CN108732167A - The method that rapid field detection is carried out to Polychlorinated biphenyls total amount with papery detection device - Google Patents
The method that rapid field detection is carried out to Polychlorinated biphenyls total amount with papery detection device Download PDFInfo
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- CN108732167A CN108732167A CN201710249839.2A CN201710249839A CN108732167A CN 108732167 A CN108732167 A CN 108732167A CN 201710249839 A CN201710249839 A CN 201710249839A CN 108732167 A CN108732167 A CN 108732167A
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Abstract
The invention discloses the method for carrying out rapid field detection to Polychlorinated biphenyls total amount with papery detection device, steps：1) there is the figure of the rectangle of circular distribution among design；2) wax spray is printed upon part of the rectangle in addition to circle is sentenced；3) it heats, wax is made to penetrate filter paper, it is cooling, papery detection device is obtained, wax spray one side claims the faces A；4) aptamer is added at the circle in the faces A, it is dry；5) hexane solution of the Polychlorinated biphenyls standard items of series concentration and sample to be tested Polychlorinated biphenyls n-hexane extract are added at different circles；It is dry；Phosphate buffer solution, gold nano colloidal sol, sodium-chloride water solution reaction is added to take pictures；6) color analysis, and make standard curve；7) sample to be tested Polychlorinated biphenyls calculates the concentration of Polychlorinated biphenyls in sample to be tested according to standard curve.Papery detection device of the present invention is small and exquisite portable, is convenient for Site Detection；It is at low cost, it is easy to operate；Used device is convenient for processing.Qualitative and quantitative analysis is carried out to Polychlorinated biphenyls.
Description
Technical field
The present invention relates to a kind of methods carrying out rapid field detection to Polychlorinated biphenyls total amount.
Background technology
Polychlorinated biphenyls is a series of general designation of chlorinated organics, belongs to persistent organic pollutants.Its chemical property is stablized,
It is not soluble in water and be soluble in fat with very high toxicity, it is easily accumulated in organism, there is carcinogenicity and neurotoxicity.
Therefore, the Polychlorinated biphenyls in environment, food is detected, especially to the detection of Trace Polychlorinated Biphenyls, is very important.Together
When, the timely monitoring of Polychlorinated biphenyls leakage accident, is also very important in environment.
The existing method for measuring Polychlorinated biphenyls includes mainly two steps, sample extraction and detection.Since Polychlorinated biphenyls is easy
It is dissolved in organic solvent, and it is not soluble in water, therefore common organic solvent, such as n-hexane are extracted and are enriched with to Polychlorinated biphenyls.
Treated sample, is often used high performance liquid chromatography (HPLC) or liquid chromatograph mass spectrography (LC/MS) is detected.By
It is needed using expensive large-scale detecting instrument in such detection method, therefore is only applicable to laboratory use, detection is spent
It is relatively high, and have stringent experimental technique requirement to operating personnel.
Simultaneously as Polychlorinated biphenyls sample is often extracted with organic solvent, therefore many common methods can not be to it
It is detected.Because existing method is aqueous phase reactions mostly, solubility is very low in organic solvent for reagent, if addition sample (
In organic solvent), lamination is will produce, to prevent the effecting reaction of solvent and determinand, leads to not be detected.
Also certain methods after organic solvent is added, may lead to its inactivation or activity change, such as using reagents such as protein
Enzyme-linked immunization (ELISA).
Invention content
It is a kind of instead of large-scale instrument the purpose of the present invention is overcoming the deficiencies of the prior art and provide, paper is used easily to operate
The method that quality detecting device carries out rapid field detection to Polychlorinated biphenyls total amount.
