CN105572107A - Method for detecting acetamiprid in waste water by chemiluminiscence - Google Patents
Method for detecting acetamiprid in waste water by chemiluminiscence Download PDFInfo
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- CN105572107A CN105572107A CN201510936545.8A CN201510936545A CN105572107A CN 105572107 A CN105572107 A CN 105572107A CN 201510936545 A CN201510936545 A CN 201510936545A CN 105572107 A CN105572107 A CN 105572107A
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Abstract
The invention discloses a method for detecting acetamiprid in waste water by chemiluminiscence. The method is based on the luminol-silver nitrate-nano silver chemiluminiscence analysis system, interaction of acetamiprid aptamer and acetamiprid are utilized, and transformation of configuration of the aptamer induces change of form of nano silver, thus reducing catalytic performance of the nano silver. Acetamiprid in waste water is detected by chemiluminiscence analysis in a way of static injection. According to the method, instruments in service are at a low price and require hardly any technical staff. Besides, the luminol-silver nitrate-nano silver chemiluminiscence analysis system is stable, so that the method is good in reproducibility. The RSD (relative standard deviation) is 2.9% to 4.2%, high sensitivity is achieved, and detection limit reaches 2.0*10-9g/L.
Description
Technical field
The invention belongs to organic agricultural chemicals detection field, particularly relate to the method for Acetamiprid in a kind of chemiluminescence detection waste water.
Background technology
All the time, the pollution that residue of pesticide causes for environment receives much concern.Acetamiprid, having another name called acetamiprid, pyrrole worm is clear, is a kind of New-type wide-spectrum nicotinic insecticide after Imidacloprid, because of characteristics such as it is efficient, low toxicity, interior absorption are strong, consumption is few, the longevity of residure is long, residual quantity is low, application widely, commercially occupies very high share.Acetamiprid can cause human nerve disorderly and poisoning, and therefore, in waste discharge, acetamiprid residue and accumulation must threaten the health of people.
The detection method of current acetamiprid residue mainly contains high performance liquid chromatography, vapor-phase chromatography, mass spectroscopy, liquid chromatograph mass spectrography, galvanochemistry, the methods such as colourimetry, fluorescent spectrometry and enzyme-linked immuno assay.These method ubiquity sample pre-treatments are loaded down with trivial details, and costly, the upper machine testing time is long, inefficiency, and the accuracy with an organic solvent measuring the complicacy impact analysis of more or matrix itself is not enough; Mass spectrometric hyphenated technique, due to expensive equipment, therefore can not get well universal; And enzyme-linked immune analytic method is easy to be disturbed and poor stability.There is the low problem of sensitivity in colourimetry and fluorescent spectrometry, electrochemical method cannot solve the problem of operate out of phase and be difficult to robotization.Therefore, develop method that sensitive, quick and practical analysis detects Acetamiprid and have realistic meaning very much for the health of environmental monitoring and people.
Chemiluminometry have highly sensitive, instrument simple, analyze and realize the advantages such as robotization fast, easily, but the research using chemiluminescence analysis to detect Acetamiprid has no report.Nano Silver can the chemiluminescence reaction of catalysis luminol and silver nitrate, and luminol-silver nitrate-Nano Silver chemiluminescence analysis system is stable and the analysis system that sensitivity is good.The present invention utilizes luminol-silver nitrate-Nano Silver chemiluminescence analysis system, utilizes the interaction of Acetamiprid aptamers and Acetamiprid, the change of the change induced nano silver form of aptamers configuration, thus causes the reduction of Nano Silver catalytic performance.Adopt the mode of static state feedback, realize the Acetamiprid in chemiluminescence analysis detection waste water.Aptamers makes this method have the selectivity of height for the high specific of object identification.
Summary of the invention
For solve existing mensuration Acetamiprid technology in Problems existing, the invention provides the method for Acetamiprid in a kind of chemiluminescence detection waste water.
