CN104990918A - Test paper film based on nanogold and method for detecting lead ion by test paper film - Google Patents
Test paper film based on nanogold and method for detecting lead ion by test paper film Download PDFInfo
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- CN104990918A CN104990918A CN201510418091.5A CN201510418091A CN104990918A CN 104990918 A CN104990918 A CN 104990918A CN 201510418091 A CN201510418091 A CN 201510418091A CN 104990918 A CN104990918 A CN 104990918A
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- 238000012360 testing method Methods 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 30
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 210000002469 basement membrane Anatomy 0.000 claims abstract description 4
- 239000010931 gold Substances 0.000 claims description 64
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 58
- 229910052737 gold Inorganic materials 0.000 claims description 57
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- -1 thiosulfate anion Chemical class 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- FRGKKTITADJNOE-UHFFFAOYSA-N sulfanyloxyethane Chemical compound CCOS FRGKKTITADJNOE-UHFFFAOYSA-N 0.000 claims description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 210000004379 membrane Anatomy 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
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- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 3
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 3
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- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
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- MCEBKLYUUDGVMD-UHFFFAOYSA-N [SiH3]S(=O)=O Chemical compound [SiH3]S(=O)=O MCEBKLYUUDGVMD-UHFFFAOYSA-N 0.000 description 2
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- JLCPHMBAVCMARE-UHFFFAOYSA-N [3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-[[3-[[3-[[3-[[3-[[3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-[[5-(2-amino-6-oxo-1H-purin-9-yl)-3-hydroxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxyoxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(5-methyl-2,4-dioxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(6-aminopurin-9-yl)oxolan-2-yl]methoxy-hydroxyphosphoryl]oxy-5-(4-amino-2-oxopyrimidin-1-yl)oxolan-2-yl]methyl [5-(6-aminopurin-9-yl)-2-(hydroxymethyl)oxolan-3-yl] hydrogen phosphate Polymers Cc1cn(C2CC(OP(O)(=O)OCC3OC(CC3OP(O)(=O)OCC3OC(CC3O)n3cnc4c3nc(N)[nH]c4=O)n3cnc4c3nc(N)[nH]c4=O)C(COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3COP(O)(=O)OC3CC(OC3CO)n3cnc4c(N)ncnc34)n3ccc(N)nc3=O)n3cnc4c(N)ncnc34)n3ccc(N)nc3=O)n3ccc(N)nc3=O)n3ccc(N)nc3=O)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cc(C)c(=O)[nH]c3=O)n3cc(C)c(=O)[nH]c3=O)n3ccc(N)nc3=O)n3cc(C)c(=O)[nH]c3=O)n3cnc4c3nc(N)[nH]c4=O)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)n3cnc4c(N)ncnc34)O2)c(=O)[nH]c1=O JLCPHMBAVCMARE-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates a test paper film based on nanogold and a method for detecting lead ion by the test paper film; a nano-titanium dioxide coating is coated on a basement membrane of the test paper film, and the nano-titanium dioxide coating is adhered with the nanogold and thiosulfuric acid root shell which are fixed by sulfydryl and amidogen. The invention also provides a method for detecting the lead ion in water by the test paper film based on the nanogold, the pre-treatment process for a sample to be detected is not needed, and large-scale equipment is not needed either; the method provided by the invention has the advantages of fast detection speed, low cost, strong anti-interference and low limit of detection; the detection lower limiting value of the lead ion can reach 5nM.
Description
Technical field
The invention belongs to ion detection technical field, being specifically related to a kind of based on nanometer gold test paper film and the method for detecting lead ion thereof.
Background technology
Lead is a kind of toxic heavy metal, the plumbous pollution to environment, and one is by the industrial and mining enterprises smelting, manufacture and use leadwork, especially causes from the lead waste water of discharging in nonferrous metallurgical process, waste gas and waste residue.Two is that the waste gas containing lead of being discharged by automobile causes, and uses lead tetraethyl as octane promoter in gasoline, and in gasoline combustion process, plumbous waste gas of just discharging with automobile enters air.In addition, some arbitrarily abandon containing lead accumulator and make lead contamination distribution extensive especially.Lead ion can cause environment and human health and have a strong impact on, even if also can have strong toxic action to human nerve during a small amount of contact, affects the behavior of people, brain development and MNCV.Child's brain is more responsive than adult to lead contamination.Lead in air has harmful effect to the intelligent development of children and behavior.When the blood lead of children exceedes every 600 micrograms per litre, there will be intellectual developmental disorder and abnormal behavior.The safety margin of national Specification potable water lead content is that 10 ppb(are about 0.048 μM).Therefore, plumbous detection is extremely important.
