CN105319192A - Method for detecting hypochlorite anions through water-soluble fluorescent silica nanoparticle - Google Patents
Method for detecting hypochlorite anions through water-soluble fluorescent silica nanoparticle Download PDFInfo
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- CN105319192A CN105319192A CN201510771476.XA CN201510771476A CN105319192A CN 105319192 A CN105319192 A CN 105319192A CN 201510771476 A CN201510771476 A CN 201510771476A CN 105319192 A CN105319192 A CN 105319192A
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- hypochlorite
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Abstract
The invention discloses a method for detecting hypochlorite anions through a water-soluble fluorescent silica nanoparticle. A probe adopted by the method is the water-soluble fluorescent silica nanoparticle which is prepared from gamma-aminopropyltrimethoxysilane (APTES) and trisodium citrate. The fluorescent silica nanoparticle can realize high-selectivity and high-sensitivity detection on hypochlorite anions. Compared with the existing hypochlorite anion detecting technology, the method has the following advantages: the fluorescent silica nanoparticle is small in size, the required raw materials are rich, the preparation process is simple, the aftertreatment is convenient, the input cost is low, and the fluorescence intensity is higher; in addition, the method has excellent selectivity and sensitivity, and a wider detection range. Therefore, the method is suitable for practical production application and popularization, and is expected to be widely applied to the technical fields of analytical chemistry, environmental sciences, bioscience and the like.
Description
Technical field
The technical field that the present invention relates to comprises biological and environment ion detection, specifically, i.e. and the application of water soluble fluorescence silicon nano in hypochlorite detects.
Background technology
Aerobic cell can produce many reactive oxygen species (reactiveoxygenspecies, ROS) in metabolic processes, as:
1o
2, H
2o
2,
. oH and HClO etc.In numerous disease, ROS plays key player, and they are at the mode of action mainly oxidative pressure of living cells, but their effects in living cells are made a world of difference.Hypochlorite is a kind of highly reactive form of oxygen material, and the maximum difference of it and other active substance has close ties with our life.In vivo; hypochlorous acid to be equivalent in biosome one natural protective barrier; major function prevents microorganism from invading; but research finds; hypochlorite take part in the pathogenic course of many human body diseases; as: angiocardiopathy, neuronal cell pathology, lung's injury, liver disease, arthritis and some ephrosis etc.Hypochlorite application in the environment also should not be underestimated, and as everyone knows, the principal ingredient of common bleaching water is exactly sodium hypochlorite, so, design a kind of highly sensitive and single-minded hypochlorite probe significant.
The means detecting hypochlorite have a lot, and common detection method has high performance liquid chromatography, iodimetric titration, spectrophotometric method, Flow Injection Chemiluminescence and enzyme sensor method etc.High performance liquid chromatography sensing range is higher, but complex operation.Iodimetric titration Monitoring lower-cut is low, is difficult to accurately detect ClO
-concentration.Spectrophotometric method has the advantages such as sensing range is wide, favorable reproducibility, equipment simple, easy operation, so enjoy favor.
Fluorescent sensor molecule detection method belongs to spectrophotometric method, is to utilize fluorescence to change to the chemical information after expressing sensitive layer molecule and analytic target effect, and have very high selectivity and sensitivity, sensitivity can reach 10
-9~ 10
-12the order of magnitude of M, receive extensive concern in recent years, and be widely used in ion traces and the different field such as microanalysis, biomolecule identification, and be usually used in analyzing large number of biological and biochemical species, comprise anionic species, cationic, neutral molecule class and gas etc.
The hypochlorous acid of hypochlorite and its proton form and the life of the mankind closely bound up, so seem particularly important to its determination and analysis, the detection method before reported is comparatively loaded down with trivial details or sensitivity is not high, and the inventive method is to ClO
-there is higher sensitivity and selectivity, and sensing range is wider, can be used for practical application.
Summary of the invention
The object of the present invention is to provide a kind of method detecting hypochlorite, the method silicon nano size used is little, required abundant raw materials, preparation flow are simple, convenient post-treatment, input cost are low, fluorescence intensity is stronger, anti-light Bleachability strong, biocompatibility is better, and the method has good selectivity and sensitivity, sensing range is wider.Further research shows, this Fluorescent silicon nanoparticle can directly realize ClO in water
-high sensitivity, high selectivity recognition function.
