine is modified is to the application of the detection of cyhalothrin
Embodiment 1, and the gold nano that mercaptoethylamine is modified is to the detection of cyhalothrin in the pure water solution:
With 0.25mL different concns (5 * 10
-5～10
-8Mol/L) cyhalothrin solution joins in Jenner's grain of rice that the mercaptoethylamine of 1.5mL modifies, and mixes, and the color of solution becomes atropurpureus by burgundy after 5 minutes.Carry out the uv-visible absorption spectra analysis after 10 minutes respectively, see Fig. 4, the absorption intensity at its 520nm place reduces gradually, and peak shape broadens, and engenders a new peak at the 580nm place.Its colorimetric detection is limited to 5 * 10
-8Mol/L.Wherein cyhalothrin concentration is respectively: b1,0; B2,5 * 10
-5B3,1 * 10
-5B4,5 * 10
-6B5,1 * 10
-6B6,5 * 10
-7B7,1 * 10
-7B8,5 * 10
-8B9,1 * 10
-8
Get 100ml lake water, add the yellow soda ash of 20mg, fully concussion can be shaken in ultrasonic cleaner 5 minutes in case of necessity, mixed, and heated and boiled half an hour then, used twice of common filter paper filtering standby at last.With the lake water of the processing that obtains, successively cyhalothrin is made into the solution (5 * 10 of different concns
-5～10
-8Mol/L).The cyhalothrin solution of getting the 0.25mL different concns joins the gold nano solution of the mercaptoethylamine modification of 1.5mL, mixes, and concentration is not less than 1 * 10 after 5 minutes
6The color of solution become hyacinthine by burgundy.Carry out the uv-visible absorption spectra analysis after 10 minutes respectively, as shown in Figure 5, the absorption intensity at its 520nm place reduces gradually, and peak shape broadens, and engenders a new peak at the 580nm place.Its colorimetric detection is limited to 1 * 10
-6Mol/L (0.44mg/L).Wherein cyhalothrin concentration is respectively: c1,0; C2,5 * 10
-5C3,1 * 10
-5C4,5 * 10
-6C5,1 * 10
-6C6,5 * 10
-7C7,1 * 10
-7C8,5 * 10
-8C9,1 * 10
-8
Claims (7)
1. the preparation method of a golden nanometer particle, it is characterized in that with the source of perchloric acid gold as gold, Trisodium Citrate is as stablizer, distilled water is as reaction solvent, mercaptoethylamine is as ion and anion receptor additives, and one pot reaction makes, and concrete preparation method is: under the room temperature, add the perchloric acid gold in distilled water, forming concentration is 10
-2Perchloric acid Jinsui River solution of mol/L adds Trisodium Citrate after stirring 1～5 minute, under agitation add sodium borohydride then, continues to stir 0.5～2 hour, and adding concentration then is 3 * 10
-5The mercaptoethylamine aqueous solution of mol/L obtains the mercaptoethylamine gold nano-particles modified; Each composition weight proportioning is a distilled water: perchloric acid Jinsui River solution: Trisodium Citrate: sodium borohydride: the mercaptoethylamine aqueous solution=1: (0.008～0.01): (0.032～0.04): (0.04～0.12): (0.005～0.05).
2. the preparation method of golden nanometer particle according to claim 1 is characterized in that each composition weight proportioning is a distilled water: perchloric acid Jinsui River solution: Trisodium Citrate: sodium borohydride: the mercaptoethylamine aqueous solution=1: 0.01: 0.04: 0.12: 0.05.
3. the preparation method of golden nanometer particle according to claim 1 is characterized in that this golden nanometer particle has monodispersity preferably in water, and its resonance absorption peak position is at 510～520nm, and solution colour is a burgundy, and particle diameter is 5～20nm.
4. the purposes of a golden nanometer particle is characterized in that claim 1 or 2 or 3 prepared golden nanometer particles are used as the probe that detects cyhalothrin.
5. according to the purposes of the described golden nanometer particle of claim 4, adopt following method when it is characterized in that the detection of described probe cyhalothrin in: get Jenner's grain of rice solution that the 1.50mL mercaptoethylamine is modified respectively, add 0.25mL5 * 10 to the aqueous solution
-5～10
-8The mol/L cyhalothrin mixes, and leaves standstill to observe the colour-change of respectively organizing mixing solutions after for some time, carries out the uv-visible absorption spectra analysis; Then, by comparison, the color generation obvious variation of the gold nano that the mercaptoethylamine of adding cyhalothrin is modified, and increase along with cyhalothrin concentration, color is deepened successively, solution colour becomes hyacinthine so that atropurpureus from burgundy, and tangible red shift takes place ultraviolet absorption peak, and its colorimetric detection is limited to 4.5 * 10
-8Mol/L～5.5 * 10
-8Mol/L.