The traditional detection method of lead ion has atomic absorption method (AAS), spectrophotometric method, inductively coupled plasma mass spectrometry (ICP – MS), x ray fluorescence spectrometry and electrochemical process etc., but these methods usually will costly equipment, all have employed comparatively complicated experimental technique condition, require that testing staff has darker professional knowledge.Therefore these detection methods are only applicable to the analysis of large-scale experiment room usually, are difficult to promote.In recent years, along with the progress of technology, some technology utilizing DNA enzymatic, Small molecular, oligonucleotides, protein etc. to detect lead ion develop to some extent, these technology have good selectivity to lead ion, accuracy is higher, but comparatively speaking, operation easier is still larger, cost is also higher, is therefore also not suitable for promoting the use of.
Compared to above-mentioned detection method, colourimetry has the advantage of its uniqueness, and such as its result naked eyes are visible, without the need to complex instrument, cost is low and be very applicable to on-site measurement.Nm of gold has very strong surface plasma resonance (SPR) performance, as shown in Figure 1, its absorption spectrum can produce a sharp-pointed surface plasma resonance peak near 520 nm, and the position at this peak can change with the change of nm of gold particle diameter and interparticle distance.When distance between nm of gold reduces (by dispersed to aggregation state change), the position of SPR absorption peak can change, and can produce than colour response, and solution colour also can become blueness from redness gradually.But can cause utilizing the detection method of nm of gold very unstable in practical operation by this aggregation method, the as easy as rolling off a log external condition that is subject to is disturbed.Find in practice that many kinds of substance can cause aggreation to cause color to change, therefore, the specificity of current colourimetry is not strong, is not suitable for detecting lead ion in complex environment, is more not suitable for detecting on the spot.
Change nm of gold particle size thus the method for the colorimetric detection lead ion causing SPR to change can strengthen its specificity by oxidation-reduction method, there is very large advantage.But detect in the liquid phase by this method and be equally easily subject to the impact of external interference factor and aggreation occurs, affect testing result.Nm of gold is adsorbed onto solid phase environmental energy to address this problem well, but nm of gold is easy to come off in solid phase environment, causes false-positive phenomenon, cause testing result distortion.How
Nm of gold is stabilized in solid phase environment be a great problem of this area always.
Summary of the invention
The invention provides and be a kind ofly intended to solve the problem based on nanometer gold test paper film and the method for detecting lead ion thereof, make the result of the colorimetric detection of lead ion accurately and be easy to detect use at the scene.
To achieve these goals, the technical solution used in the present invention is as follows:
Based on a test paper film for nm of gold, basilar memebrane is covered with nanometer titanium dioxide coating, this coating is attached with the nm of gold and thiosulfate anion shell of being fixed by sulfydryl and amino.Basilar memebrane is the one in ordinary filter paper, nitrocellulose filter, cellulose acetate membrane, pvdf membrane.
