CN109908874A - A kind of novel MoS2QDs@MIPs molecularly imprinted polymer and preparation method - Google Patents
A kind of novel MoS2QDs@MIPs molecularly imprinted polymer and preparation method Download PDFInfo
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Abstract
The invention belongs to molecular imprinting technologies and bioanalysis detection technique field, are related to a kind of novel MoS2QDs@MIPs molecularly imprinted polymer and preparation method.The preparation method is that first preparing quantum dot MoS2 QDs, then MoS is wrapped in by the way that amikacin to be embedded into silica shell2 Quantum dot compound is obtained on QDs core, finally elutes amikacin in quantum dot compound to obtain the molecularly imprinted polymer MoS with amikacin space imprinted sites2 QDs@MIPs.The method is simple and easy, low in cost, gained MoS2QDs@MIPs has relatively stable optical property, have to tested substance amikacin highly selective, there is the shorter response time simultaneously, having the advantages that low testing cost, high sensitivity, fireballing when for detecting amikacin, can be used for the content detection of amikacin.
Description
Technical field
The invention belongs to molecular imprinting technology and bioanalysis detection technique field, it is related to a kind of for antibiotic detection
Novel molecular engram polymer and preparation method thereof more particularly to a kind of novel MoS2QDs@MIPs molecularly imprinted polymer and
Preparation method.
Background technique
In recent years, with the development of society, scientific and technological, medical technology be constantly progressive, antibiotic is widely used, with
Also there is the problem of abuse of antibiotics, in the drug-fast bacteria generated by abuse of antibiotics and organism, human body and environment
A series of the problem of remaining part antibiotic has caused secure contexts, therefore how to eliminate the pollution and residual of antibiotic
Just become one of the hot spot of domestic and foreign scholars' research.Since ingredient is extremely complex in organism, human body and environmental sample, and it is residual
The antibiotic agents content being left in them is again relatively relatively low, and there are more problems during detecting to it, such as examines
The problems such as sensitivity of survey method, selectivity, poor Stability and veracity.
After being studied as biomarker CdSe quantum dot from Alivisatos in 1998 etc., semiconductor amount
Application of the son point in analysis detection is greatly developed.Quantum dot (quantum dots, QDs) is since there are significant sizes
Effect, skin effect, quantum effect have ultraviolet light absorbing, the response of supper-fast optical nonlinearity, luminescence generated by light and Qiang Kangguang
The unique photoelectric properties such as oxidisability, therefore be widely used.But single quantum dot fluorescence probe detection is vulnerable to ring
The interference of border condition haves the shortcomings that poor selectivity, stability are limited.To solve this problem, by quantum dot and other technologies phase
In conjunction with research gradually increase.
Molecular imprinting technology (Molecular imprinting technique, MIT) is a kind of prepares to a certain specific
Molecule has the technology of the polymer of distinctive selectivity identification function, and the polymer of preparation is known as molecularly imprinted polymer
(Molecularly imprinted polymers, MIP).By the height of quantum dot excellent optical property and molecular imprinting technology
Selective binding is got up, and is compensated for quantum dot fluorescence probe just using the high target target-locating and enriching ability of MIP and is selected
Property difference disadvantage, a kind of novel optical sensor for being based on molecular imprinting functionalization quantum dot (QDs MIP) can be constructed.
Molecularly imprinted polymer material can be customized for object " cutting the garment according to the figure ", realize the single-minded identification to target molecule, can
It compares favourably with natural biological recognition system (enzyme-to-substrate), has and prepare simple, stability good (acid and alkali-resistance, high temperature, height
Pressure, organic solvent and harsh environment), the features such as service life is long, easy to maintain, cheap, in Solid Phase Extraction, chiral separation, mould
Quasi- biological antibody, catalysis and organic synthesis etc. are widely used, and are solved in the complex systems such as environment, biology
Simple and direct, the reliable means of the highly selective identification of specific target molecules.
