CN104165874A - Quantum dot fluorescent aspirin imprinted sensor and its preparation method and use - Google Patents

Quantum dot fluorescent aspirin imprinted sensor and its preparation method and use Download PDF

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CN104165874A
CN104165874A CN201410354544.8A CN201410354544A CN104165874A CN 104165874 A CN104165874 A CN 104165874A CN 201410354544 A CN201410354544 A CN 201410354544A CN 104165874 A CN104165874 A CN 104165874A
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aspirin
quantum dot
fluorescence
preparation
solution
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卫潇
戴江栋
李洪吉
高林
王吉祥
于志新
周志平
闫永胜
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Jiangsu University
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Abstract

The invention provides a quantum dot fluorescent aspirin imprinted sensor and its preparation method and use and belongs to the technical field of material preparation and drug content detection. The preparation method comprises the following steps of preparing a precursor NaHTe solution from sodium borohydride, tellurium powder and water in an ultrasonic environment, injecting the precursor NaHTe solution into a CdCl2.2.5H2O solution fed with nitrogen for oxygen removal, having a pH value of 10.5-11.5 and containing thioglycollic acid (TGA), carrying out backflow reaction processes in a nitrogen protective atmosphere at a temperature of 100-110 DEG C to obtain quantum dots having different sizes according to different backflow time periods, and synthesizing a fluorescent molecule imprinted polymer from the CdTe quantum dots as fluorescent carriers, aspirin as a template molecule, (3-aminopropyl)triethoxysilane (APTES) as a functional monomer and tetraethyl orthosilicate (TEOS) as a cross-linking agent by a sol-gel method, wherein the fluorescent molecule imprinted polymer can be used for optical detection of aspirin. The fluorescent molecule imprinted polymer has good optical and pH stability and has an aspirin selective-identification function.

Description

A kind of quantum dot fluorescence aspirin trace sensor and its preparation method and application
Technical field
The present invention relates to a kind of quantum dot fluorescence aspirin trace sensor and its preparation method and application, belong to material preparation and medicament contg detection technique field.
Background technology
Aspirin (aspirin), is also acetylsalicylic acid (acetylsalicylic acid), is that a class is applied the earliest, the widest and prevailing analgesic-antipyretic antirheumatic drug.There is many-sided pharmacological actions such as antipyretic, analgesia, anti-inflammatory, antirheumatic and platelet aggregation-against, be usually used in cold, fever, headache, neuralgia arthralgia, courbature, rheumatic fever, acute interior wet arthritis, rheumatoid arthritis and toothache etc.There is performance drug effect rapid, efficacy stability, overdose is easy to the features such as diagnosis and processing.But along with the widespread use of aspirin, its bad reaction also increases gradually, that more common symptom has is nauseating, vomiting, epigastric discomfort or pain etc., so most important to the monitoring of aspirin consumption.At present, the assay method of aspirin content mainly uses chromatography, but chromatography has certain limitation, as large in solvent-oil ratio, time-consuming, loaded down with trivial details sample pretreatment and poor selectivity etc.Therefore,, for being widely used of aspirin, setting up simple, quick, sensitive detection method is to carry out the task of top priority that aspirin content is measured.
Along with analyzing improving constantly of requiring, particularly Pharmaceutical Analysis, environmental analysis, food analysis and product detect the growing of demand, and sensor, as important detection means, more and more receives people's concern.Organic have good molecular recognition function with biological sensitive materials, molecularly imprinted polymer material wherein can be for the object customization of " cutting the garment according to the figure ", realize the single-minded identification to target molecule, can compare favourably with natural biological recognition system (enzyme-to-substrate), there is preparation simple, good stability, life-span is long, easily preserve, the feature such as cheap, in Solid-Phase Extraction, chiral separation, simulation biological antibody, catalysis and and synthetic aspect be widely used, to solve environment, biology waits simple and direct that in complex system, specific target molecules high selectivity is identified, reliable means.
Molecular imprinting (Molecular imprinting technology, MIT) be preparation has single-minded recognition capability polymkeric substance process to a certain specific molecular, the polymkeric substance of preparation is called molecularly imprinted polymer (Molecularly imprinted polymers, MIPs).The general formation supramolecular complex that first template molecule and selected function monomer interacted of the preparation process of MIPs, under crosslinking chemical effect, form polymkeric substance again, finally remove after template molecule by certain means, in the MIPs of acquisition, just left binding site template molecule to specific recognition.In recent years, the structure of MIPs effect precordainment, specific recognition and extensive practicality have attracted more and more many scientific workers' interest and favor.