Technical scheme of the present invention is summarized as follows：
The method for carrying out rapid field detection to Polychlorinated biphenyls total amount with papery detection device, includes the following steps：
1) design detection device figure, the detection device figure be centre have circle 1 distribution rectangle, the circle it is straight
Diameter is 5.0mm；
2) wax spray printer is used, according to the design of step 1), wax spray prints on filter paper, and the wax of printing is made to be located at rectangle
Part 2 in addition to circle is sentenced；
3) filter paper after printing wax spray is placed in heating dish, and heating makes wax penetrate filter paper, is cooled to room temperature, obtains papery
The one side that the wax spray of filter paper prints is known as the faces A by detection device；
4) aptamer 10pmol is added at the circle in the faces A, it is dry；
5) by the hexane solution of the Polychlorinated biphenyls standard items of 0.5 μ L series concentrations and 0.5 μ L sample to be tested Polychlorinated biphenyls
N-hexane extract is added at different circles；It is dry；5 μ L, pH=7.2,10mM phosphate buffer solution is added, reacts 15 points
Clock；1 μ L of gold nano colloidal sol are added, react 5 minutes；2 μ L, 0.25M sodium-chloride water solutions is added, places 5 minutes, observation result is simultaneously
It takes pictures；
6) image analysis software is used, to the hexane solution of the Polychlorinated biphenyls standard items of the series concentration of step 5) acquisition
Photo carry out result color analysis, and make standard curve；
7) image analysis software is used, the sample to be tested Polychlorinated biphenyls n-hexane extract photo that step 5) obtains is carried out
As a result color analysis calculates the concentration of Polychlorinated biphenyls in sample to be tested according to standard curve.
Positive integer among the circular number is 5-96 is a.
The filter paper is qualitative filter paper or quantitative filter paper.
Advantages of the present invention：
1, papery detection device is small and exquisite, carries, conveniently moving, without using large-scale instrument, is convenient for Site Detection；
2, testing cost is cheap, easy to operate；
3, used device generation environment will not pollute again convenient for processing.
4, qualitative and quantitative analysis can be carried out to sample to be tested Polychlorinated biphenyls n-hexane extract.
Description of the drawings
Fig. 1 is to have 96 circular papery detection devices.
Fig. 2 is the measurement of Polychlorinated biphenyls sample.
Specific implementation mode
Aptamer source document：Mehta J,Rouah-Martin E,Van Dorst B,Maes B,Herrebout
W,Scippo ML,Dardenne F,Blust R,Robbens J.Selection and characterization of
PCB-binding DNA aptamers.Anal.Chem.2012；84:Aptamer 9.3 in 1669-76..
It is prepared by gold nano colloidal sol：
The 1mM aqueous solution of chloraurate of 50mL is heated to reflux and is stirred, after solution boiling, rapidly joins the 38.8mM of 5mL
Sodium citrate aqueous solution, after solution becomes peony, after continuing reflux 15 minutes, stirring is cooled to room temperature, in 4 degree of refrigerators
It preserves.
To wax spray printer without limiting, used wax spray printer is selected from the present invention：Xerox ColorQube
8580, Xerox ColorQube 8700, Xerox ColorQube 8880 or Xerox ColorQube 8900.The present invention is each
Embodiment uses Xerox ColorQube 8700.
It is selected from using image analysis software：ImageJ, photoshop etc..
In order to make technical scheme of the present invention and feature be more clear, below in conjunction with the drawings and specific embodiments, to this
Invention is described further.Specific embodiment described herein is only used for explaining the present invention, but does not limit the protection of the present invention
Range.
Embodiment 1
The method for carrying out rapid field detection to Polychlorinated biphenyls total amount with papery detection device, includes the following steps：
1) detection device figure is designed on computers, and detection device figure is the rectangle that centre there are 96 circles 1 to be distributed, and is seen
Fig. 1, diameter of a circle 5.0mm；
2) wax spray printer is used, according to the design of step 1), wax spray prints on qualitative filter paper, and the wax of printing is made to be located at
Part 2 of the rectangle in addition to circle is sentenced；
3) filter paper after printing wax spray is placed in heating dish, is heated 3 minutes at 130 DEG C, so that wax is penetrated filter paper, be cooled to
Room temperature obtains papery detection device, and the one side that the wax spray of filter paper prints is known as the faces A；It is hydrophobic region that wax, which penetrates at filter paper, round
Place is hydrophilic region；
4) aptamer 10pmol is added at the circle in the faces A, it is dry；
5) hexane solution of Polychlorinated biphenyls standard items is prepared：Concentration is respectively 0,700,7 × 104With 7 × 106ng/L；Respectively
0.5 μ L are taken to be added at different circles；It is 1 minute dry；
It is another that 0.5 μ L sample to be tested Polychlorinated biphenyls n-hexane extracts is taken to be added at other circle；It is 1 minute dry；
(separately take 0.5 μ L a concentration of 1 × 107The circle of not aptamer is added in the hexane solution of ng/L Polychlorinated biphenyls
Place, it is 1 minute dry, be positive control)；
Each sample does three repeated experiments.