Amikacin is aminoglycoside antibiotics, and antimicrobial spectrum is similar to gentamicin, and clinic is mainly used for big to celebrating mould
Element, the various infection as caused by Escherichia coli, proteus and Pseudomonas aeruginosa of the drug resistant gram negative bacilli of kanamycins, no
Good reaction mainly causes cochlear nerve lesion, similar to ear, renal toxicity and gentamicin.Amikacin is as antibiotic in quilt
During extensive use, to environment, organism and human body, there is also certain harmfulness.The side of existing detection amikacin
Although there are many kinds of methods, such as liquid chromatography, colorimetric method, molecular engram SPR nano-sensor method, the shortcomings that liquid chromatography
It is if mobile phase changes from the flow pattern for being injected into detector, any diffusion and the isolated material of reservation will significantly be led
The expansion of coloring spectral peak and the reduction of column efficiency;Micellar electrokinetic chromatography is easy to be broken there are bubble generation, detects sensitive
Low, the problems such as filling kind is limited is spent, and testing cost is high, the time is long；And colorimetric method, the disadvantage is that serious interference, is tested group
Divide purity higher, sensitivity is lower；And for the detection method using molecular engram SPR nano-sensor, although aptamer goes out
Now provide a kind of new tool of quickly detection antibiotic, but this process is more than above-mentioned high performance liquid chromatography and colorimetric method
It is complicated.
Currently, more and more researchers have begun using molecular engram the detection for carrying out antibiotic.But it is existing
Have in technology, there has been no combine the excellent optical property of quantum dot and the highly selective of molecular imprinting technology to A meter Ka
The method report that star is detected.
To sum up, main problem of the existing technology has: (1) single quantum dot fluorescence probe detection is vulnerable to environmental condition
Interference, have the shortcomings that poor selectivity, stability are limited；(2) single molecularly imprinted polymer technology has highly selective,
But do not have excellent optical property mostly；(3) existing amikacin detection method is at high cost, the time is long, poor sensitivity.
Therefore, research can by the excellent optical property of quantum dot and molecular imprinting technology it is highly selective combine to Ah
The method that meter Ka Xing is quick and precisely detected, ensure human health, food safety, in terms of all have it is important
Meaning and prospect.
Summary of the invention
For overcome the deficiencies in the prior art, above-mentioned problems of the prior art are solved, it is an object of the invention to
A kind of novel molecular engram polymer MoS is provided2 The preparation method of QDs MIPs first prepares quantum dot MoS2 QDs, then again
MoS is wrapped in by the way that antibiotic amikacin to be embedded into silica shell2 To form molecular engram polymerization on QDs core
Object MoS2 QDs@MIPs, the material have good photostability, to tested substance amikacin have it is highly selective, simultaneously
With the shorter response time, response detection can be carried out immediately.
The technical solution adopted by the present invention is that: a kind of novel molecular engram polymer MoS2 The preparation method of QDs@MIPs,
Characterized by comprising the following steps: preparing quantum dot MoS first2 QDs, then again by the way that amikacin is embedded into dioxy
MoS is wrapped in SiClx shell2 Quantum dot compound is obtained on QDs core, finally elutes amikacin in quantum dot compound
Get off to obtain the molecularly imprinted polymer MoS with amikacin space imprinted sites2 QDs@MIPs。
Further, the molecularly imprinted polymer MoS2 The preparation method of QDs@MIPs, which is characterized in that specifically include with
Lower step:
S1. MoS2 The preparation of QDs
L-cysteine is dissolved in deionized water, ultrasound obtains solution A；
By Na2MoPO4·2H2O is dissolved in deionized water, ultrasound, adjusts pH to 5.8-6.5 with the HCl solution of 1mol/L, obtains molten
Liquid B；
Solution B is added dropwise in solution A, ultrasound obtains mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) autoclave
In, 36 h are reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of membrane filtration, finally
It dialyses to obtain quantum dot MoS with the bag filter that the molecular weight that shuts off is 20002 QDs。
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8-3.6 mL, 3- aminopropyl triethoxysilane 40 μ L, amikacin 10-15.0 mg, ammonium hydroxide 50-300 μ L and just
100 μ L of silester, sealing, is stirred overnight.The solution obtained after stirring is demulsified with acetone, is centrifuged, discards after removing impurity
Supernatant, obtained sediment are quantum dot compound, are 4 ︰'s 1 by the volume ratio of quantum dot compound Yi Yi Chun ︰ acetonitrile
Ethanol/acetonitrile solution is washed as eluent, is centrifuged at a high speed, by the body of the obtained sediment of centrifugation Yong Yi Chun ︰ acetonitrile again
Product is than being that the ethanol/acetonitrile solution of 4 ︰ 1 washs repeatedly, until supernatant can't detect amikacin, high speed centrifugation, finally
Gained sediment is placed in 80 DEG C of 12 h of drying in baking oven again, MoS can be obtained2 QDs@MIPs powder.