6. according to the purposes of the described golden nanometer particle of claim 4, it is characterized in that the detection of described probe cyhalothrin in for actual lake water, handle carrying out heating and filtering behind lake water and the yellow soda ash mixing earlier, detect by the following method again: get Jenner's grain of rice solution that the 1.50mL mercaptoethylamine is modified respectively, add 0.25mL 5 * 10
-5～10
-8The mol/L cyhalothrin mixes, and leaves standstill to observe the colour-change of respectively organizing mixing solutions after for some time, carries out the uv-visible absorption spectra analysis; Then, by comparison, the color generation obvious variation of the gold nano that the mercaptoethylamine of adding cyhalothrin is modified, and increase along with cyhalothrin concentration, color is deepened successively, and solution colour becomes bluish voilet so that atropurpureus from burgundy, and tangible red shift takes place ultraviolet absorption peak.
7. according to the purposes of the described golden nanometer particle of claim 6, it is characterized in that: the minimum variable color detectable level of cyhalothrin in lake water is 0.1mg/L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288556A (en) * | 2011-06-03 | 2011-12-21 | 华东理工大学 | Use and method for detecting sulfate ions based on cysteamine modified nano gold solution |
| RU2470297C1 (en) * | 2011-11-11 | 2012-12-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Омский государственный аграрный университет" имени П.А. Столыпина" | Method to determine gamma-cyhalothrin in biological objects using thin-layer chromatography |
| CN103645178A (en) * | 2013-09-12 | 2014-03-19 | 华中师范大学 | On-site detection and separation technologies of imidacloprid |
| CN104785776A (en) * | 2015-05-11 | 2015-07-22 | 厦门大学 | Surface cleaning method for silver nanoparticle with sodium borohydride aqueous solution |
| CN106370708A (en) * | 2016-08-29 | 2017-02-01 | 南京师范大学 | Electrochemistry sensor for measuring organophosphorus pesticide residues and measurement method thereof |
| CN108152277A (en) * | 2016-12-05 | 2018-06-12 | 中国科学院宁波材料技术与工程研究所 | A kind of method for detecting pesticide residue |
| CN109181690A (en) * | 2018-11-02 | 2019-01-11 | 青岛大学 | Preparation method based on double emissive quantum dots/nano grain of silver compound cymoxanil ratio fluorescent probe |
| CN113384551A (en) * | 2021-05-07 | 2021-09-14 | 西安交通大学 | Preparation method and application of bionic nano-carrier for reducing excessive calcium ions in tumors |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288556A (en) * | 2011-06-03 | 2011-12-21 | 华东理工大学 | Use and method for detecting sulfate ions based on cysteamine modified nano gold solution |
| RU2470297C1 (en) * | 2011-11-11 | 2012-12-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Омский государственный аграрный университет" имени П.А. Столыпина" | Method to determine gamma-cyhalothrin in biological objects using thin-layer chromatography |
| CN103645178A (en) * | 2013-09-12 | 2014-03-19 | 华中师范大学 | On-site detection and separation technologies of imidacloprid |
| CN103645178B (en) * | 2013-09-12 | 2016-04-13 | 华中师范大学 | The Site Detection of Imidacloprid and isolation technics |
| CN104785776A (en) * | 2015-05-11 | 2015-07-22 | 厦门大学 | Surface cleaning method for silver nanoparticle with sodium borohydride aqueous solution |
| CN106370708A (en) * | 2016-08-29 | 2017-02-01 | 南京师范大学 | Electrochemistry sensor for measuring organophosphorus pesticide residues and measurement method thereof |
| CN106370708B (en) * | 2016-08-29 | 2018-09-14 | 南京师范大学 | A kind of electrochemical sensor and its detection method of organophosphorus pesticide residual quantity detection |
| CN108152277A (en) * | 2016-12-05 | 2018-06-12 | 中国科学院宁波材料技术与工程研究所 | A kind of method for detecting pesticide residue |
| CN109181690A (en) * | 2018-11-02 | 2019-01-11 | 青岛大学 | Preparation method based on double emissive quantum dots/nano grain of silver compound cymoxanil ratio fluorescent probe |
| CN109181690B (en) * | 2018-11-02 | 2019-06-25 | 青岛大学 | Preparation method based on double emissive quantum dots/nano grain of silver compound cymoxanil ratio fluorescent probe |
| US10900899B1 (en) | 2018-11-02 | 2021-01-26 | Qingdao University | Method for preparing ratiometric fluorescent probe for cymoxanil based on double-emission quantun dot-silver nanoparticle complex |
| CN113384551A (en) * | 2021-05-07 | 2021-09-14 | 西安交通大学 | Preparation method and application of bionic nano-carrier for reducing excessive calcium ions in tumors |
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