Quantum dot is as optical material, because it has excellent photoelectric properties, larger specific surface area and quantum size effect is in these years used widely in research fields such as biological chemistry, molecular biology, genomics, proteomics, bio-molecular interactions.In these researchs, quantum dot fluorescence probe and imaging in vivo thereof are one of emphasis of research at present.Quantum dot is compared with traditional organic fluorescence element, there is good photostability, compared with large Stokes shift and a series of features such as fluorescence spectrum is narrow and symmetrical, and there is fluorescent characteristic, be expected to develop into the novel light-emitting biomarker material with development prospect of a class.
Through the literature search of prior art is found, " the Selective Recognition of 2 that Pan Jianming etc. deliver for 2011 on " The Journal of Physical Chemistry C " (physical chemistry C), 4, 6-TriehloroPhenol by Molecularly Imprinted Polymers Based on Magnetic Halloysite Composites " (the surface imprinted selectivity identification 2 of halloysite nanotubes magnetic composite, 4, 6-trichlorophenol), this article has successfully been prepared magnetic molecularly imprinted compound substance for Selective Separation 2, 4, 6-trichlorophenol, there is good selectivity." measuring the new method research of niacin norfloxacin based on CdTe quantum dot " that Wei Hong etc. deliver for 2011 on " chemical journal ", this article has successfully utilized detection that the fluorescence property of CdTe quantum dot is simple, quick, sensitive niacin norfloxacin.But the former testing process workload is larger, speed is slow, and sensitivity is lower; Latter lacks certain universality and selectivity.Therefore, high-sensitive fluoroscopic examination is combined with molecular imprinting, utilize fluorescence signal to make up the defect that molecularly imprinted polymer lacks signal conduction, prepare molecular engram fluorescent optical sensor, meet anti-interference, the high selection of sensory device, high-sensitive demand, become the study hotspot in the fields such as current sensing, separation.The preparation of molecular engram fluorescent optical sensor is further expanded range of application and the using method of MIPs in analyzing and testing, and the selectivity of MIPs also makes the sensitivity of compound fluorescence probe and selectivity be significantly improved simultaneously.Utilizing molecular engram fluorescent optical sensor to carry out the research that thereby optical analysis reaches fast, convenience detects residual quantity necessitates.
Summary of the invention
The object of the present invention is to provide a kind of quantum dot fluorescence aspirin trace sensor and its preparation method and application, large to overcome in the process that detects aspirin content in prior art solvent-oil ratio, time-consuming, the loaded down with trivial details defect such as sample pretreatment and poor selectivity.
First sodium borohydride, tellurium powder and water generate presoma NaHTe solution under ultrasound environments.The CdCl that mercaptoacetic acid (TGA) that what the pH that then presoma is injected into letting nitrogen in and deoxidizing was 10.5-11.5 have exists 22.5H 2in O aqueous solution, at nitrogen protection 100-110 oback flow reaction under C condition, according to the difference of return time, has obtained the quantum dot of different size.Then utilize sol-gel process to synthesize taking CdTe quantum dot as fluorescence carrier, aspirin is template molecule, (3-aminopropyl) triethoxysilane (APTES) is function monomer, the fluorescence molecule imprinted polymer that ethyl orthosilicate (TEOS) is crosslinking chemical, and for optical detection aspirin.The fluorescence molecule imprinted polymer of preparation has good optics and pH stability, and has the ability of selectivity identification aspirin.
the technical solution used in the present invention is:
A kind of quantum dot fluorescence aspirin molecular engram sensor and preparation method thereof, carries out according to following steps:
(1) sodium borohydride (NaBH4) and tellurium powder are joined in centrifuge tube, and then add redistilled water that solid is dissolved completely; Centrifuge tube is positioned over to ultrasonic reaction in ultrasonic machine, and keeps the mouth of pipe to give vent to anger, final white liquid is required presoma NaHTe solution.
(2), under the condition of letting nitrogen in and deoxidizing, the presoma NaHTe solution that step (1) is obtained is injected into the CdCl that has mercaptoacetic acid (TGA) to exist of letting nitrogen in and deoxidizing 22.5H 2in O aqueous solution, mixed solution is back flow reaction under nitrogen protection condition, according to the difference of return time, obtains the quantum dot of different size.