The object of the invention is to be realized by following manner: a kind of water soluble fluorescence silicon nano detects the method for hypochlorite, comprises the following steps:
(1) configure the hypochlorite solution of variable concentrations, get appropriate hypochlorite solution and be added in silicon nano aqueous solution, stir 5 minutes; Measure the fluorescence intensity of silicon nano 445nm when 360nm excites, fluorescence intensity change value and hypochlorite concentration are worth linear fit, obtain standard regressive method;
(2) get in the water sample from the beginning that hypochlorite solution to be measured is added to containing silicon nano, stir 5 minutes; Measuring the fluorescence intensity of silicon nano 445nm when 360nm excites, by contrasting with standard regressive method, the concentration of hypochlorite to be measured in tap water can be obtained.
As optimization, in step (1), the buffer solution of described silicon nano water pH=7 is made into the aqueous solution that solid content is 0.03wt%.
As optimization, in step (1), described silicon nano is obtained by the method comprised the following steps:
A, trisodium citrate is soluble in water, be made into the solution that 10mL concentration is 30 ~ 50mg/ml, in nitrogen protection and under oxygen free condition, the aminopropyl trimethoxysilane (APTES) of relative trisodium citrate material amount 6 ~ 15 times (being preferably 8 ~ 9 times) is expelled in above-mentioned solution, stirring at normal temperature 10 minutes, in hydrothermal reaction kettle, react 4 ~ 8 hours at 160 DEG C;
B, select the bag filter of suitable molecular cut off, the solution be obtained by reacting by step a is dialysed 3 ~ 5 times in water, remove unreacted aminopropyl trimethoxysilane (APTES) and trisodium citrate, reacting coarse product is through dialysis, concentrated, precipitation, dry thus obtained one has ClO
-the Fluorescent silicon nanoparticle of recognition function.
As optimization, in step a, the concentration of described citric acid three sodium solution is 34mg/ml.
As optimization, in step a, the thing mass ratio of described trisodium citrate thing and aminopropyl trimethoxysilane (APTES) is 1:8 ~ 9.
As optimization, in step b, the molecular cut off of bag filter is 500.
That prepares according to above-mentioned preparation method has ClO
-the Fluorescent silicon nanoparticle of recognition function, its concrete course of reaction is as follows:
Fluorescent silicon nanoparticle in the present invention, a large amount of amino and part carboxyl of surface exposure, it is water-soluble preferably that this makes this silicon nano have, and the amino on surface is electron-donating group, thus make this nano particle have stronger blue-fluorescence.As everyone knows, ClO
-be a kind of strong oxidizer, and the amino activity on this silicon nano surface is higher, easily by ClO
-be oxidized to nitro or nitroso-, and nitro and nitroso-are the electron withdraw groups that a class is stronger, thus the electron withdraw group on silicon nano surface can be made to increase, reduce its fluorescence intensity.
Accompanying drawing explanation
Fig. 1 is Fluorescent silicon nanoparticle atomic force scanning electron microscope (SEM) photograph and slice map thereof, can find out that this silicon nano is evenly distributed, and mean diameter is 2 ran.
Fig. 2 is the uv absorption spectrogram of Fluorescent silicon nanoparticle, and absorption peak is positioned at 346nm wavelength place.
When Fig. 3 is different hypochlorite concentration, the fluorescence emission spectrum variation diagram (λ of Fluorescent silicon nanoparticle (solid content: 0.03wt%)
ex=360nm, λ
em=445nm), [ClO
-]=0(a), 1.0 × 10
-6mol/L(b), 2.0 × 10
-6mol/L(c), 3.0 × 10
-6mol/L(d), 4.0 × 10
-6mol/L(e), 5.0 × 10
-6mol/L(f), 7.0 × 10
-6mol/L(g), 1.0 × 10
-5mol/L(h), 4.0 × 10
-5mol/L(i), 7.0 × 10
-5mol/L(j), 1.0 × 10
-4mol/L(k), 2.0 × 10
-4mol/L(l), 4.0 × 10
-4mol/L(m), 7.0 × 10
-4mol/L(n), 1.0 × 10
-3mol/L(o).