Further, in step s 2, the centrifugation is specially with 2000 turns of supercentrifuge 2 min of centrifugation.
Further, in step s 2, the detection is specially to be detected with ultraviolet-uisible spectrophotometer.
Further, the operation of step S1 is as follows:
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A；
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, with the HCl of 1mol/L adjust pH to
5.8-6.5 obtaining solution B；
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then that mixed liquor is transferred to polytetrafluoroethylene (PTFE) high pressure is anti-
It answers in kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of membrane filtration,
Finally dialyse to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
The present invention also provides a kind of novel molecular engram polymer MoS2 QDs@MIPs, it is characterised in that: by MoS2
QDs nano particle, which is located in MIPs ball, to be constituted.
Further, the MoS2 The partial size of QDs nano particle is 1-10nm.
Further, the partial size of the MIPs ball is 15-50 nm.
Further, the molecularly imprinted polymer MoS2 QDs@MIPs is by above-mentioned molecularly imprinted polymer MoS2 QDs@
The preparation method of MIPs is made.
Preferably, the molecularly imprinted polymer MoS2 QDs@MIPs is made by following preparation method:
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A；
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, with the HCl of 1mol/L adjust pH to
5.8-6.5 obtaining solution B；
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then that mixed liquor is transferred to polytetrafluoroethylene (PTFE) high pressure is anti-
It answers in kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of membrane filtration,
Finally dialyse to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8-3.6 mL, 3- aminopropyl triethoxysilane 40 μ L, amikacin 10-15.0 mg, ammonium hydroxide 50-300 μ L and just
100 μ L of silester, sealing, is stirred overnight.The solution obtained after stirring is demulsified with acetone, is centrifuged, discards after removing impurity
Supernatant, obtained sediment are quantum dot compound, are 4 ︰'s 1 by the volume ratio of quantum dot compound Yi Yi Chun ︰ acetonitrile
Ethanol/acetonitrile solution is washed as eluent, 2000 turn of 2 min centrifuge separation of supercentrifuge, the sediment that centrifugation is obtained
Again Yong the volume ratio of Yi Chun ︰ acetonitrile be 4 ︰ 1 ethanol/acetonitrile solution wash repeatedly, until supernatant with UV, visible light be divided light
Until degree meter can't detect amikacin, gained sediment is finally placed in baking oven again by 2000 turn of 2 min centrifugation of supercentrifuge
In 80 DEG C of 12 h of drying, MoS can be obtained2 QDs@MIPs powder.
The present invention also provides a kind of novel molecular engram polymer MoS2 QDs@MIPs detects antibiotic amikacin
Purposes can be applied in antibiotic amikacin content detection, such as the remaining A meter Ka in detection environment, food sample
Star.
The principle of the present invention is:
MoS of the invention2QDs@MIPs molecularly imprinted polymer is that antibiotic is embedded into silica shell to be wrapped in
MoS2To form molecularly imprinted polymer on QDs core, which has high selectivity.
MoS of the present invention2In QDs@MIPs synthesis process, select Qula logical as surfactant, hexamethylene as continuous
Phase, ammonium hydroxide are as catalyst, 3- aminopropyl triethoxysilane as function monomer, ethyl orthosilicate as crosslinking agent, template
Molecule is antibiotic amikacin.In preparation method of the present invention, quantum dot is dispersed in hexamethylene and the logical middle formation gel of Qula,
It is hydrolyzed by ethyl orthosilicate, ammonium hydroxide makees catalyst and forms silicon dioxide layer on the surface of quantum dot.During polymerization
Amino (- NH in reaction, in 3- aminopropyl triethoxysilane2) and template molecule function (- OH and-NH2) group is to pass through
It is hydrogen-bonded.Therefore, Successful antibiotic it is embedded into the MoS of Silica-coated2In QDs.During elution, template
Hydrogen bond in molecule and 3- aminopropyl triethoxysilane is interrupted, and leaves the antibiotic imprinted sites in silicon matrix.The trace
The size of the size in site, structure and antibiotic is consistent with structure, therefore can be with specific detection antibiotic.
