CN111303475B - Synthesis method of molecularly imprinted polymer based on nontoxic zinc oxide quantum dots - Google Patents
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Abstract
The invention discloses a synthesis method of a molecular imprinting polymer based on nontoxic zinc oxide quantum dots, which comprises the steps of preparing the zinc oxide quantum dots by a simple reflux method, modifying the zinc oxide quantum dots by 3-aminopropyltriethoxysilane APTES, mixing sulfadimidine, 3-aminopropyltriethoxysilane APTES, the zinc oxide quantum dots, tetraethoxysilane TEOS and ammonia water, and finally preparing the molecular imprinting polymer by a sol-gel method. The molecular imprinting polymer is synthesized based on the nontoxic zinc oxide quantum dots, is applied to the detection of sulfamethazine, and has good selectivity on the sulfamethazine.
Description
Technical Field
The invention belongs to the field of polymer synthesis, and particularly relates to a synthesis method of a molecularly imprinted polymer based on non-toxic zinc oxide quantum dots.
Background
Sulfadimidine is a commonly used antibacterial drug, plays a great role in disease prevention and treatment, is low in price, and is widely applied to the livestock industry in various countries all over the world. However, the abuse of the drug also causes great problems, and the drug has stable structure and is not easy to decompose, can enter a food chain along with the metabolism of animals and indirectly flows to a human body, so that the research finds that the excessive sulfamethazine can damage the health of the human body and has potential carcinogenicity. The maximum content of sulfonamides in food and feed regulated by Ministry of agriculture of China must not exceed 0.1mg kg -1 Currently, the common method for detecting sulfamethazine is mainly gas chromatography-mass spectrometry (GS-MS), High Performance Liquid Chromatography (HPLC) liquid chromatography-tandem mass spectrometry (LS-MS/MS), and the like. However, the method has high price of required instruments and complicated detection steps, so that the application of the method is limited. Therefore, it has become a hot spot to develop a rapid and simple detection method.
At present, a molecularly imprinted polymer prepared by combining quantum dots with a molecularly imprinted technology is applied to the field of detection, and the principle of the molecularly imprinted polymer is mainly that fluorescence of the quantum dots is changed according to electron or energy transfer between the quantum dots and a detected drug, so that the drug content is detected. Most of common imprinted polymers are based on cadmium telluride (CdTe) quantum dots serving as display signals for drug detection, but the cadmium telluride quantum dots contain heavy metals and cause secondary harm if leakage occurs. Therefore, researchers are seeking non-toxic and harmless quantum dots as display signals for further application.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for synthesizing a molecularly imprinted polymer based on non-toxic zinc oxide quantum dots, and the synthesized molecularly imprinted polymer has good selectivity on sulfadimidine.
In order to achieve the above object, the present invention comprises the steps of:
step one, adding 1.1g of zinc acetate dihydrate into every 150mL of absolute ethyl alcohol, preparing an absolute ethyl alcohol mixed solution by adopting a reflux method, adding 392mg of potassium hydroxide into every 20mL of absolute ethyl alcohol mixed solution, and uniformly stirring to obtain zinc oxide quantum dots (ZnO QDs);
modifying zinc oxide quantum dots ZnO QDs by using 3-aminopropyltriethoxysilane APTES, and modifying the zinc oxide quantum dots ZnO QDs by using 3-aminopropyltriethoxysilane APTES;
mixing sulfamethazine with ethanol, adding 3-Aminopropyltriethoxysilane (APTES), and uniformly mixing to obtain a solution A; dispersing zinc oxide quantum dot ZnO QDs powder modified by 3-aminopropyltriethoxysilane APTES in ethanol to obtain a solution B; mixing the solution A and the solution B, adding tetraethyl orthosilicate TEOS and ammonia water, and uniformly mixing to obtain a mixed solution A;
and step four, treating the mixed solution A by using a sol-gel method to prepare the molecularly imprinted polymer MIPs-ZnO QDs to obtain a final product.