Fig. 4 is the linear fit curve of fluorescence intensity change value and hypochlorite concentration's value.
Fig. 5 is that on the correlation data figure that affects of Fluorescent silicon nanoparticle fluorescence intensity, (solid content: 0.03wt%, the concentration of the negative ion after adding is 1.0 × 10 to various negative ion
-4mol/L, I/I
0the Fluorescent silicon nanoparticle adding front and back for each negative ion is taking 360nm as excitation wavelength, and 445nm is the ratio of transmitted wave strong point fluorescence intensity).
Fig. 6 is that on the correlation data figure that affects of Fluorescent silicon nanoparticle fluorescence intensity, (solid content: 0.03wt%, the anion concentration after adding is 1.0 × 10 to various negative ion when coexisting with hypochlorite ion respectively
-4mol/L, I/I
0the Fluorescent silicon nanoparticle adding front and back for each negative ion is taking 360nm as excitation wavelength, and 445nm is the ratio of transmitted wave strong point fluorescence intensity).
Fig. 7 is the life span comparison figure that Fluorescent silicon nanoparticle (solid content: 0.03wt%) adds before and after hypochlorite.
Fig. 8 is the anti-light bleachability of water soluble fluorescence nano particle.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Embodiment 1:
One has ClO
-the preparation method of the Fluorescent silicon nanoparticle of recognition function, comprises the following steps:
(1) by soluble in water for appropriate trisodium citrate, be made into 10mL solution, in nitrogen protection and under oxygen free condition, the aminopropyl trimethoxysilane (APTES) of relative trisodium citrate material amount 9 times is expelled in above-mentioned solution, stirring at normal temperature 10 minutes, in hydrothermal reaction kettle, react 5 hours at 160 DEG C;
(2) selective retention molecular weight is the bag filter of 500, solution step (1) be obtained by reacting is dialysed 4 times in water, remove unreacted aminopropyl trimethoxysilane (APTES) and trisodium citrate, reacting coarse product is through dialysis, concentrated, precipitation, dry thus obtained one has ClO
-the fluorescent nano particles of recognition function.
Embodiment 2: the test experience of hypochlorite:
(1) get 15 5ml cuvettes, what add gained in embodiment 1 respectively is diluted to the buffer solution of pH=7 the 3ml Fluorescent silicon nanoparticle aqueous solution that solid content is 0.03wt%, is then 0(a by concentration respectively), 1.0 × 10
-3mol/L(b), 2.0 × 10
-3mol/L(c), 3.0 × 10
-3mol/L(d), 4.0 × 10
-3mol/L(e), 5.0 × 10
-3mol/L(f), 7.0 × 10
-3mol/L(g), 0.01mol/L(h), 0.04mol/L(i), 0.07mol/L(j), 0.1mol/L(k), 0.2mol/L(l), 0.4mol/L(m), 0.7mol/L(n), 1.0mol/L(o) 3 μ l liquor natrii hypochloritises join in 15 cuvettes respectively, stir under normal temperature after 5 minutes, take 360nm as excitation wavelength, measure the fluorescence intensity of these samples respectively, obtain the fluorescence emission spectrum variation diagram of 15 samples, see Fig. 3.Test result shows: the fluorescence intensity of this Fluorescent silicon nanoparticle solution is along with ClO
-the increase gradually of concentration and progressively declining, and ClO
-during concentration >1 μm of ol/L, the fluorescence intensity of the aqueous solution of Fluorescent silicon nanoparticle occurs obviously to decline.
