CN105548153A - Gold nanoparticle-containing glucose visual detection sensor and its preparation method and use - Google Patents
Gold nanoparticle-containing glucose visual detection sensor and its preparation method and use Download PDFInfo
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Abstract
The invention discloses a gold nanoparticle-containing glucose visual detection sensor and its preparation method and use. The preparation method comprises that 1, chloroauric acid and trisodium citrate undergo a contact reaction in a solvent to produce a colloidal gold solution, and 2, pH of the colloidal gold solution is adjusted to 6.0-7.5 and 3-aminophenylboronic acid (APBA) and amino-terminated poly(N-isopropylacrylamide) (PNIPAM-NH2) are added into the colloidal gold solution for electrostatic interaction so that the gold nanoparticle-containing glucose visual detection sensor is obtained. The sensor has good sensitivity, selectivity and ion interference resistance in the glucose detection. The preparation method can be operated simply and easily and the detection result can be read through naked eyes.
Description
Technical field
The present invention relates to visible sensor, particularly, relate to a kind of golden nanometer particle Visual retrieval glucose sensor and its preparation method and application.
Background technology
Gold size solution and solution of gold nanoparticles (AuNPs).Golden nanometer particle has very high extinction coefficient, and wherein, the extinction coefficient of 13nm golden nanometer particle is up to 2.7 × 10
8mol/ (Lcm), higher than general dye molecule more than 1000 times, according to Beer-Lambert law, the detectability that golden nanometer particle can reach is far below dye molecule.On the other hand, because golden nanometer particle system has different color changes under different conditions, therefore occupy an important position in Visual retrieval.Visual retrieval mechanism based on golden nanometer particle is: monodisperse gold nanometer particle presents redness in the solution, when adding detected material, golden nanometer particle is assembled, thus interparticle plasmon coupling is changed, absorption peak generation red shift, the color of solution becomes purple or blueness from redness.
Golden nanometer particle is except having above-mentioned optical characteristics, its surface is easy to carry out chemical modification also for the widespread use of golden nanometer particle in analysis detects provides convenient condition, such as golden nanometer particle surface by modifying the specific detection of the realizations such as Small molecular, protein, polypeptide, DNA to different target substance, can comprise Small molecular, heavy metal ion, protein, nucleic acid, tumour cell and pathogen etc.Visible detection method based on golden nanometer particle does not rely on any large-scale instrument, namely solution colour change can be used as read output signal, signal detects speed, material requested cost is comparatively cheap, is particularly useful for there is quick detection, Site Detection needs condition for peace relatively to fall behind not possess the region of large-scale instrument.
Glucose is the widest and of paramount importance a kind of monose of distributed in nature, and containing five hydroxyls in its structure, an aldehyde radical, has the character of polynary alcohols and aldehydes.Glucose is ubiquitous Power supply thing in the most basic material of biosome and bioprocess, but much research shows, renal glucosuria, cystic fibrosis, diabetes etc. all carry obstacle relevant with glucose.Therefore the quick and precisely detection of glucose is very important.There are many methods based on golden nanometer particle Visual retrieval glucose at present.As document " RadhakumaryC; SreenivasanK.Nakedeyedetectionofglucoseinurineusinggluco seoxidaseimmobilizedgoldnanoparticles [J] .Analyticalchemistry; 2011; 83 (7): 2829-2833. " is reported: adopt carbodiimides, glucose oxidase is modified at the surface of golden nanometer particle, add glucose, golden nanometer particle is assembled, when the content of glucose is greater than 100mg/L, the color of solution of gold nanoparticles becomes blueness.Also such as " JiangY; ZhaoH; LinY; etal.Colorimetricdetectionofglucoseinratbrainusinggoldna noparticles [J] .AngewandteChemie; 2010; 122 (28): 4910-4914. " reports: the optical property and the cascade reaction that utilize golden nanometer particle, can build the method for glucose in a kind of fast and convenient Visual retrieval cerebrospinal fluid.Utilize boric acid and adjacent hydroxyl compound that covalently bound characteristic can occur, the sensor that boric acid and derivant thereof are used for detecting glucose as recognition component is had certain Research foundation.Again such as " BiX; LiuZ.Facilepreparationofglycoprotein-imprinted96-wellmic roplatesforenzyme-linkedimmunosorbentassaybyboronateaffi nity-basedorientedsurfaceimprinting [J] .Analyticalchemistry; 2013; 86 (1): 959-966. " reports: utilize 4-aminobenzene boric acid modified Graphene, increase the detection signal to monosaccharide material, Be very effective.Also such as " Ma; YandYang; X; Onesaccharidesensorbasedonthecomplexoftheboronicacidandt