Beneficial effects of the present invention.
1, MoS of the invention2When QDs@MIPs is detected for antibiotic, testing cost is low, detection sensitivity is high, detection is fast
Degree is fast, and detection efficiency is high.
2, MoS of the invention2QDs@MIPs has specific selectivity to analyte, in several similar antibiotic sulphur
Sour streptomysin (SS), kanamycin sulfate (KS), tobramycin sulfate (TS), gentamicin sulphate (QS), ribostamin
(HS) and in neomycinsulphate (NS) it can be achieved to can be realized selective enumeration method to the high degree of recognition of amikacin.
3, MoS of the invention2QDs@MIPs can keep relatively stable optical property in 18 days, have good steady
It is qualitative, it is easy to save.
4, MoS of the invention2Preparation method is simple, low in cost by QDs@MIPs.
Detailed description of the invention
Fig. 1 (A) is MoS prepared by the embodiment of the present invention 12The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer；
Fig. 1 (B) is the MoS of comparative example 1 of the present invention preparation2The transmission electron microscope picture of QDs@NIPs non-molecularly imprinted polymer；
Fig. 1 (C) is MoS prepared by the embodiment of the present invention 22The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer；
Fig. 1 (D) is MoS prepared by the embodiment of the present invention 32The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer；
Fig. 1 (E) is MoS prepared by the embodiment of the present invention 42The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer；
Fig. 1 (F) is MoS prepared by the embodiment of the present invention 52The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer；
Fig. 2 (A) is MoS prepared by the embodiment of the present invention 12QDs@MIPs molecularly imprinted polymer interacts glimmering with antibiotic
Light spectrogram；
Fig. 2 (B) is MoS prepared by the embodiment of the present invention 12The line of QDs@MIPs molecularly imprinted polymer and antibiotic interaction
Property fitted figure；
Fig. 3 (A) is the MoS of comparative example 1 of the present invention preparation2What QDs@NIPs non-molecularly imprinted polymer and antibiotic interacted
Fluorescence spectra；
Fig. 3 (B) is the MoS of comparative example 1 of the present invention preparation2What QDs@NIPs non-molecularly imprinted polymer and antibiotic interacted
Linear Fit Chart；
Fig. 4 is MoS prepared by the embodiment of the present invention 12The fluorescent stability figure of QDs@MIPs molecularly imprinted polymer at room temperature；
Fig. 5 is MoS prepared by the embodiment of the present invention 12Selection of the QDs@MIPs molecularly imprinted polymer to several similar antibiotic
Property response diagram.
Specific embodiment
Technical solution of the present invention is described in detail with reference to the accompanying drawing, but the contents of the present invention are not limited to
This.
Embodiment 1:
MoS2The preparation of QDs@MIPs
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8 mL, 3- aminopropyl triethoxysilane, 40 μ L, 12 mg of amikacin, ammonium hydroxide 200 μ L and 100 μ of ethyl orthosilicate
L, sealing, is stirred overnight.The solution obtained after stirring is demulsified with acetone, with 2000 turn 2 of supercentrifuge after removing impurity
Min centrifugation, discards supernatant liquid, obtained sediment is quantum dot compound, by the body of quantum dot compound Yi Yi Chun ︰ acetonitrile
Product is washed than the ethanol/acetonitrile solution for being 4 ︰ 1 as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge will be centrifuged
To sediment washed repeatedly Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 again, until supernatant is with ultraviolet
Until visible spectrophotometer can't detect amikacin, 2000 turn of 2 min centrifugation of supercentrifuge finally again precipitates gained
Object is placed in 80 DEG C of 12 h of drying in baking oven, and MoS can be obtained2 QDs@MIPs molecularly imprinted polymer powder.
The MoS prepared by embodiment 12The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer is shown in Fig. 1 (A).