(3) the quantum dot stoste and the redistilled water that step (2) are obtained are mixed to join in flask, add (3-aminopropyl) triethoxysilane and aspirin simultaneously, stir; Then ethyl orthosilicate and ammoniacal liquor are joined to above-mentioned system reaction; After reaction finishes, water and ethanol washing several times, to remove the complete material of unreacted, product is dried in vacuum drying oven; Primary template molecule aspirin is eluted from products therefrom with eluant, eluent to wash-out three times; Remove after template molecule, obtain quantum dot fluorescence imprinted polymer MIPs-CdTe QDs.
Wherein, the mol ratio of the sodium borohydride described in step (1) and tellurium powder is 2-4:1.
Wherein, the CdCl that has mercaptoacetic acid (TGA) to exist described in step (2) 22.5H 2the pH of O aqueous solution is 10.5-11.5; Wherein, CdCl 22.5H 2the mol ratio of O, TGA and NaHTe is 1:2.0-2.5:0.4-0.6, and wherein the molar weight of NaHTe draws according to the molar weight of tellurium powder in step (1); Described back flow reaction temperature is 100 oc-110 oC.
Wherein, the volume ratio of the quantum dot solution described in step (3) and redistilled water is 0.1-3:100; The ratio of the described aspirin adding and quantum dot solution is 0.1-3 mL:0.025 mmol; The mol ratio of described aspirin, (3-aminopropyl) triethoxysilane, ethyl orthosilicate is 1:2-12:8-24; The volume ratio of ammoniacal liquor and ethyl orthosilicate is 1:1-2; Eluant, eluent used is water and ethanol (V/V 1:1), wash-out three times; Described mixing time is 20-30 min; It is described that ethyl orthosilicate and ammoniacal liquor are joined to the above-mentioned system reaction time is 10-14 hour.
Synthesizing except not containing template molecule of non-molecularly imprinted polymer (NIPs-CdTe QDs), other processes are identical with trace process.
Technological merit of the present invention: using CdTe as fluorescent functional material, utilize sol-gel process method to synthesize fluorescence molecule imprinted polymer; Utilize the fluorescence molecule imprinted polymer that the present invention obtains to there is good optical stability, can realize the ability of identification fast and optical detection aspirin.The preparation of molecular engram fluorescent optical sensor is further expanded range of application and the using method of MIPs in analyzing and testing, and the selectivity of MIPs also makes the sensitivity of compound fluorescence probe and selectivity be significantly improved simultaneously.For the research of expanding the field that Environmental Analytical Chemistry and environmental pollution chemistry and environmental pollution control chemistry are new provides science reliable foundation.For be further engaged in correlation theory research and practical application as: on-the-spot, fast, selectivity identification analyzes and measures water body with visual detection, the trace/ultratrace objectionable impurities in food and biosome is established solid theory and practice basis.
Brief description of the drawings
Fig. 1: parameter is 0.1 mL quantum dot stoste, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and the disposable transmission electron microscope picture that adds CdTe quantum dot fluorescence molecularly imprinted polymer synthetic under condition of ethyl orthosilicate.
Fig. 2: parameter is 0.1 mL quantum dot stoste, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate divides 5 times and adds, the transmission electron microscope picture of synthetic CdTe quantum dot fluorescence molecularly imprinted polymer under 10 minutes conditions of every minor tick.
Fig. 3: parameter is 2.0 mL quantum dot stostes, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and the disposable transmission electron microscope picture that adds CdTe quantum dot fluorescence molecularly imprinted polymer synthetic under condition of ethyl orthosilicate.
Fig. 4: parameter is 2.0 mL quantum dot stostes, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate divides 5 times and adds, the transmission electron microscope picture of synthetic CdTe quantum dot fluorescence molecularly imprinted polymer under 10 minutes conditions of every minor tick.
Fig. 5: the impact of pH value on quantum dot fluorescence molecularly imprinted polymer fluorescence intensity.
Fig. 6: the time stability of quantum dot fluorescence molecularly imprinted polymer fluorescence intensity.
Fig. 7: the reaction time is detected the impact of aspirin on quantum dot fluorescence molecularly imprinted polymer.Can find out that quantum dot fluorescence molecularly imprinted polymer and aspirin effect are basicly stable after 35 minutes.