The specific method of the first step is as follows:
firstly, mixing zinc acetate dihydrate and absolute ethyl alcohol, refluxing for 2 hours at 80 ℃ to completely dissolve the zinc acetate dihydrate in the absolute ethyl alcohol, and cooling to room temperature to obtain an absolute ethyl alcohol mixed solution;
and secondly, stirring the mixed solution of potassium hydroxide and absolute ethyl alcohol to completely dissolve the potassium hydroxide to obtain the zinc oxide quantum dots ZnO QDs.
The specific method of the second step is as follows:
firstly, weighing 400 mu L of 3-aminopropyltriethoxysilane APTES and 2mL of deionized water, uniformly mixing, then dropwise adding the mixed solution into a zinc oxide quantum dot ZnO QDs solution to obtain zinc oxide quantum dot ZnO QDs wrapped by the 3-aminopropyltriethoxysilane APTES with good water solubility,
and secondly, centrifuging the zinc oxide quantum dot ZnO QDs wrapped by the 3-aminopropyltriethoxysilane APTES, centrifuging and cleaning the centrifuged precipitate by absolute ethyl alcohol to remove unreacted impurities, drying in vacuum to constant weight, and grinding to obtain the zinc oxide quantum dot ZnO QDs powder modified by the 3-aminopropyltriethoxysilane APTES.
The concrete method of the third step is as follows:
firstly, weighing 222.64mg of sulfamethazine, dissolving in 40mL of ethanol, then adding 748 mu L of 3-aminopropyltriethoxysilane APTES, and stirring uniformly to obtain a solution A;
secondly, dispersing 100mg of zinc oxide quantum dot ZnO QDs powder modified by 3-aminopropyltriethoxysilane APTES in 40mL of ethanol to obtain a solution B;
and step three, mixing the solution A and the solution B, adding 1.6mL of tetraethoxysilane TEOS after uniformly stirring, adding 400 mu L of ammonia water, and uniformly stirring under a dark condition to obtain a mixed solution A.
The concrete method of the step four is as follows;
and (3) absorbing the precipitate of the mixed solution A, performing Soxhlet extraction by using the mixed solution of ethanol and acetonitrile, centrifuging and washing the precipitate for multiple times by using the mixed solution of ethanol and acetonitrile, and finally drying to obtain the molecularly imprinted polymer MIPs-ZnO QDs.
The volume ratio of ethanol to acetonitrile is 8:2, the Soxhlet extraction time is 48h, and the extraction solution is changed every 12 h.
Compared with the prior art, the preparation method comprises the steps of preparing the zinc oxide quantum dots by a simple reflux method, modifying the zinc oxide quantum dots by 3-aminopropyltriethoxysilane APTES, mixing the sulfamethazine, the 3-aminopropyltriethoxysilane APTES, the zinc oxide quantum dots, tetraethoxysilane TEOS and ammonia water, and finally preparing the molecularly imprinted polymer by a sol-gel method. The molecular imprinting polymer is synthesized based on the nontoxic zinc oxide quantum dots, is applied to the detection of sulfamethazine, and has good selectivity on the sulfamethazine.
Drawings
FIG. 1 shows the addition of different concentrations of SM to MIPs-ZnO and NIPs-ZnO 2 The later fluorescence spectrum; wherein, (a) is MIPs-ZnO, and (b) is NIPs-ZnO;
FIG. 2 shows MIPs-ZnO and NIPs-ZnO and SM 2 A linear fit of the existing line graph; wherein, (a) is MIPs-ZnO, and (b) is NIPs-ZnO;
FIG. 3 shows MIPs-ZnO and SDZ, SM 2 Linear fit straight line graphs exist.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The invention comprises the following steps:
step one, weighing 1.1g of zinc acetate dihydrate and 150mL of absolute ethyl alcohol, refluxing for 2 hours at 80 ℃ to completely dissolve the zinc acetate dihydrate in the absolute ethyl alcohol, and cooling the solution to room temperature. Then, 392mg of potassium hydroxide and 20mL of absolute ethanol were weighed and stirred with ultrasound for 30 minutes to completely dissolve the potassium hydroxide. To the ethanol solution of zinc acetate, an ethanol solution of potassium hydroxide was added dropwise with stirring, and it was seen that the solution rapidly became white and then gradually became colorless and transparent, indicating that ZnO QDs in the solution had been formed.