Comparative example 1
Non-molecularly imprinted polymer (MoS2QDs@NIPs) preparation:
It is prepared using method same as Example 1, but does not add template molecule amikacin.
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@NIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 μ L of 100 2.8 mL, 3- aminopropyl triethoxysilane, 40 μ L, 200 μ L of ammonium hydroxide and ethyl orthosilicate, sealing are stirred
Night.The solution obtained after stirring is demulsified with acetone, is centrifuged, is discarded with 2000 turn of 2 min of supercentrifuge after removing impurity
Clear liquid, obtained sediment are quantum dot compound, the second for being 4 ︰ 1 by the volume ratio of quantum dot compound Yi Yi Chun ︰ acetonitrile
Alcohol/acetonitrile solution is washed as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge, the sediment that centrifugation is obtained is again
It is washed repeatedly Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1, until supernatant UV, visible light spectrophotometric
Until meter can't detect amikacin, gained sediment is finally placed in baking oven by 2000 turn of 2 min centrifugation of supercentrifuge again
80 DEG C of 12 h of drying, can be obtained MoS2 QDs@NIPs non-molecularly imprinted polymer powder.
The MoS prepared by comparative example 12The transmission electron microscope picture of QDs@NIPs non-molecularly imprinted polymer is shown in Fig. 1 (B).
Embodiment 2:
MoS2The preparation of QDs@MIPs
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 3.6 mL, 3- aminopropyl triethoxysilane, 40 μ L, 10 mg of amikacin, ammonium hydroxide 200 μ L and 100 μ of ethyl orthosilicate
L, sealing, is stirred overnight.The solution obtained after stirring is demulsified with acetone, with 2000 turn 2 of supercentrifuge after removing impurity
Min centrifugation, discards supernatant liquid, obtained sediment is quantum dot compound, by the body of quantum dot compound Yi Yi Chun ︰ acetonitrile
Product is washed than the ethanol/acetonitrile solution for being 4 ︰ 1 as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge will be centrifuged
To sediment washed repeatedly Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 again, until supernatant is with ultraviolet
Until visible spectrophotometer can't detect amikacin, 2000 turn of 2 min centrifugation of supercentrifuge finally again precipitates gained
Object is placed in 80 DEG C of 12 h of drying in baking oven, and MoS can be obtained2 QDs@MIPs molecularly imprinted polymer powder.
The MoS prepared by embodiment 22The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer is shown in Fig. 1 (C).
Embodiment 3:
MoS2The preparation of QDs@MIPs
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 3.0 mL, 3- aminopropyl triethoxysilane, 40 μ L, 15.0 mg of amikacin, 200 μ L of ammonium hydroxide and ethyl orthosilicate
100 μ L, sealing, are stirred overnight.The solution obtained after stirring is demulsified with acetone, with 2000 turns of supercentrifuge after removing impurity
2 min centrifugation, discards supernatant liquid, obtained sediment is quantum dot compound, by quantum dot compound Yi Yi Chun ︰ acetonitrile
The ethanol/acetonitrile solution that volume ratio is 4 ︰ 1 is washed as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge will be centrifuged
Obtained sediment is washed Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 repeatedly again, until supernatant is purple
Until outer visible spectrophotometer can't detect amikacin, 2000 turn of 2 min centrifugation of supercentrifuge finally again sinks gained
Starch is placed in 80 DEG C of 12 h of drying in baking oven, and MoS can be obtained2 QDs@MIPs molecularly imprinted polymer powder.
The MoS prepared by embodiment 32The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer is shown in Fig. 1 (D).
Embodiment 4:
MoS2The preparation of QDs@MIPs
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8 mL, 3- aminopropyl triethoxysilane, 40 μ L, 12.0 mg of amikacin, 50 μ L of ammonium hydroxide and ethyl orthosilicate 100
μ L, sealing, is stirred overnight.The solution obtained after stirring is demulsified with acetone, with 2000 turn 2 of supercentrifuge after removing impurity
Min centrifugation, discards supernatant liquid, obtained sediment is quantum dot compound, by the body of quantum dot compound Yi Yi Chun ︰ acetonitrile
Product is washed than the ethanol/acetonitrile solution for being 4 ︰ 1 as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge will be centrifuged
To sediment washed repeatedly Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 again, until supernatant is with ultraviolet
Until visible spectrophotometer can't detect amikacin, 2000 turn of 2 min centrifugation of supercentrifuge finally again precipitates gained
Object is placed in 80 DEG C of 12 h of drying in baking oven, and MoS can be obtained2 QDs@MIPs molecularly imprinted polymer powder.