Fig. 8: the impact of the aspirin of variable concentrations on fluorescence molecule imprinted polymer (left side) and non-imprinted polymer (right side) fluorescence spectrum.
Fig. 9: the relative intensity linear graph after the aspirin of variable concentrations and fluorescence molecule imprinted polymer (left side) and non-imprinted polymer (right side) effect.
Figure 10: (50 μ mol/L) different antibiotic medicines relative intensity of fluorescence to fluorescence molecule imprinted polymer and non-imprinted polymer under same concentration, in figure, A is that aspirin, B are that erythromycin, C are that Norfloxacin and D are Ciprofloxacin.
Embodiment
Below in conjunction with concrete embodiment, the present invention will be further described.
embodiment 1:
(1) by 30.3 mg sodium borohydride (NaBH 4) and 51.04 mg tellurium powder join in centrifuge tube, and then add 3.0 mL redistilled waters that solid is dissolved completely; Centrifuge tube is positioned over to ultrasonic reaction in ultrasonic machine, and keeps the mouth of pipe to give vent to anger, final white liquid is required presoma NaHTe solution.
(2) CdCl that has mercaptoacetic acid (TGA) to exist that the presoma NaHTe just having obtained to be injected into the pH of letting nitrogen in and deoxidizing be 10.5 2in aqueous solution, wherein add the CdCl of 228.34 mg 22.5H 2the TGA of O and 138.5 μ L.Mixed solution is in nitrogen protection 100 ounder C condition, back flow reaction 60 hours, obtains red fluorescence quantum dot.
(3) 3 mL quantum dot stostes and 10 mL redistilled waters are mixed to join in flask, add 11.7 μ L (3-aminopropyl) triethoxysilane and 4.5 mg aspirin simultaneously, stir 20 min.Then 44.8 μ L ethyl orthosilicates and 44.8 μ L ammoniacal liquor are joined to above-mentioned system, react 10 hours.After reaction finishes, water and ethanol washing several times, to remove the complete material of unreacted, product is dried in vacuum drying oven.Primary template molecule aspirin is eluted from products therefrom with eluant, eluent to wash-out three times; Remove after template molecule, obtain quantum dot fluorescence imprinted polymer MIPs-CdTe QDs.
Synthesizing except not containing template molecule of non-molecularly imprinted polymer (NIPs-CdTe QDs), other processes are identical with trace process.
embodiment 2:
(1) 60.6 mg sodium borohydride (NaBH 4) and 51.04 mg tellurium powder join in centrifuge tube, and then add 3.0 mL redistilled waters that solid is dissolved completely; Centrifuge tube is positioned over to ultrasonic reaction in ultrasonic machine, and keeps the mouth of pipe to give vent to anger, final white liquid is required presoma NaHTe solution.
(2) CdCl that has mercaptoacetic acid (TGA) to exist that the presoma NaHTe just having obtained to be injected into the pH of letting nitrogen in and deoxidizing be 11.5 2in aqueous solution, wherein add the CdCl of 152.23 mg 22.5H 2the TGA of O and 115.44 μ L.Mixed solution is in nitrogen protection 110 ounder C condition, back flow reaction 60 hours, obtains red fluorescence quantum dot.
(3) 0.1 mL quantum dot stoste and 10 mL redistilled waters are mixed to join in flask, add 70.2 μ L (3-aminopropyl) triethoxysilane and 4.5 mg aspirin simultaneously, stir 30 min.Then 134.4 μ L ethyl orthosilicates and 268.8 μ L ammoniacal liquor are joined to above-mentioned system, react 14 hours.After reaction finishes, water and ethanol washing several times, to remove the complete material of unreacted, product is dried in vacuum drying oven.Primary template molecule aspirin is eluted from products therefrom with eluant, eluent to wash-out three times; Remove after template molecule, obtain quantum dot fluorescence imprinted polymer MIPs-CdTe QDs.
Synthesizing except not containing template molecule of non-molecularly imprinted polymer (NIPs-CdTe QDs), other processes are identical with trace process.
embodiment 3:
(1) by 45.4 mg sodium borohydride (NaBH 4) and 51.04 mg tellurium powder join in centrifuge tube, and then add 3.0 mL redistilled waters that solid is dissolved completely; Centrifuge tube is positioned over to ultrasonic reaction in ultrasonic machine, and keeps the mouth of pipe to give vent to anger, final white liquid is required presoma NaHTe solution.