hemonosaccharideusingelectrochemicalimpedancespectroscop y [J] .JournalofElectroanalyticalChemistry; 2005; 580:348-352. " reports: in acid condition, 3-aminobenzene boric acid (APBA) voltolisation with higher electron transmission efficiency is incorporated into gold electrode surfaces, obtains poly-aminobenzene boric acid (PABA) film.PABA film can the different monose of covalent bond, the kind of sugar and the different initiation film dielectric property change in various degree of concentration.In conjunction with AC impedance (EIS) identifiable design glucose, fructose, mannitol, D-sorbite four kinds of monose, and have good linear relationship, highly sensitive, the range of linearity is wider.Last such as " LiYP, JiangL, ZhangT, etal.Colorimetricdetectionofglucoseusingaboronicacidderi vativereceptorattachedtounmodifiedAuNPs [J] .ChineseChemicalLetters, 2014, 25 (1): 77-79. " report: the visual sensing of golden nanometer particle is combined with the affinity interaction of boric acid, realize the high selectivity to glucose, rapid sensitive detects also has relevant report, merely boronic acid derivatives is modified naked golden nanometer particle surface, prepare a kind of colorimetric sensing, under acidity and alkali condition, glucose is quantitatively detected respectively.
In above-mentioned detection method, or utilize boric acid and adjacent hydroxyl compound that covalently bound characteristic can occur, boric acid and derivant thereof are used for as recognition component the sensor detecting glucose.Be to improve detection sensitivity further, the combination of golden nanometer particle and boric acid and adjacent hydroxyl compound is detected glucose.But due to golden nanometer particle be nanometer materials, be inevitably faced with the problem of reunion, during the too high salt solusion of the ion concentration especially existed in testing environment, agglomeration is obvious, severe jamming testing result.
Summary of the invention
The object of this invention is to provide a kind of golden nanometer particle Visual retrieval glucose sensor and its preparation method and application, the detection of this sensor to glucose has good sensitivity, selectivity and anti-ion interference ability, and preparation method is simple to operation simultaneously, testing result bore hole is readable.
To achieve these goals, the invention provides a kind of preparation method of golden nanometer particle Visual retrieval glucose sensor, it is characterized in that, comprise
1) gold chloride and trisodium citrate are carried out contact reaction in solvent and obtain gold size solution;
2) pH of gold size solution is adjusted to 6.0-7.5, then adds 3-aminobenzene boric acid (APBA) and amino-terminated poly-N-isopropyl acrylamide (PNIPAM-NH
2) carry out electrostatic interaction with obtained golden nanometer particle Visual retrieval glucose sensor.
Present invention also offers a kind of golden nanometer particle Visual retrieval glucose sensor, this sensor is obtained by the preparation of above-mentioned method.
Invention further provides the application of a kind of above-mentioned golden nanometer particle Visual retrieval glucose sensor in glucose detects.
Pass through technique scheme, the present invention adopts reduction of sodium citrate method directly to synthesize the gold size solution of domain size distribution at about 13nm, golden nanometer particle surface distributed prepared by the method excessive citrate ion, electronegative, its effect offsets the Van der Waals force between golden nanometer particle by electrostatic repulsion on the one hand, thus guaranty money's nanoparticle dispersion evenly, is not easily reunited; On the other hand, being can with amino-terminated poly-N-isopropyl acrylamide (PNIPAM-NH
2) and 3-aminobenzene boric acid (APBA) in amino group generation electrostatic interaction, thus make two kinds of compounds successfully modify golden nanometer particle surface.Wherein, the effect of 3-aminobenzene boric acid is the recognition component as sensor, utilizes its boric acid base group to go selective binding to contain the glucose of adjacent oh group, realizes detecting highly sensitive, the high selectivity of glucose.Amino-terminated poly-N-isopropyl acrylamide is a kind of chain-like macromolecule compound, at 25 DEG C, it presents a kind of extended position, solution is made to keep water wettability, even if golden nanometer particle also can be stablized do not reunite in the salt solusion that ion concentration is higher, improve the anti-ion interference ability of this sensor, for the detection of this sensor in complex environment provides possibility.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Fig. 1 is the ultraviolet spectrogram that in test example 1, sensors A 1 detects different glucose;
Fig. 2 is the optical picture of the selective enumeration method of sensors A 1 couple of Glu, Lcy, Gly, His, AA, DA and UA in test example 2;
Fig. 3 is sensors A 1 couple of K in test example 2
+, Na
+, Cl
-and Ca
2+the optical picture that detects of anti-ion interference;
Fig. 4 is the optical picture that in test example 2, the anti-ion interference of sensor B1 to K+, Na+, Cl-and Ca2+ detects;
Fig. 5 is the optical picture that in test example 1, sensors A 1 detects different glucose.