The MoS prepared by embodiment 42The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer is shown in Fig. 1 (E).
Embodiment 5:
MoS2The preparation of QDs@MIPs
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A.
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, is adjusted with the HCl of 1mol/L
PH to 5.8-6.5, obtains solution B.
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, 36 h is reacted at 200 oC.It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of filter membrane
Filtering finally dialyses to obtain MoS with the bag filter that the molecular weight that shuts off is 20002Quantum dot (MoS2 QDs).
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8 mL, 3- aminopropyl triethoxysilane, 40 μ L, 12.0 mg of amikacin, 100 μ L of ammonium hydroxide and ethyl orthosilicate
100 μ L, sealing, are stirred overnight.The solution obtained after stirring is demulsified with acetone, with 2000 turns of supercentrifuge after removing impurity
2 min centrifugation, discards supernatant liquid, obtained sediment is quantum dot compound, by quantum dot compound Yi Yi Chun ︰ acetonitrile
The ethanol/acetonitrile solution that volume ratio is 4 ︰ 1 is washed as eluent, and 2000 turn of 2 min centrifuge separation of supercentrifuge will be centrifuged
Obtained sediment is washed Yong the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 repeatedly again, until supernatant is purple
Until outer visible spectrophotometer can't detect amikacin, 2000 turn of 2 min centrifugation of supercentrifuge finally again sinks gained
Starch is placed in 80 DEG C of 12 h of drying in baking oven, and MoS can be obtained2 QDs@MIPs molecularly imprinted polymer powder.
The MoS prepared by embodiment 52The transmission electron microscope picture of QDs@MIPs molecularly imprinted polymer is shown in Fig. 1 (F).
Embodiment 6:
(1) MoS2The performance test of QDs@MIPs
It is added into the phosphate buffer (pH=7.0) of 10 mL by the resulting MoS of embodiment 12The polymerization of QDs@MIPs molecular engram
2.0 mg of object, ultrasonic vibration 20 minutes.It is separately added into the above-mentioned solution of 1 mL into the colorimetric cylinder of 16 10 mL, and is separately added into
A series of amikacin standard solution 1mL of various concentrations, the concentration of amikacin standard solution be followed successively by 0.5nmol/L,
1nmol/L、2nmol/L、5nmol/L、10nmol/L、15nmol/L、20nmol/L、30nmol/L、40nmol/L、50nmol/
L, 60nmol/L, 80nmol/L, 100nmol/L, 200nmol/L, 500nmol/L and 1000nmol/L.It is uniformly mixed.Using glimmering
Excitation wavelength is adjusted to 350 nm by light spectrophotometer, and spectral region is selected in 390 and 560nm, measures a series of above-mentioned solution
Fluorescence emission spectrum.Observation various concentration amikacin corresponds to the fluorescence spectrum of system, observes whether its fluorescence intensity generates
Quenching determines MoS with this2Whether QDs MIPs has selection performance.MoS2The interaction of QDs@MIPs and antibiotic it is glimmering
Light spectrogram is shown in Fig. 2 (A)；The Linear Fit Chart that fluorescence intensity ratio changes with amikacin concentration is drawn simultaneously, sees Fig. 2
(B)。
By Fig. 2 (A) and Fig. 2 (B) it is found that under identical testing conditions, MoS2QDs@MIPs molecularly imprinted polymer pair
Template molecule amikacin has apparent fluorescence response, and system fluorescence generates quenching, i.e. MoS2QDs@MIPs to template molecule Ah
Meter Ka Xing has specific recognition effect.When amikacin concentration is 0.5-1000nmol/L, fluorescence intensity ratio and A meter Ka
The concentration of star is in a linear relationship, linear equation are as follows: y=1.208+0.0150x, R2=0.9948, it follows that fluorescence intensity ratio
It is good with amikacin linear relationship.After tested, MoS2QDs@MIPs molecularly imprinted polymer is limited to the detection of amikacin
0.23nmol/L。
(2)MoS2The performance detection of QDs@NIPs
It is added into the phosphate buffer (pH=7.0) of 10 mL by the resulting MoS of comparative example 12The non-molecular engram of QDs NIPs is poly-
Close 2.0 mg of object, ultrasonic vibration 20 minutes.It is separately added into the above-mentioned solution of 1 mL into the colorimetric cylinder of 9 10 mL, and is separately added into
A series of amikacin standard solution 1mL of various concentrations, the concentration of amikacin standard solution be followed successively by 0.5nmol/L,
1nmol/L,2nmol/L,4nmol/L,6nmol/L,8nmol/L,10nmol/L,12nmol/L,15nmol/L.It is uniformly mixed.