(2) 11 5mL cuvettes are got, what be respectively charged into gained in embodiment 1 is diluted to the buffer solution of pH=7 the 3ml Fluorescent silicon nanoparticle aqueous solution that solid content is 0.03wt%, measure these 11 samples respectively to excite at 360nm wavelength, the fluorescent emission intensity at 445nm wavelength emission place record; Then be the ClO of 0.1mol/L by concentration respectively
-, S
2-, NO
2 -, NO
3 -, CO
3 2-, OH
-, HCO
3 -, ClO
4 -, Cl
-, SO
4 2-and S
2o
3 2-respectively getting 3 μ l joins in 11 article colorimetric wares, stirring at normal temperature 5 minutes, then measures these 11 samples respectively and excites at 360nm wavelength, the fluorescent emission intensity at 445nm wavelength emission place record, and the result of front and back intensity contrast gained as shown in Figure 4.Measurement result shows: except ClO
-outward, the fluorescence intensity of other various negative ion above-mentioned to prepared Fluorescent silicon nanoparticle has no significant effect.
(3) 11 5ml cuvettes are got, what be respectively charged into gained in embodiment 1 is diluted to the buffer solution of pH=7 the 3ml Fluorescent silicon nanoparticle aqueous solution that solid content is 0.03wt%, measure these 11 samples respectively to excite at 360nm wavelength, the fluorescent emission intensity at 445nm wavelength emission place also keeps a record; Then, be the S of 0.1mol/L by concentration respectively
2-, NO
2 -, NO
3 -, CO
3 2-, OH
-, HCO3
-, ClO
4 -, Cl
-, SO
4 2-and S
2o
3 2-respectively get 3 μ l to join wherein in 10 article colorimetric wares, and in these 11 cuvettes, add 3 μ l concentration be the ClO of 0.1mol/L
-, stirring at normal temperature 5 minutes, measures these 11 samples respectively and excites at 360nm wavelength, the fluorescent emission intensity at 445nm wavelength emission place record, only adds ClO
-sample as blank, front and back intensity contrast acquired results is as shown in Figure 5.Result shows, it is less that these 10 kinds of negative ion above-mentioned detect interference to the hypochlorite of Fluorescent silicon nanoparticle.
(4) get a 5mL cuvette, what load gained in embodiment 1 is diluted to the buffer solution of pH=7 the 3ml Fluorescent silicon nanoparticle aqueous solution that solid content is 0.03wt%, measures its life-span; Then be the ClO of 0.6mol/L by 3 μ l concentration
-join in above-mentioned cuvette, stirring at normal temperature 5 minutes, measures its life-span.As shown in Figure 6, result shows the result recorded, and along with fluorescent weakened, the life-span of sample also shortens, and meets objective fact.
Embodiment 3: trying to achieve of standard regressive method comprises the following steps:
(1) buffer solution of the silicon nano pH=7 of embodiment 2 is made into the aqueous solution that solid content is 0.03wt%.
(2) get the above-mentioned solution of 3ml, add the hypochlorite solution of 3 μ l variable concentrations respectively, make the ultimate density of hypochlorite be respectively 0,1.0 × 10
-6mol/L, 2.0 × 10
-6mol/L, 3.0 × 10
-6mol/L, 4.0 × 10
-6mol/L, 5.0 × 10
-5mol/L, 7.0 × 10
-6mol/L, 1.0 × 10
-5mol/L, 4.0 × 10
-5mol/L, 7.0 × 10
-5mol/L, 1.0 × 10
-4mol/L, 2.0 × 10
-4mol/L, 4.0 × 10
-4mol/L, 7.0 × 10
-4mol/L, 1.0 × 10
-3mol/L.All stir 5min, measure the fluorescence intensity of their 445nm when 360nm excites respectively.
(3) carry out linear fit with the Strength Changes value of maximum fluorescence emission peak (445nm) and hypochlorite concentration, see Fig. 7, obtain equation of linear regression (F-F
0)/F
0=0.0449 × [hypochlorite] (R
2=0.992), sensing range is 1 μM ~ 7 μMs, and detect and be limited to 300nM, wherein [hypochlorite] represents the concentration of hypochlorite, and unit is μM.