The preparation method of the above-mentioned test paper film based on nm of gold, comprises the following steps:
1) soak modification: at 50-70 DEG C, basilar memebrane is placed in absolute ethyl alcohol and soaks 2-4 hour, then be placed in dry 10-20 minute under 40-60 DEG C of condition;
2) connect titania process: be immersed in titanium solution by the basilar memebrane after step 1) process, be positioned on shaking table and shake 30 minutes, the surplus liquid of erasing basement membrane surface, makes titanium solution be evenly distributed on basilar memebrane, dry 10-20 minute at 40-60 DEG C; Repeat aforesaid operations twice; The mixing solution that described titanium solution is the absolute ethyl alcohol of volume ratio 10:2 ~ 6:1, butyl titanate, glacial acetic acid are made into;
3) be hydrolyzed: by step 2) process after basilar memebrane put into deionized water, at 120-150 DEG C, be hydrolyzed 2-5 hour, take out this basilar memebrane be placed in 40-60 DEG C at dry 10-20 minute, obtain the test paper film of titania overlay film;
4) sulfydryl is connect: with (3-mercaptopropyi) trimethoxy silane of absolute ethyl alcohol to be solvent dose volume concentration be 1%-4%, test paper film step 3) obtained soaks wherein, and reacts 0.4-0.8 hour at 90-110 DEG C; Take out above-mentioned test paper film, use deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C;
5) amino is connect: by the 3-aminopropyl trimethoxysilane of absolute ethyl alcohol to be solvent dose volume concentration be 2%-5%, test paper film step 4) obtained soaks wherein, reacts 0.5-0.8 hour at being placed in 80-100 DEG C; Take out this test paper film, use deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C;
6) AuNps-BSA solution is prepared: utilize 1% acetic acid solution dissolve shitosan and make chitosan concentration reach 3mg/mL, by 2mL massfraction be 1% chlorauric acid solution join in the above-mentioned solution of 50mL, heat under 70-100 DEG C of condition, when solution from faint yellow become peony time stop heating, stir until cool to room temperature, form nano-Au solution; Bovine serum albumin and BSA added above-mentioned nano-Au solution and mixes, making the concentration of BSA in solution be 3 μMs, forming AuNps-BSA solution;
7) nanometer gold test paper film is prepared: by the test paper film cutting slivering obtained in step 5); AuNps-BSA dissolution homogeneity step 6) prepared is added drop-wise on described test paper film, then uses deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C; Repeat aforesaid operations 2-5 time, to increase the amount of the AuNps-BSA that test strips is adsorbed and to heighten the color; Obtained nanometer gold test paper film;
8) nm of gold and thiosulfate anion shell is formed: it is 5-20 minute in the hypo solution of 200-600mM that test paper film step 9) obtained is immersed in concentration, use deionized water rinsing several times again and at 40-60 DEG C dry 10-20 minute, the obtained test paper film based on nm of gold.
Detect a method for lead ion in water, comprise the following steps:
1) with the 3-mercaptoethanol solution of deionized water to be solvent compound concentration be 200-500mM;
2) solution to be detected is added drop-wise in the solution of step 1) preparation, and the above-mentioned test paper film based on nm of gold is placed in this solution, at 50-85 DEG C, heat 15-40 minute, when test strips is faded, get final product qualitative detection to lead ion.
If realize quantitative detection, so above-mentioned steps 2) should operate according to the following steps:
(1) the 3-mercaptoethanol solution being 500mM by 50 μ L solution to be measured and 950 μ L concentration mixes, and the test paper film based on nm of gold is placed in this solution, is settled to 1mL, at 50-85 DEG C, heat 15-40 minute; Take out test paper film, by washed with de-ionized water, dry 5-20 minute at being placed in 40-60 DEG C;
(2) sweep the picture of the test paper film got in step (1) with scanner, analyzed the changes values obtaining green passage by RGB, bring the plumbum ion concentration that quantitatively can detect solution to be measured in typical curve into.
Compared with prior art, the present invention has following beneficial effect:
1. the present invention is based on the test paper film of nm of gold, wherein nm of gold makes and adopts shitosan reducing process, due to the space steric effect of shitosan, makes nm of gold more stable, not easily clustering phenomena occurs; Shitosan and base material film combine, and make nm of gold better be fixed on film material, have better stability under its normal temperature condition; Also there is the advantages such as environmental protection simultaneously.
2. further, test paper film production is simple and easy, and cost is very low, convenient to operation, can carry out real-time on-site operation and test paper membrane stability is very high, does not fade under the high temperature conditions.The test strips holding time is long, can lay in for a long time, can preserve about 12 months according to practice examining.
3. the present invention detects the method for lead ion in water, simple to operate, detects degree of accuracy high, can detect and be about 48.3nM lower than in national standard to the minimum value 10ppb(of the lead ion pollution content of potable water).
4. the antijamming capability detecting the lead ion of lead ion in water is strong, good antijamming capability is had to potassium, sodium, magnesium, iron, aluminium, manganese, calcium, zinc, cobalt, nickel, copper, germanium, silver-colored plasma, very strong to the detection selectivity of lead ion, and good Detection results can be had in complex environment in human serum.
Accompanying drawing explanation
Fig. 1-nm of gold is at the uv absorption spectra at 520 nm places;
Fig. 2-test paper film provided by the present invention;
Fig. 3-canonical plotting of the present invention;
RGB changing value figure in Fig. 4-ion interference experiment of the present invention;
Color variation diagram after Fig. 5-test paper film of the present invention and lead at different concentrations ionic reaction.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
one, based on a test paper film for nm of gold,this test paper film is that basilar memebrane is covered with nanometer titanium dioxide coating, this coating is attached with the nm of gold and thiosulfate anion shell of being fixed by sulfydryl and amino.