The present invention is achieved by the following technical solutions:
A method for Acetamiprid in chemiluminescence detection waste water, comprises the following steps:
Acetamiprid aptamers and the waste water containing Acetamiprid are interacted, add Nano silver solution, then Nano Silver-the aptamers after effect-Acetamiprid solution is moved in chemiluminescence pond, inject luminol-silver nitrate chemical illuminating reagent, carry out luminescence-producing reaction, detect chemiluminescent signal simultaneously.After Acetamiprid and its aptamers effect, aptamers changes specific conformation into by single stranded DNA, the change of the conformational change induced nano silver form of Acetamiprid aptamers, thus causes Nano Silver to the reduction of the catalytic activity of the chemiluminescence reaction of luminol-silver nitrate; Quantitative measurement is carried out to the intensity of luminescence-producing reaction, the concentration of Acetamiprid in waste water can be obtained.
Further improvement, the Nano Silver particle diameter in described Nano silver solution is 15nm, and concentration is 3.2 × 10
-10mol/L.
Further improvement, the concentration of aptamers is 6 × 10
-6mol/L, the action time of aptamers and Acetamiprid is 10 minutes.
Further improvement, described Nano silver solution is adopted and is obtained with the following method: be 1 × 10 by 25mL concentration
-3the 75mL concentration that the liquor argenti nitratis ophthalmicus of mol/L dropwise joins high-speed stirred is 2 × 10
-3in the sodium borohydride solution of mol/L, react 10 minutes, adding 5mL massfraction is that 1% sodium citrate solution is as stabilizing agent.
Further improvement, described Lu meter Nuo – silver nitrate chemical illuminating reagent is by 5 × 10
-5the luminol solution of mol/L and 1.0 × 10
-4the liquor argenti nitratis ophthalmicus of mol/L is mixed to get with 1:1 volume ratio.
Further improvement, the pH value of described luminol-silver nitrate chemical illuminating reagent is 12.0.
Compared with prior art, the present invention has the following advantages:
(1) adopt chemiluminescence analytical technique, instrument is cheap, to technician's almost no requirement (NR); (2) use the luminol-silver nitrate chemiluminescence analysis system of Nano Silver catalysis, this stable system, makes this method favorable reproducibility, and RSD is between 2.9% ~ 4.2%, highly sensitive, and detection limit reaches 2.0 × 10
– 9g/L; (3) aptamer is for the high specific of object identification, makes this method selectivity good; (4) whole experimental implementation is gentle, and all carries out in liquid-phase system, is easy to operation, is conducive to the analysis operation of robotization; (5) experimental implementation is fast easy, and analytical test time shorten is within 30 minutes.The method that the present invention sets up has filled up the blank that chemiluminescence analysis detects Acetamiprid research field undoubtedly.
Accompanying drawing explanation
Fig. 1 is the response diagram of luminol-silver nitrate-Nano Silver chemiluminescence signal, and wherein a is the luminous signal of aptamers, and b is the luminous signal of Acetamiprid+aptamers;
Fig. 2 is the sensitivity analysis that chemiluminescence analysis detects Acetamiprid.
Concrete case study on implementation
Used key instrument equipment and reagent:
Acetamiprid aptamers be can with the nucleic acid of Acetamiprid selective binding, purchased from Sheng Gong bio tech ltd, Shanghai, Acetamiprid is purchased from Aladdin chemical reagent company limited.Experimental water is secondary deionized water.Silver nitrate is purchased from Solution on Chemical Reagents in Shanghai company.The sewage sample used takes from the waste water of city sewage treatment plant of University of Fuzhou, after being filtered by waste water sample respectively, dilutes to volume in 100mL volumetric flask by secondary deionized water with Medium speed filter paper.IFFL-D Flow Injection Analysis/Chemiluminescence instrument and support equipment (Xi'an Rui Mai Analytical Instrument Co., Ltd) thereof, TU-1901 type spectrophotometry instrument (Beijing Pu Xi all purpose instrument company limited), transmission electron microscope (Hitachi, Ltd, specifications and models: H-600).
Acetamiprid aptamers Tris-HCl buffer solution (pH7.5) dissolves and is prepared in refrigerator freezing storage, within 5 minutes, need then be cooled to normal temperature stand-by before using in high temperature 80 DEG C heating.Use intermediate water to dissolve Acetamiprid and obtain standard solution, re-use standard solution and dilute Acetamiprid standard serial solution.