Embodiment 4: in tap water, hypochlorite concentration measures:
Get the cuvette of 5mL, add 3mL water-reducible Fluorescent silicon nanoparticle solution from the beginning, regulate pH=7, measure the fluorescent emission intensity at its 445nm place when 360nm excites and record.Then the hypochlorite solution of 3 μ L variable concentrations is added respectively, stir 5 minutes, measure the fluorescence intensity (3 times) of its 445nm when 360nm excites again, by contrasting with equation of linear regression, the concentration of hypochlorite to be measured in tap water can be obtained, result is as shown in table 1, and the response rate that hypochlorite measures is better.
Table 1 is the detection to hypochlorite in tap water of water soluble fluorescence silicon nano
Embodiment 5: water soluble fluorescence nano particle anti-light Bleachability, step is as follows:
First, get 9 5ml cuvettes, what be respectively charged into gained in embodiment 1 is diluted to the buffer solution of pH=7 the 3ml Fluorescent silicon nanoparticle aqueous solution that solid content is 0.03wt%, measures these 9 samples respectively and excites at 365nm wavelength, and the fluorescent emission intensity at 445nm wavelength emission place also keeps a record; Then they being placed in wavelength is under the uviol lamp of 360nm, irradiate 10,20,30,40,50,60,70,80,90 minutes respectively, then measure them to excite at 365nm wavelength, the fluorescent emission intensity at 445nm wavelength emission place, contrasts the fluorescence intensity after pre-irradiation.As seen from Figure 8, this water soluble fluorescence nano particle has good anti-light Bleachability.
Above-described embodiment is used for explaining and the present invention is described, but not limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (6)
1. water soluble fluorescence silicon nano detects a method for hypochlorite, it is characterized in that, comprises the following steps:
(1) configure the hypochlorite solution of variable concentrations, get appropriate hypochlorite solution and be added in silicon nano aqueous solution, stir 5 minutes; Measure the fluorescence intensity of silicon nano 445nm when 360nm excites, fluorescence intensity change value and hypochlorite concentration are worth linear fit, obtain standard regressive method;
(2) get in the water sample from the beginning that hypochlorite solution to be measured is added to containing silicon nano, stir 5 minutes; Measuring the fluorescence intensity of silicon nano 445nm when 360nm excites, by contrasting with standard regressive method, the concentration of hypochlorite to be measured in tap water can be obtained.
2. water soluble fluorescence silicon nano according to claim 1 detects the method for hypochlorite, and it is characterized in that, as optimization, in step (1), the buffer solution of described silicon nano water pH=7 is made into the aqueous solution that solid content is 0.03wt%.
3., for detecting a preparation method for the water soluble fluorescence silicon nano of hypochlorite, it is characterized in that, step comprises:
A, by soluble in water for a certain amount of trisodium citrate, be made into 10mL solution, in nitrogen protection and under oxygen free condition, the aminopropyl trimethoxysilane of relative trisodium citrate material amount 6 ~ 15 times (being preferably 8 ~ 9 times) is expelled in above-mentioned solution, stirring at normal temperature 10 minutes, in hydrothermal reaction kettle, react 4 ~ 8 hours at 160 DEG C;
B, select the bag filter of suitable molecular cut off, the solution be obtained by reacting by step a is dialysed 3 ~ 5 times in water, remove unreacted aminopropyl trimethoxysilane and trisodium citrate, reacting coarse product is through dialysis, concentrated, precipitation, dry thus obtained one has ClO
-the Fluorescent silicon nanoparticle of recognition function.
4. the preparation method of the water soluble fluorescence silicon nano for detecting hypochlorite according to claim 3, is characterized in that, as optimization, in step a, the concentration of described citric acid three sodium solution is 20 ~ 80mg/ml, is preferably 30 ~ 50mg/ml.
5. the preparation method of the water soluble fluorescence silicon nano for detecting hypochlorite according to claim 3, is characterized in that, in step a, the material amount proportioning of described trisodium citrate thing and aminopropyl trimethoxysilane is 1:8 ~ 9.
6. the preparation method of the water soluble fluorescence silicon nano for detecting hypochlorite according to claim 3, is characterized in that, in step b, the molecular cut off of bag filter is 500.
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| CN108410449A (en) * | 2018-01-31 | 2018-08-17 | 兰州大学 | A kind of preparation and its application of the water soluble fluorescence nano silicon particles of detection of alkaline phosphatase |
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