Wherein, basilar memebrane is the one in ordinary filter paper, nitrocellulose filter, cellulose acetate membrane, pvdf membrane.
two, the preparation method of the above-mentioned test paper film based on nm of gold, comprise the following steps:
1) soak modification: at 50-70 DEG C, basilar memebrane is placed in absolute ethyl alcohol and soaks 2 hours, then to be placed under 40 DEG C of conditions dry 10 minutes;
2) connect titania process: be immersed in titanium solution by the basilar memebrane after step 1) process, be positioned on shaking table and shake 30 minutes, the surplus liquid of erasing basement membrane surface, makes titanium solution be evenly distributed on basilar memebrane, drying 10 minutes at 50 DEG C; Repeat aforesaid operations twice; The mixing solution that described titanium solution is the absolute ethyl alcohol of volume ratio 10:3:1, butyl titanate and glacial acetic acid are made into;
3) be hydrolyzed: by step 2) basilar memebrane after process puts into deionized water, at 135 DEG C, be hydrolyzed 4 hours, take out this basilar memebrane be placed in 50 DEG C at dry 10 minutes, obtain the test paper film of titania overlay film;
4) connect sulfydryl: with absolute ethyl alcohol to be solvent dose volume concentration be 2.5% (3-mercaptopropyi) trimethoxy silane, test paper film step 3) obtained soaks wherein, and reacts 0.5 hour at 100 DEG C; Take out above-mentioned test paper film, use deionized water rinsing several times, drying 15 minutes at being placed in 50 DEG C;
5) connect amino: with absolute ethyl alcohol to be solvent dose volume concentration be 3% 3-aminopropyl trimethoxysilane, test paper film step 4) obtained soaks wherein, reacts 0.5 hour at being placed in 100 DEG C; Take out this test paper film, use deionized water rinsing several times, drying 10 minutes at being placed in 50 DEG C;
6) AuNps-BSA solution is prepared: utilize 1% acetic acid solution dissolve shitosan and make chitosan concentration reach 3mg/mL, by 2mL massfraction be 1% chlorauric acid solution join in the above-mentioned solution of 50mL, heat under 100 DEG C of conditions, when solution from faint yellow become peony time stop heating, stir until cool to room temperature, form nano-Au solution;
Bovine serum albumin and BSA added above-mentioned nano-Au solution and mixes, making the concentration of BSA in solution be 3 μMs, forming AuNps-BSA solution;
7) nanometer gold test paper film is prepared: the strip test paper film obtained in step 5) being cut into 0.9cm*0.9cm size; AuNps-BSA dissolution homogeneity step 6) prepared is added drop-wise on described test paper film, then uses deionized water rinsing several times, drying 10 minutes at being placed in 50 DEG C; Repeat aforesaid operations three times, to increase the amount of the AuNps-BSA that test strips is adsorbed and to heighten the color; Obtained nanometer gold test paper film;
8) form nm of gold and thiosulfate anion shell: it is in the hypo solution of 500mM 10 minutes that test paper film step 9) obtained is immersed in concentration, then use deionized water rinsing several times and at 50 DEG C dry 10 minutes, the obtained test paper film based on nm of gold.
Basilar memebrane covers nanometer titanium dioxide coating, and adheres to sulfydryl and amino on the coating layer, nm of gold so just can be enable to be fixed on test paper film firmly, make it can not come off in processing thereafter with in detecting: because TiO
2as base material, for follow-up silylating reagent provides attachment site, amino silane and hydrosulphonyl silane are all used to enable nm of gold receive on test paper mould by chemical bond-linking, but hydrosulphonyl silane hydrophobicity, amino silane water wettability, only just can make nm of gold stable and uniform be adsorbed onto on made test paper film according to a definite sequence and ratio.