(2) CdCl that has mercaptoacetic acid (TGA) to exist that the presoma NaHTe just having obtained to be injected into the pH of letting nitrogen in and deoxidizing be 11.2 2in aqueous solution, wherein add the CdCl of 182.672 mg 22.5H 2the TGA of O and 133 μ L.Mixed solution is in nitrogen protection 105 ounder C condition, back flow reaction 60 hours, obtains red fluorescence quantum dot.
(3) 2 mL quantum dot stostes and 10 mL redistilled waters are mixed to join in flask, add 23.4 μ L (3-aminopropyl) triethoxysilane and 4.5 mg aspirin simultaneously, stir 25 min.Then 112 μ L ethyl orthosilicates and 168 μ L ammoniacal liquor are joined to above-mentioned system, react 12 hours.After reaction finishes, water and ethanol washing several times, to remove the complete material of unreacted, product is dried in vacuum drying oven.Primary template molecule aspirin is eluted from products therefrom with eluant, eluent to wash-out three times; Remove after template molecule, obtain quantum dot fluorescence imprinted polymer MIPs-CdTe QDs.
Synthesizing except not containing template molecule of non-molecularly imprinted polymer (NIPs-CdTe QDs), other processes are identical with trace process.
Fig. 1-Fig. 4 is the transmission electron microscope picture of the synthetic CdTe quantum dot fluorescence molecularly imprinted polymer of different parameters.Corresponding parameter is followed successively by: Fig. 1: 0.1 mL quantum dot stoste, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate is disposable adds; Fig. 2: 0.1 mL quantum dot stoste, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate divides 5 times to add, every minor tick 10 minutes; Fig. 3: 2.0 mL quantum dot stostes, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate is disposable adds; Fig. 4: 2.0 mL quantum dot stostes, 20 μ L (3-aminopropyl) triethoxysilane, 100 μ L ethyl orthosilicates, and ethyl orthosilicate divides 5 times to add, every minor tick 10 minutes.
In the specific embodiment of the invention, identification and optical detection performance evaluation are carried out by the following method: the object solution of the aqueous solution of appropriate quantum dot fluorescence polymkeric substance and a series of concentration known is joined in 5 mL color comparison tubes, leave standstill 35 minutes (as shown in Figure 7) under room temperature after vibration.Detect the fluorescence intensity of solution by molecular fluorescence photometer measurement system.According to Stern-Volmer equation ( f 0 / F=1+K sv [c]) taking concentration [c] as horizontal ordinate, relative intensity of fluorescence ( f 0 / F)for ordinate is drawn fluorescence response curve.Select several antibiotic medicines, material as a comparison, participates in the research of MIPs-CdTe QDs recognition performance.
Test example 1: first investigated pH value on the impact of fluorescence intensity (as shown in Figure 5, prepared fluorescence molecule imprinted polymer is that within the scope of 6.0-9.0, fluorescence intensity keeps stable at pH) and the fluorescence time stability (as shown in Figure 6, prepared fluorescence molecule imprinted polymer has good stability) of resulting polymers.Finally select the solution of the pH=7.0 less on fluorescence intensity impact to do fluorometric investigation experiment.Fluorescence molecule imprinted material is configured to the aqueous solution of 100 mg/L, antibiotics object is configured as the aqueous solution of 1 mmol/L.Get the polymer solution of 175 μ L and the aqueous solution of 0-0.25 mL aspirin joins in 5 mL color comparison tubes, regulating pH value is 7.0 water constant volumes also, leaving standstill 35 minutes after the vibration of test fluid room temperature, then detect the fluorescence intensity of solution with fluorospectrophotometer.According to Stern-Volmer equation ( f 0 / F=1+K sv [c]) taking concentration [c] as horizontal ordinate, relative intensity of fluorescence ( f 0 / F)for ordinate is drawn fluorescence response curve.As shown in Figure 8, along with the rising of aspirin concentration, fluorescence intensity weakens, according to Stern-Volmer equation ( f 0 / F=1+K sv [c]) taking concentration [c] as horizontal ordinate, relative intensity of fluorescence ( f 0 / F)draw fluorescence response curve for ordinate, obtain respectively related coefficient and be 0.9925 and 0.9927 straight line (as shown in Figure 9).Result shows, quantum dot fluorescence molecularly imprinted polymer has the ability of good optical detection aspirin.