Embodiment
The invention provides a kind of preparation method of golden nanometer particle Visual retrieval glucose sensor, it is characterized in that, comprise
1) gold chloride and trisodium citrate are carried out contact reaction in solvent and obtain gold size solution;
2) pH of gold size solution is adjusted to 6.0-7.5, then adds 3-aminobenzene boric acid (APBA) and amino-terminated poly-N-isopropyl acrylamide (PNIPAM-NH
2) carry out electrostatic interaction with obtained golden nanometer particle Visual retrieval glucose sensor.
In step 1 of the present invention) in, the concrete kind of solvent can be selected in wide scope, but taking cost into account, preferably, solvent is deionized water.
In step 1 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to improve the productive rate of golden nanometer particle, preferably, relative to the water of 100 weight portions, the consumption of gold chloride is 0.015-0.02 weight portion, and the consumption of trisodium citrate is 0.25-0.3 weight portion.
In step 1 of the present invention) in, catalytic condition can be selected in wide scope, but in order to improve the productive rate of golden nanometer particle, preferably, contact reaction at least meets the following conditions: temperature of reaction 98-105 DEG C, and the reaction time is 20-40min.
In step 2 of the present invention) in, the consumption of each material can be selected in wide scope, but in order to improve PNIPAM-NH
2, APBA and golden nanometer particle the quantity of combination, preferably, in step 2) in, relative to the gold size solution of 1mL, the consumption of APBA is 1.5 × 10
-4-2.5 × 10
-4mmol, PNIPAM-NH
2consumption be 3.5 × 10
-5-4.5 × 10
-5mmol.
In step 2 of the present invention) in, the concrete steps of electrostatic interaction and condition can be selected in wide scope, but in order to improve PNIPAM-NH
2, APBA and golden nanometer particle the quantity of combination, preferably, electrostatic interaction is by first by gold size solution, APBA and PNIPAM-NH
2mixing, then leaves standstill; Wherein leave standstill and at least meet the following conditions: dwell temperature is 15-30 DEG C, and time of repose is 10-20min.
In step 2 of the present invention) in, the method of the adjustment of pH can be the control method of any one routine in this area, but in order to improve the efficiency of adjustment, preferably, in step 2) in, pH is adjusted to: first by gold size solution dilution to the 40%-60% of original content, then regulate pH by sodium hydroxide solution.
Present invention also offers a kind of golden nanometer particle Visual retrieval glucose sensor, this sensor is obtained by the preparation of above-mentioned method.
Invention further provides the application of a kind of above-mentioned golden nanometer particle Visual retrieval glucose sensor in glucose detects.
Below will be described the present invention by embodiment.In following examples, three hydration gold chlorides are Aladdin companies market product, trisodium citrate is the commercially available product of traditional Chinese medicines group, 3-aminobenzene boric acid is the commercially available product of Shanghai uncle's card chemistry, and amino-terminated poly-N-isopropyl acrylamide is the number-average molecular weight of Sigma-Aldrich is the commercially available product of 2500.
Embodiment 1
1) method recorded according to " FrensG.Controllednucleationfortheregulationoftheparticle sizeinmonodispersegoldsuspensions [J] .Nature; 1973,241 (105): 20-22. " carries out the preparation of gold size solution: first by glass apparatus chloroazotic acid (HCl:HNO
3=3:1, volume ratio) clean removal of impurities, then use deionized water drip washing clean, naturally dry stand-by; Then by 5mLHAuCl
4(0.01mol/L) join in 100mL deionized water, magnetic agitation is even; Then gained solution is heated to reflux (100 DEG C), then the citric acid three sodium solution (1 % by weight) of 5mL is joined in above-mentioned solution fast.The color observing solution finally becomes claret from the colourless purple that becomes within a few minutes, continue heating 30min, namely obtain the gold size solution that homogeneous citric acid is firm, remove heating arrangement, at 25 DEG C cool, close be stored in the refrigerator of 4 DEG C stand-by.