With thiosulfuric acid reactant salt, make test paper film generates gold and thiosulfate anion shell, namely following reaction occur:
4Au
0+ O
2+ 2H
2o+8(S
2o
3)
2- 4Au (S
2o
3)
2 3-+ 4OH
-, gold and thiosulfate anion shell can stop itself and 3-mercaptoethanol to react, and make test paper film have exclusive reaction for lead ion.
three, a kind of method detecting lead ion in water, comprise the following steps:
1) with the 3-mercaptoethanol solution of deionized water to be solvent compound concentration be 500mM;
2) solution to be detected is added drop-wise in the solution of step 1) preparation, and the above-mentioned test paper film based on nm of gold is placed in this solution, heat 20 minutes at 65 DEG C, when test strips armpit look and qualitative detection are to lead ion.
Wherein, step 2) quantitative detection can be realized by following steps:
(1) the 3-mercaptoethanol solution being 500mM by 50 μ L solution to be measured and 950 μ L concentration mixes, and the above-mentioned test paper film based on nm of gold is placed in this solution, be settled to 1mL, heat 20 minutes at 65 DEG C, take out test paper film, spend appropriate deionized water washings, drying 10 minutes at being placed in 50 DEG C;
(2) sweep the picture of the test paper film got in step (1) with scanner, analyzed the changes values obtaining green passage by RGB, bring the plumbum ion concentration that quantitatively can detect solution to be measured in typical curve into.
Gold and thiosulfate anion shell can stop itself and 3-mercaptoethanol to react, but after adding lead ion, can form Pb-Au key, destroy this shell, and reaction is continued.First nm of gold stable and uniform is adsorbed in the test strips of making by the present invention, and be soaked in certain density hypo solution, its surface is made to form one deck gold shell, after adding lead ion and mercaptoethanol, reaction continues, thus cause gold nano particle diameter to reduce until react completely, color produces significant change, color change and plumbum ion concentration positive correlation.
four, Specification Curve of Increasing:
The solution be the 2-ME solution of 500mM by five part of 950 μ L concentration being 0nM, 50nM, 100nM, 250nM, 500nM, 750nM with 50 μ L plumbum ion concentrations respectively mixes, all be settled to 1mL, test paper film based on nm of gold is soaked wherein respectively, heating 20 minutes at 65 DEG C, take out test paper film, spend appropriate deionized water washings, drying 10 minutes at being placed in 50 DEG C.
Sweep the picture getting above-mentioned test paper film with scanner respectively, analyzed the changes values obtaining green passage by RGB, obtain curve as shown in Figure 3: y=0.07888x+24.43 R
2=0.9719 range of linearity is 50-800nM/L.Lowest detectable limit is about 5nM, lower than GB lower limit.
five, ion interference capacity experimental
To be 2-ME solution and the 50 μ L concentration of 500mM respectively by 950 μ L concentration be, and lead, potassium, sodium, magnesium, iron, aluminium, manganese, calcium, zinc, cobalt, nickel, copper, germanium, the silver-colored isoionic solution of 10 μMs mixes, all be settled to 1mL, test paper film based on nm of gold is soaked wherein respectively, heat 20 minutes at 65 DEG C, take out test paper film, spend appropriate deionized water washings, drying 10 minutes at being placed in 50 DEG C.
Sweep with scanner the picture getting above-mentioned test paper film respectively again, analyzed the changes values obtaining green passage by RGB, result as shown in Figure 4.The test paper film based on nm of gold in the present invention has good antijamming capability to potassium, sodium, magnesium, iron, aluminium, manganese, calcium, zinc, cobalt, nickel, copper, germanium, silver-colored plasma, proves extremely strong selectivity.
six, based on the discoloration after the test paper film of nm of gold and lead at different concentrations ionic reaction
By the 2-ME solution of 500mM/L respectively with Pb
2+concentration be 0nM, 50nM, 100nM, 250nM, 500nM, 750nM solution by volume 19:1 be mixed to form six Duplicate Samples, again the test paper film based on nm of gold is soaked in Duplicate Samples solution respectively, water-bath at 65 DEG C, take out after about 20 minutes, by washed with de-ionized water, drying 10 minutes at being placed in 50 DEG C.
Test paper color change in each Duplicate Samples is followed successively by shown in Fig. 5.After this experiment proved response, the color of test paper film is thin out with the increase of the plumbum ion concentration reacted with it.
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. based on a test paper film for nm of gold, it is characterized in that, basilar memebrane is covered with nanometer titanium dioxide coating, this coating is attached with the nm of gold and thiosulfate anion shell of being fixed by sulfydryl and amino.