Step two, weighing 400 mu L of 3-aminopropyltriethoxysilane APTES and 2mL of deionized water, uniformly mixing, dropwise adding the mixed solution into the ZnO QDs solution obtained in the step one to obtain 3-aminopropyltriethoxysilane APTES-coated ZnO QDs with good water solubility, wherein a large amount of white precipitates can be seen to be separated out, centrifuging for 2 minutes by using a centrifuge at 3000 r/min, centrifugally cleaning the centrifuged precipitates for three times by using absolute ethyl alcohol to remove unreacted impurities, drying in vacuum at 80 ℃ to constant weight, and moderately grinding to obtain 3-aminopropyltriethoxysilane APTES-modified ZnO QDs. .
Weighing 222.64mg sulfamethazine, dissolving in 40mL ethanol, adding 748 mu L3-aminopropyl triethoxysilane APTES, and stirring for 30 min; 100mg of 3-aminopropyltriethoxysilane APTES modified ZnOQDs is ultrasonically dispersed in 40mL of ethanol, then the two solutions are mixed, stirred for 20min, then 1.6mL of TEOS is added, stirred for 10min, finally 400 mu L of ammonia water is added, and stirred for 24h under dark conditions.
And step four, after the reaction is finished, sucking the precipitate, performing Soxhlet extraction by using a mixed solution of ethanol and acetonitrile, wherein the volume ratio of the ethanol to the acetonitrile is 8:2, extracting for 48h, replacing an extracting solution every 12h, centrifuging and washing the precipitate for multiple times by using the mixed solution of ethanol and acetonitrile, and finally drying for 12h at 60 ℃ to obtain the molecularly imprinted polymer MIPs-ZnO.
Comparative example:
synthesizing a molecularly imprinted polymer NIPs-ZnO without sulfamethazine.
Step one, weighing 1.1g of zinc acetate dihydrate and 150mL of absolute ethyl alcohol, refluxing for 2 hours at 80 ℃ to completely dissolve the zinc acetate dihydrate in the absolute ethyl alcohol, and cooling the solution to room temperature. Then, 392mg of potassium hydroxide and 20mL of absolute ethanol were weighed and stirred with ultrasound for 30 minutes to completely dissolve the potassium hydroxide. To the ethanol solution of zinc acetate, an ethanol solution of potassium hydroxide was added dropwise with stirring, and it was seen that the solution rapidly became white and then gradually became colorless and transparent, indicating that ZnO QDs in the solution had been formed.
Step two, weighing 400 mu L of 3-aminopropyltriethoxysilane APTES and 2mL of deionized water, uniformly mixing, dropwise adding the mixed solution into the ZnO QDs solution obtained in the step one to obtain 3-aminopropyltriethoxysilane APTES-coated ZnO QDs with good water solubility, wherein a large amount of white precipitates can be seen to be separated out, centrifuging for 2 minutes by using a centrifuge at 3000 r/min, centrifugally cleaning the centrifuged precipitates for three times by using absolute ethyl alcohol to remove unreacted impurities, drying in vacuum at 80 ℃ to constant weight, and moderately grinding to obtain 3-aminopropyltriethoxysilane APTES-modified ZnO QDs. .
And step three, weighing 100mg of 3-aminopropyltriethoxysilane APTES modified ZnO QDs, ultrasonically dispersing the ZnO QDs in 40mL of ethanol, adding 748 mu L of 3-aminopropyltriethoxysilane APTES, stirring for 20min, adding 1.6mL of TEOS, stirring for 10min, finally adding 400 mu L of ammonia water, and stirring for 24h under the dark condition.
And step four, after the reaction is finished, sucking the precipitate, performing Soxhlet extraction by using a mixed solution of ethanol and acetonitrile, wherein the volume ratio of the ethanol to the acetonitrile is 8:2, extracting for 48h, replacing an extracting solution every 12h, centrifuging and washing the precipitate for multiple times by using the mixed solution of the ethanol and the acetonitrile, and finally drying the precipitate for 12h at 60 ℃ to obtain the molecularly imprinted polymer MIPs-ZnO not containing the sulfamethazine.