The preparation of Nano Silver: adopt sodium borohydride reduction silver ion, trisodium citrate is as stabilizing agent.Glassware used in preparation process all uses chloroazotic acid soaking and washing (1:3HNO
3– HCl), then use secondary deionized water cleaning down clean, dry for standby.By 1 × 10 of 25mL
-3the liquor argenti nitratis ophthalmicus of mol/L dropwise joins 2 × 10 of the 75mL of high-speed stirred
-3in mol/L sodium borohydride solution, react after 10 minutes, add 5mL massfraction be 1% sodium citrate solution as stabilizing agent, continue stirring 10 minutes, stop stirring.Be put in by the nano silver colloidal sol obtained in brown reagent bottle, preserve in 4 DEG C of refrigerators, slaking is stand-by two days later.
4.43g luminol pressed powder to be dissolved in 20mL0.10Mmol/L solution and to be diluted to 1L, preparing 2.5 × 10
– 2mol/L luminol stock solution.Keep in Dark Place a week to guarantee the stable of reagent properties before use.The working solution of luminol is obtained by the dilution of stock solution.Silver nitrate intermediate water dissolves prepares storing solution, and working solution is obtained by dilution storing solution.Lu meter Nuo – silver nitrate reagent is by 5 × 10
-5the luminol solution of mol/L and 1.0 × 10
-4the liquor argenti nitratis ophthalmicus of mol/L is mixed to get with 1:1 volume ratio, and its pH value is 12.0.
Measure: 200 μ L Acetamiprid standard serial solutions and testing sample are mixed with 200 μ L Acetamiprid aptamers solution respectively, Acetamiprid aptamers solution concentration is 6 × 10
-6mol/L, acts on 10 minutes; After adding Nano silver solution, act on 5 minutes; Then adding 50 μ L concentration is the NaCl solution of 0.5mol/L, obtains mixed solution after mixing; Pipette 100 μ L mixed solutions in chemiluminescence pond, and inject 200 μ L Lu meter Nuo – silver nitrate reagent, detected by IFFL-D chemiluminescent analyzer and record luminous signal, according to the concentration of luminous intensity and Acetamiprid solution, production standard curve, then establishing criteria curve calculates the concentration of Acetamiprid in testing sample.The chemiluminescence signal response of representative as shown in Figure 1.
Testing Acetamiprid standard serial solution concentration used is: 1.5 × 10
-7, 6.5 × 10
-7, 1.5 × 10
-6, 6.5 × 10
-6, 1.5 × 10
-5, 5.8 × 10
-5g/L.Experimental result shows, under the experiment condition optimized, along with the increase of Acetamiprid concentration, chemiluminescence signal reduces gradually.Find the linear correlativity of logarithm value of chemiluminescence intensity and Acetamiprid concentration.According to the chemiluminescence intensity recorded, drawing standard curve.As shown in Figure 2, it detects and is limited to 2.0 × 10
– 9g/L (S/N=3).And to 6.5 × 10
-6the Acetamiprid replicate determination of g/L 6 times, its relative standard deviation is 2.6%.Experimental result shows that the method detection limit is low, and precision is good, and easy and simple to handle.
Simultaneously test sewage sample, the results are shown in table 1.Experimental result shows, the method that the present invention sets up has good accuracy and precision, and the recovery is respectively 94.5% ~ 106.13%, RSD is between 2.9% ~ 4.2%, analysis time is short, does not need to use large-scale instrument, can be used for the quick detection of Acetamiprid in waste water.
The result that in table 1 waste water, Acetamiprid measures
The selectivity analysis of this method:
To poison cicada, parathion and pentachlorophenol three kinds of co-existed pesticides with poison for representative, the selectivity that investigation method measures Acetamiprid.Aptamers/Acetamiprid, aptamers (without Acetamiprid), aptamers/poison cicada, aptamers/parathion, aptamers/pentachlorophenol and any DNA sequence/Acetamiprid with poison to the response of chemiluminescence signal is examined in experiment.In experiment, aptamers and any DNA sequence are as identification DNA sequence dna, and its concentration is 6 × 10
-6mol/L.Other contrast pesticide concentration is identical with Acetamiprid concentration, is 1.5 × 10
-5g/L, all the other experiment conditions are identical.Experimental result finds, chemiluminescent response several compared to other, aptamers-Acetamiprid demonstrates the chemiluminescence signal of a remarkable cancellation.Result shows: this method has good selectivity.