2. the test paper film based on nm of gold according to claim 1, is characterized in that, described basilar memebrane is ordinary filter paper, nitrocellulose filter, cellulose acetate or pvdf membrane.
3. the test paper film based on nm of gold according to claim 1 and 2, is characterized in that, adopt following preparation method, comprise the following steps:
1) soak modification: at 50-70 DEG C, basilar memebrane is placed in absolute ethyl alcohol and soaks 2-4 hour, then be placed in dry 10-20 minute under 40-60 DEG C of condition;
2) connect titania process: be immersed in titanium solution by the basilar memebrane after step 1) process, be positioned on shaking table and shake 30 minutes, the surplus liquid of erasing basement membrane surface, makes titanium solution be evenly distributed on basilar memebrane, dry 10-20 minute at 40-60 DEG C; Repeat aforesaid operations twice; The mixing solution that described titanium solution is the absolute ethyl alcohol of volume ratio 10:2 ~ 6:1, butyl titanate and glacial acetic acid are made into;
3) be hydrolyzed: by step 2) process after basilar memebrane put into deionized water, at 120-150 DEG C, be hydrolyzed 2-5 hour, take out this basilar memebrane be placed in 40-60 DEG C at dry 10-20 minute, obtain the test paper film of titania overlay film;
4) sulfydryl is connect: with (3-mercaptopropyi) trimethoxy silane of absolute ethyl alcohol to be solvent dose volume concentration be 1%-4%, test paper film step 3) obtained soaks wherein, and reacts 0.4-0.8 hour at 90-110 DEG C; Take out above-mentioned test paper film, use deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C;
5) amino is connect: by the 3-aminopropyl trimethoxysilane of absolute ethyl alcohol to be solvent dose volume concentration be 2%-5%, test paper film step 4) obtained soaks wherein, reacts 0.5-0.8 hour at being placed in 80-100 DEG C; Take out this test paper film, use deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C;
6) AuNps-BSA solution is prepared: utilize 1% acetic acid solution dissolve shitosan and make chitosan concentration reach 3mg/mL, by 2mL massfraction be 1% chlorauric acid solution join in the above-mentioned solution of 50mL, heat under 70-100 DEG C of condition, when solution from faint yellow become peony time stop heating, stir until cool to room temperature, form nano-Au solution;
Bovine serum albumin and BSA to be added in above-mentioned nano-Au solution and to mix, making the concentration of BSA in solution be 3 μMs, forming AuNps-BSA solution;
7) nanometer gold test paper film is prepared: by the test paper film cutting slivering obtained in step 5); AuNps-BSA dissolution homogeneity step 6) prepared is added drop-wise on described test paper film, then uses deionized water rinsing several times, dry 10-20 minute at being placed in 40-60 DEG C; Repeat aforesaid operations 2-5 time, to increase the amount of the AuNps-BSA that test strips is adsorbed and to heighten the color; Obtained nanometer gold test paper film;
8) nm of gold and thiosulfate anion shell is formed: it is 5-20 minute in the hypo solution of 200-600mM that test paper film step 9) obtained is immersed in concentration, use deionized water rinsing several times again and at 40-60 DEG C dry 10-20 minute, the obtained test paper film based on nm of gold.
4. detect a method for lead ion in water, it is characterized in that, comprise the following steps:
1) with the 3-mercaptoethanol solution of deionized water to be solvent compound concentration be 200-500mM;
2) solution to be detected is added drop-wise in the solution of step 1) preparation, and the test paper film based on nm of gold described in claim 1,2 or 3 is placed in this solution, at 50-85 DEG C, heat 15-40 minute, when test strips is faded, get final product qualitative detection to lead ion.
5. the method for detection lead ion according to claim 5, is characterized in that, described step 2) comprise the following steps:
(1) the 3-mercaptoethanol solution being 500mM by 50 μ L solution to be measured and 950 μ L concentration mixes, and the test paper film based on nm of gold according to claim 1 or claim 2 is placed in this solution, be settled to 1mL, at 50-85 DEG C, heat 15-40 minute; Take out test paper film, by washed with de-ionized water, dry 5-20 minute at being placed in 40-60 DEG C;
(2) sweep the picture of the test paper film got in step (1) with scanner, analyzed the changes values obtaining green passage by RGB, bring the plumbum ion concentration that quantitatively can detect solution to be measured in typical curve into.
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