2) at 25 DEG C, the gold size solution of taking 0.5mL adds deionized water and is diluted to 1mL, then adds NaOH solution (0.05mol/L) and regulate pH to 7.0; Then the PNIPAM-NH of 10 μ L is added
2the APBA solution (1mmol/L) of solution (10mmol/L) and 20 μ L mixes to above-mentioned gold size solution, leaves standstill 15min with obtained golden nanometer particle Visual retrieval glucose sensor A1.
Embodiment 2
Carry out obtained sensors A 2 according to the method for embodiment 1, difference is: step 2) in pH be adjusted to 6.0.
Embodiment 3
Carry out obtained sensors A 3 according to the method for embodiment 1, difference is: step 2) in pH be adjusted to 7.5.
Embodiment 4
Carry out obtained sensors A 4 according to the method for embodiment 1, difference is: step 2) middle PNIPAM-NH
2the consumption of solution (10mmol/L) is 12.5 μ L.
Embodiment 5
Carry out obtained sensors A 5 according to the method for embodiment 1, difference is: step 2) middle PNIPAM-NH
2the consumption of solution (10mmol/L) is 7.5 μ L.
Embodiment 6
Carry out obtained sensors A 6 according to the method for embodiment 1, difference is: step 2) in the consumption of APBA solution (1mmol/L) be 22.5 μ L.
Embodiment 7
Carry out obtained sensors A 7 according to the method for embodiment 1, difference is: step 2) in the consumption of APBA solution (1mmol/L) be 17.5 μ L.
Comparative example 1
Carry out obtained sensor B1 according to the method for embodiment 1, difference is: step 2) in do not use PNIPAM-NH
2solution.
Test example 1
At pH=7.0, under the condition of T=25 DEG C, the glucose solution (0.25mM-3mM) of variable concentrations is added in sensors A 1, then UV-vis, optical photograph is passed through (see Fig. 5, wherein, a-g represents that the glucose solution of the glucose solution of the glucose solution of the glucose solution of the glucose solution of 0.25mM, 0.75mM, 1mM, 1.5mM, the glucose solution of 2mM, the glucose solution of 2.5mM and 3mM is added to optical effect figure in sensors A 1 successively) characterize, the relation between gold size reunion degree and glucide concentration.
According to the ratio (A of the absorbance of characteristic peak respectively at 520nm and 610nm place of golden nanometer particle
520/ A
610) quantitatively can detect glucose, set up A
520/ A
610and the linear relationship between the concentration of glucose is the foundation of qualitative detection.As shown in Figure 1, wherein, interior list of illustrations shows that this sensor detects the calibration curve of glucose, and the sensing range of glucose is 0.25-3mM, linear equation: Y (A
520/ A
610)=7.52-2.08c
glu(mmol/L).It can thus be appreciated that golden nanometer particle Visual retrieval glucose sensor provided by the invention quantitatively can detect efficiently to glucose solution.
Similarly, also quantitatively can be detected efficiently glucose solution by the known A2-A7 of above-mentioned method.And B1 (as shown in Figure 3) is owing to cannot resist ion interference, gold size solution is easily reunited, and quantitatively cannot detect glucose.
Test example 2
1) Glu (glucose) of 3mM is added to the red sensors A of display 1 (see in Fig. 2 a), the color observing sensors A 1 becomes blue (b see in Fig. 2), by Lcy (Cys) solution of 3mM, Gly (glycocoll) solution of 3mM, His (histidine) solution of 3mM, AA (ascorbic acid) solution of 3mM, DA (dopamine) solution of 30 μMs and UA (uric acid) solution of 30 μMs add in sensors A 1 respectively, concrete outcome is shown in Fig. 2, c wherein in Fig. 2 refers to Lcy and is added to design sketch in sensors A 1, d refers to Gly and is added to design sketch in sensors A 1, e refers to His and is added to design sketch in sensors A 1, f refers to AA and is added to design sketch in sensors A 1, g refers to DA and is added to design sketch in sensors A 1, h refers to UA and is added to design sketch in sensors A 1, from result, have almost no change relative to the color of solution in sensors A 1, c-e, g-h, and after adding AA, solution colour has had slight intensification, and this may be because the concentration of one side AA is comparatively large, may be on the other hand because AA is also adjacent hydroxyl compound.It can thus be appreciated that sensors A 1 has excellent selectivity for Glu.Similarly, A2-A7 also has excellent selectivity.