Compared with the comparative example, QDs @ SiO 2 @ MIPs was used to determine different concentrations of SM 2 (2-30μmol L -1 ) Based on Fluorescence (FL) quenching, QDs @ SiO 2 @ NIPs were also used as a comparative study. The quantitative relationship between the relative fluorescence intensity and the template concentration is expressed by Stern-Volmer equation (1):
F 0 /F＝1+K sv [C]
wherein F 0 And F is respectively the absence of SM 2 And has existence of SM 2 FL intensity of time. [ C ]]Is SM 2 Ksv is the quenching constant factor of the Stern-Volmer equation. Quenching and sensitivity are usually estimated using Ksv, using a imprinting factor K sv，MIP And K sv，NIP To evaluate the sensingSelectivity of the device.
Under the optimal conditions, namely the response time is 18min and the concentration of MIPs-ZnO is 150mg L -1 Adding different concentrations of SM to MIPs-ZnO solution 2 To study the sensitivity of MIPs-ZnO. For comparison, the NIPs-ZnO were studied under the same conditions. As shown in FIGS. 1(a) and (b), the fluorescence intensities of MIPs-ZnO and NIPs-ZnO are dependent on SM 2 The concentration changes. It is apparent that with SM 2 The decrease of the fluorescence intensity of the concentration MIPs-ZnO is obviously larger than that of the concentration NIPs-ZnO. Fluorescence quenching data follows the Stern-Volmer equation. As shown in FIG. 2(a), MIPs-ZnO is in the range of 0-40 for SM 2 Exhibits a linear response mu molL -1 The correlation coefficient 0.98547 of (c) and Ksv, MIP is 17910m -1 As shown in fig. 2(b), Ksv, NIP is 6330M -1 And a correlation coefficient 0.95236. The blot factor (IF), an important indicator polymer for evaluating blot selectivity, is defined as Ksv, MIP and a Ksv (k, k), NIP the ratio of (a) to (b). The IF is 2.83 by calculation, which shows that the selectivity of MIPs-ZnO is superior to NIP-ZnO. The detection limit (3. sigma./k) was 0.62. mu. mol L -1 。
Specific selectivity of MIPs-ZnO and target (SM) 2 ) And the change in fluorescence intensity after interaction with other congeners (SM, SDZ). As can be seen from FIG. 3, Stern-Volmer constant value pair SM for MIPs-ZnO 2 The sensitivity of (A) is higher than that of SM and SDZ, which shows that MIPs-ZnO is opposite to SM 2 Has excellent sensitivity, and further proves that the MIPs-ZnO has the same property with SM in the preparation process of the MIPs-ZnO 2 The specific recognition site of interest.
Claims (4)
1. A synthetic method of a molecular imprinting polymer based on nontoxic zinc oxide quantum dots is characterized by comprising the following steps:
step one, adding 1.1g of zinc acetate dihydrate into 150mL of absolute ethyl alcohol, preparing an absolute ethyl alcohol mixed solution by adopting a reflux method, adding 392mg of potassium hydroxide into 20mL of absolute ethyl alcohol mixed solution, and uniformly stirring to obtain zinc oxide quantum dots (ZnO QDs);
modifying zinc oxide quantum dots ZnO QDs by using 3-aminopropyltriethoxysilane APTES, and modifying the zinc oxide quantum dots ZnO QDs by using 3-aminopropyltriethoxysilane APTES; the specific method comprises the following steps:
firstly, weighing 400 mu L of 3-aminopropyltriethoxysilane APTES and 2mL of deionized water, uniformly mixing, then dropwise adding the mixed solution into a zinc oxide quantum dot ZnO QDs solution to obtain zinc oxide quantum dot ZnO QDs wrapped by the 3-aminopropyltriethoxysilane APTES with good water solubility,
centrifuging zinc oxide quantum dots (ZnO QDs) wrapped by 3-Aminopropyltriethoxysilane (APTES), centrifuging the centrifuged precipitate by absolute ethyl alcohol to remove unreacted impurities, drying in vacuum to constant weight, and grinding to obtain zinc oxide quantum dot (ZnO QDs) powder modified by 3-Aminopropyltriethoxysilane (APTES);