Test example 2: the aqueous solution that fluorescence molecule imprinted material is configured to 100 mg/L, select aspirin (A), erythromycin (B), Norfloxacin (C) and four kinds of objects of Ciprofloxacin (D), above several antibiotic medicines are configured as to the aqueous solution of 1 mmol/L.Get the aqueous solutions of polymers of 175 μ L and the antibiotics aqueous solution of 250 μ L joins in 5 mL color comparison tubes, regulating pH value is 7.0 water constant volumes also, leaving standstill 35 minutes after the vibration of test fluid room temperature, then detect the fluorescence intensity of solution with fluorospectrophotometer.As shown in figure 10, as seen from the figure, the quencher amount maximum of aspirin to fluorescence molecule imprinted polymer, illustrates that fluorescence molecule imprinted polymer has specific recognition capability to template molecule aspirin.Result shows, fluorescence molecule imprinted polymer prepared by the present invention has obvious specific recognition ability to aspirin, and quencher effect is higher than other microbiotic.

Claims (6)

1. a quantum dot fluorescence aspirin trace sensor, it is characterized in that, described sensor is taking CdTe quantum dot as fluorescence carrier, aspirin is template molecule, 3-aminopropyl triethoxysilane is function monomer, ethyl orthosilicate is that crosslinking chemical is prepared from, and has the ability of selectivity identification aspirin.
2. quantum dot fluorescence aspirin trace sensor and its preparation method and application, is characterized in that, carries out according to following step:
(1) sodium borohydride and tellurium powder are joined in centrifuge tube, and then add redistilled water that solid is dissolved completely; Centrifuge tube is positioned over to ultrasonic reaction in ultrasonic machine, and keeps the mouth of pipe to give vent to anger, final white liquid is required presoma NaHTe solution;
(2), under the condition of letting nitrogen in and deoxidizing, the presoma NaHTe solution that step (1) is obtained is injected into the CdCl that has mercaptoacetic acid to exist of letting nitrogen in and deoxidizing 22.5H 2in O aqueous solution, mixed solution is back flow reaction under nitrogen protection condition, according to the difference of return time, obtains the quantum dot of different size;
(3) the quantum dot stoste and the redistilled water that step (2) are obtained are mixed to join in flask, add (3-aminopropyl) triethoxysilane and aspirin simultaneously, stir; Then ethyl orthosilicate and ammoniacal liquor are joined to above-mentioned system reaction; After reaction finishes, water and ethanol washing several times, to remove the complete material of unreacted, product is dried in vacuum drying oven; Primary template molecule aspirin is eluted from products therefrom with eluant, eluent; Remove after template molecule, obtain quantum dot fluorescence imprinted polymer MIPs-CdTe QDs.
3. a kind of quantum dot fluorescence aspirin trace sensor according to claim 2 and its preparation method and application, is characterized in that, the mol ratio of the sodium borohydride described in step (1) and tellurium powder is 2-4:1.
4. a kind of quantum dot fluorescence aspirin trace sensor according to claim 2 and its preparation method and application, is characterized in that, the CdCl that has mercaptoacetic acid to exist described in step (2) 22.5H 2the pH of O aqueous solution is 10.5-11.5; Wherein, CdCl 22.5H 2the mol ratio of O, TGA and NaHTe is 1:2.0-2.5:0.4-0.6, and wherein the molar weight of NaHTe draws according to the molar weight of tellurium powder in step (1); Described back flow reaction temperature is 100 oc-110 oc.
5. a kind of quantum dot fluorescence aspirin trace sensor according to claim 2 and its preparation method and application, is characterized in that, the volume ratio of the quantum dot solution described in step (3) and redistilled water is 0.1-3:100; The ratio of the described aspirin adding and quantum dot solution is 0.1-3mL:0.025mmol; The mol ratio of described aspirin, (3-aminopropyl) triethoxysilane, ethyl orthosilicate is 1:2-12:8-24; The volume ratio of ammoniacal liquor and ethyl orthosilicate is 1:1-2; Eluant, eluent used is the mixed solution of water and ethanol, and volume ratio is 1:1, wash-out three times; Described mixing time is 20-30 min; It is described that ethyl orthosilicate and ammoniacal liquor are joined to the above-mentioned system reaction time is 10-14 hour.
6. a kind of quantum dot fluorescence aspirin trace sensor according to claim 2 and its preparation method and application, is characterized in that, the trace sensor of preparing according to the method is for identifying fast and optical detection aspirin.
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