2) due to the energy supply material that glucose is important in biosome, therefore, may be subject to the interference of common ion in biosome in actual testing process, in order to verify the anti-ion interference ability of this sensor, ion K common in human body is selected in this experiment
+, Na
+, Cl
-, Ca
2+, result as shown in Figure 3, represents the K adding 5mM in four sensors A prepared 1 successively respectively to a, b, c, d
+solution, the Na of 100mM
+solution, the Cl of 100mM
-solution, the Ca of 2mM
2+solution, solution still keeps red, does not have agglomeration to produce, and this is owing to can effectively hinder ion for the impact of gold size containing PNIPAM macromolecular chain in this sensor.Similarly, the testing result of A2-A7 and A1 is consistent.
3) e, f, g, h of Fig. 4 represent the K adding 5mM in Xiang Si the sensor B1 prepared
+solution, the Na of 100mM
+solution, the Cl of 100mM
-solution, the Ca of 2mM
2+solution, observes obvious agglomeration.This demonstrates sensor provided by the invention further from the negative and not only has good selectivity, also has good anti-ion interference ability.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out combination in any between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (9)
1. a preparation method for golden nanometer particle Visual retrieval glucose sensor, is characterized in that, comprises
1) gold chloride and trisodium citrate are carried out contact reaction in solvent and obtain gold size solution;
2) pH of described gold size solution is adjusted to 6.0-7.5, then adds 3-aminobenzene boric acid (APBA) and amino-terminated poly-N-isopropyl acrylamide (PNIPAM-NH
2) carry out electrostatic interaction with obtained described golden nanometer particle Visual retrieval glucose sensor.
2. preparation method according to claim 1, wherein, described solvent is water.
3. preparation method according to claim 2, wherein, relative to the water of 100 weight portions, the consumption of described gold chloride is 0.015-0.02 weight portion, and the consumption of described trisodium citrate is 0.25-0.3 weight portion.
4. preparation method according to claim 3, wherein, described contact reaction at least meets the following conditions: temperature of reaction is 98-105 DEG C, and the reaction time is 20-40min.
5. according to the preparation method in claim 1-4 described in any one, wherein, in step 2) in, relative to the described gold size solution of 1mL, the consumption of described APBA is 1.5 × 10
-4-2.5 × 10
-4mmol, described PNIPAM-NH
2consumption be 3.5 × 10
-5-4.5 × 10
-5mmol.
6. preparation method according to claim 5, wherein, described electrostatic interaction is by first by described gold size solution, APBA and PNIPAM-NH
2mixing, then leaves standstill; Wherein said leaving standstill at least meets the following conditions: dwell temperature is 15-30 DEG C, and time of repose is 10-20min.
7. preparation method according to claim 5, wherein, in step 2) in, pH is adjusted to: first by described gold size solution dilution to the 40%-60% of original content, then regulate pH by sodium hydroxide solution.
8. a golden nanometer particle Visual retrieval glucose sensor, is characterized in that, described sensor is obtained by the method preparation in claim 1-7 described in any one.
9. the application of golden nanometer particle Visual retrieval glucose sensor according to claim 8 in glucose detects.
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| CN109765279A (en) * | 2019-01-14 | 2019-05-17 | 安徽师范大学 | Sandwich style electrochemical sensor and its preparation method and application based on the affine building of boric acid |
| CN109765279B (en) * | 2019-01-14 | 2020-12-01 | 安徽师范大学 | Sandwich type electrochemical sensor constructed based on boric acid affinity and preparation method and application thereof |
| CN110672544A (en) * | 2019-10-12 | 2020-01-10 | 天津科技大学 | Glucose visualization sensor based on cyclic peptide recognition element and preparation method and application thereof |
| CN111375355A (en) * | 2019-12-17 | 2020-07-07 | 中科康磁医疗科技（苏州）有限公司 | Boric acid hydrogel synthesis method for continuous monitoring of saliva glucose |
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