mixing sulfamethazine with ethanol, adding 3-Aminopropyltriethoxysilane (APTES), and uniformly mixing to obtain a solution A; dispersing zinc oxide quantum dot ZnO QDs powder modified by 3-Aminopropyltriethoxysilane (APTES) in ethanol to obtain a solution B; mixing the solution A and the solution B, adding tetraethyl orthosilicate TEOS and ammonia water, and uniformly mixing to obtain a mixed solution A; the specific method comprises the following steps:
firstly, weighing 222.64mg of sulfamethazine, dissolving in 40mL of ethanol, then adding 748 mu L of 3-aminopropyltriethoxysilane APTES, and stirring uniformly to obtain a solution A;
secondly, dispersing 100mg of zinc oxide quantum dot ZnO QDs powder modified by 3-aminopropyltriethoxysilane APTES in 40mL of ethanol to obtain a solution B;
step three, mixing the solution A and the solution B, adding 1.6mL of tetraethoxysilane TEOS after uniformly stirring, adding 400 mu L of ammonia water, and uniformly stirring under a dark condition to obtain a mixed solution A;
and step four, treating the mixed solution A by using a sol-gel method to prepare the molecularly imprinted polymer MIPs-ZnO QDs to obtain a final product.
2. The method for synthesizing the nontoxic zinc oxide quantum dot based molecularly imprinted polymer according to claim 1, is characterized in that the specific method in the first step is as follows:
firstly, mixing zinc acetate dihydrate and absolute ethyl alcohol, refluxing for 2 hours at 80 ℃ to completely dissolve the zinc acetate dihydrate in the absolute ethyl alcohol, and cooling to room temperature to obtain an absolute ethyl alcohol mixed solution;
and secondly, stirring the mixed solution of potassium hydroxide and absolute ethyl alcohol to completely dissolve the potassium hydroxide to obtain the zinc oxide quantum dots ZnO QDs.
3. The method for synthesizing the nontoxic zinc oxide quantum dot based molecularly imprinted polymer according to claim 1, wherein the specific method of the fourth step is as follows;
and (3) absorbing the precipitate of the mixed solution A, performing Soxhlet extraction by using the mixed solution of ethanol and acetonitrile, centrifuging and washing the precipitate for multiple times by using the mixed solution of ethanol and acetonitrile, and finally drying to obtain the molecularly imprinted polymer MIPs-ZnO QDs.
4. The method for synthesizing the nontoxic zinc oxide quantum dot-based molecularly imprinted polymer according to claim 3, wherein the volume ratio of ethanol to acetonitrile is 8:2, the Soxhlet extraction time is 48h, and the extraction solution is changed every 12 h.
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| KR20080032277A (en) * | 2006-10-09 | 2008-04-15 | 충북대학교 산학협력단 | Fabrication method of nanoscale multi-quantum dot junction device |
| CN104277190A (en) * | 2014-09-17 | 2015-01-14 | 兰州大学 | Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection |
| CN107384367A (en) * | 2017-06-19 | 2017-11-24 | 江苏大学 | A kind of ZnO quantum dot/porous silicon method of manufacturing fluorescent material and application |
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| KR20080032277A (en) * | 2006-10-09 | 2008-04-15 | 충북대학교 산학협력단 | Fabrication method of nanoscale multi-quantum dot junction device |
| CN104277190A (en) * | 2014-09-17 | 2015-01-14 | 兰州大学 | Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection |
| CN107384367A (en) * | 2017-06-19 | 2017-11-24 | 江苏大学 | A kind of ZnO quantum dot/porous silicon method of manufacturing fluorescent material and application |
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| "An optical sensor with specific binding sites for the detection of thioridazine hydrochloride based on ZnO-QDs coated with molecularly imprinted polymer";Ali A. Ensafi et al.;《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》;20180825;第460-465页 * |
| "Magnetic ZnO surface-imprinted polymers prepared by ARGET ATRP and the application for antibiotics selective recognition";Longcheng Xu et al.;《RSC Advances》;20120404;第5571-5579页 * |
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