5 μ L pH=7.2,10mM phosphate buffer solutions is added, reacts 15 minutes；1 μ L gold nano colloidal sols are added, react 5 points
Clock；2 μ L 0.25M sodium-chloride water solutions are added, place 5 minutes, observe result and take pictures；
6) ImageJ image analysis softwares are used, after becoming multichannel picture, red channel is analyzed, step 5) is obtained
The photo and positive control photo of the hexane solution of the Polychlorinated biphenyls standard items of series concentration carry out result color analysis, will just
The color of hexane is as 100%, and positive control color is as 0%, to the hexane solution color of serial Polychlorinated biphenyls standard items
Data normalization is carried out, and makes standard curve；
7) ImageJ image analysis softwares are used, after becoming multichannel picture, red channel are analyzed, to the more chlorine of sample to be tested
The photo of biphenyl n-hexane extract carries out result color analysis and is obtained according to the color gamut of above-mentioned 0% and 100% defined
To the color result numerical value of the sample, and according to the concentration of Polychlorinated biphenyls in standard curve calculating sample, see Fig. 2.
According to the solution colour of standard curve and sample, the concentration of Polychlorinated biphenyls in sample is calculated：Obtained standard curve
For y=-12.96+96.68, formula calculates x=2.11 according to this, and Polychlorinated biphenyls concentration is 102.11=128.8ng/L.
Above-described embodiment is only preferred examples of the present invention, and is not intended to limit the present invention, all within the principle of the present invention,
Any modifications and variations done, within protection scope of the present invention.
Circular number is also selected from the arbitrary positive integer among 5-96.
Filter paper can also select quantitative filter paper.
Claims (3)
1. the method for carrying out rapid field detection to Polychlorinated biphenyls total amount with papery detection device, it is characterized in that including following step
Suddenly：
1) detection device figure is designed, the detection device figure is the rectangle that there is round (1) distribution in centre, the diameter of a circle
For 5.0mm；
2) wax spray printer is used, according to the design of step 1), wax spray prints on filter paper, and the wax of printing is made to be located at rectangle except circle
With outer part (2) at shape；
3) the filter paper heating after printing wax spray, makes wax penetrate filter paper, is cooled to room temperature, obtain papery detection device, by filter paper
The one side of wax spray printing is known as the faces A；
4) aptamer 10pmol is added at the circle in the faces A, it is dry；
5) by the hexane solution of the Polychlorinated biphenyls standard items of 0.5 μ L series concentrations and 0.5 μ L samples to be tested Polychlorinated biphenyls just oneself
Alkane extract is added at different circles；It is dry；5 μ L, pH=7.2,10mM phosphate buffer solution is added, reacts 15 minutes；
1 μ L of gold nano colloidal sol are added, react 5 minutes；2 μ L, 0.25M sodium-chloride water solutions is added, places 5 minutes, observation result is gone forward side by side
Row is taken pictures；
6) image analysis software is used, to the photograph of the hexane solution of the Polychlorinated biphenyls standard items of the series concentration of step 5) acquisition
Piece carries out result color analysis, and makes standard curve；
7) image analysis software is used, result is carried out to the sample to be tested Polychlorinated biphenyls n-hexane extract photo that step 5) obtains
Color analysis calculates the concentration of Polychlorinated biphenyls in sample to be tested according to standard curve.
2. according to the method described in claim 1, it is characterized in that the positive integer among the circular number is 5-96 is a.
3. according to the method described in claim 1, it is characterized in that the filter paper is qualitative filter paper or quantitative filter paper.
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Application publication date: 20181102 |