Claims (6)
1. the method for Acetamiprid in chemiluminescence detection waste water, is characterized in that, comprise the following steps:
Acetamiprid aptamers and the waste water containing Acetamiprid are interacted, adds Nano silver solution; Moved in chemiluminescence pond by Nano Silver-aptamers after effect-Acetamiprid solution, the luminol that reinjects-silver nitrate chemical illuminating reagent, carries out luminescence-producing reaction, carries out quantitative measurement, namely obtain the concentration of Acetamiprid in waste water to the intensity of luminescence-producing reaction.
2. in the chemiluminescence detection waste water according to claims 1, the method for Acetamiprid, is characterized in that, the Nano Silver particle diameter in described Nano silver solution is 15nm, and concentration is 3.2 × 10
-10mol/L.
3. in the chemiluminescence detection waste water according to claims 1, the method for Acetamiprid, is characterized in that, the concentration of Acetamiprid aptamers is 6 × 10
-6mol/L, the action time of Acetamiprid aptamers and Acetamiprid is 10 minutes.
4. in the chemiluminescence detection waste water according to claims 1, the method for Acetamiprid, is characterized in that, described Nano silver solution is adopted and obtained with the following method: be 1 × 10 by 25mL concentration
-3the 75mL concentration that the liquor argenti nitratis ophthalmicus of mol/L dropwise joins high-speed stirred is 2 × 10
-3in the sodium borohydride solution of mol/L, react 10 minutes, then to add 5mL massfraction be that 1% sodium citrate solution is as stabilizing agent.
5. in the chemiluminescence detection waste water according to claims 1, the method for Acetamiprid, is characterized in that, described Lu meter Nuo – silver nitrate chemical illuminating reagent is by 5 × 10
-5the luminol solution of mol/L and 1.0 × 10
-4the liquor argenti nitratis ophthalmicus of mol/L is mixed to get with 1:1 volume ratio.
6. in the chemiluminescence detection waste water according to claims 1, the method for Acetamiprid, is characterized in that, the pH value of described luminol-silver nitrate chemical illuminating reagent is 12.0.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044862A (en) * | 2019-02-15 | 2019-07-23 | 东莞出入境检验检疫局检验检疫综合技术中心(东莞国际旅行卫生保健中心) | Method based on ferroso-ferric oxide polypyrrole and fluorescent material detection Acetamiprid |
| CN111443080A (en) * | 2019-01-17 | 2020-07-24 | 大韩民国(国立水产科学院) | Intelligent water quality measuring system for aquaculture |
Citations (1)
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| CN104964967A (en) * | 2015-05-26 | 2015-10-07 | 福建工程学院 | Method for detecting aniline in water sample by using chemiluminescence reagent |
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| CN104964967A (en) * | 2015-05-26 | 2015-10-07 | 福建工程学院 | Method for detecting aniline in water sample by using chemiluminescence reagent |
Non-Patent Citations (2)
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| 奚忠华: "基于核酸适配体与纳米银作用的无标记比色和化学发光分析", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111443080A (en) * | 2019-01-17 | 2020-07-24 | 大韩民国(国立水产科学院) | Intelligent water quality measuring system for aquaculture |
| CN110044862A (en) * | 2019-02-15 | 2019-07-23 | 东莞出入境检验检疫局检验检疫综合技术中心(东莞国际旅行卫生保健中心) | Method based on ferroso-ferric oxide polypyrrole and fluorescent material detection Acetamiprid |
| CN110044862B (en) * | 2019-02-15 | 2021-06-25 | 东莞海关综合技术中心 | Method for detecting acetamiprid based on ferroferric oxide polypyrrole and fluorescent material |
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