Excitation wavelength is adjusted to by 350 nm using sepectrophotofluorometer, spectral region is selected in 390 and 560nm, measures an above-mentioned system
The fluorescence emission spectrum of column solution.Observation various concentration amikacin corresponds to the fluorescence spectrum of system, and observing its fluorescence intensity is
No generation quenching determines MoS with this2Whether QDs NIPs has selection performance.MoS2The phase interaction of QDs NIPs and antibiotic
Fluorescence spectra is shown in Fig. 3 (A)；The Linear Fit Chart that fluorescence intensity ratio changes with amikacin concentration is drawn simultaneously, is seen
Fig. 3 (B).
System fluorescence intensity is almost unchanged it can be seen from Fig. 3 (A), by Fig. 3 (A) and Fig. 3 (B) it is found that identical
Under testing conditions, MoS2QDs@NIPs non-molecularly imprinted polymer does not have apparent fluorescence response to template molecule amikacin,
Quenching is not generated to system fluorescence.
Embodiment 7:
MoS2The optical stability of QDs@MIPs
In order to test MoS2The optical stability of QDs@MIPs utilizes the resulting MoS of embodiment 12QDs@MIPs molecular engram is poly-
Object is closed, at room temperature, continuous 30 days, measures its fluorescence spectrum, excitation wavelength is 350 nm, and draws fluorescent stability figure.Room
The lower MoS of temperature2The fluorescent stability figure of QDs@MIPs, is shown in Fig. 4.As seen from Figure 4, MoS at room temperature2The fluorescence of QDs@MIPs is strong
Degree just gradually decreases after 18 days, and wherein spectral width and launch wavelength remain unchanged.It follows that gained MoS2QDs@MIPs points
Sub- imprinted polymer is able to maintain relatively stable optical property in 18 days, this phenomenon also illustrates MoS2QDs@MIPs has
Good stability.
Embodiment 8:
MoS2The selective enumeration method of QDs@MIPs
In order to test MoS2The selectivity of QDs@MIPs, while using MoS2QDs@NIPs is compared, and uses several antibiotics
Like object streptomycin sulphate (SS), kanamycin sulfate (KS), tobramycin sulfate (TS), gentamicin sulphate (QS), sulfuric acid core
Saccharocin (HS) and neomycinsulphate (NS) have carried out MoS2QDs@MIPs and MoS2Selectivity of the QDs@NIPs to amikacin
Test.Gained MoS2QDs@MIPs and MoS2QDs@NIPs is shown in Fig. 5 to the selective response figure of above-mentioned several antibiotic.
As shown in Figure 5, MoS2QDs@MIPs is higher than to streptomycin sulphate (SS), sulfuric acid the degree of recognition of amikacin (AS)
Kanamycins (KS), tobramycin sulfate (TS), gentamicin sulphate (QS), ribostamin (HS) and neomycinsulphate
(NS) degree of recognition, i.e. MoS2QDs@MIPs only has specific recognition effect to template molecule amikacin.And MoS2QDs@
NIPs is to antibiotic amikacin (AS), streptomycin sulphate (SS), kanamycin sulfate (KS), tobramycin sulfate (TS), sulphur
Sour gentamicin (QS), ribostamin (HS) are almost the same with the fluorescence reaction of neomycinsulphate (NS).These result tables
It is bright, MoS2The recognition mechanism of QDs@MIPs is the shape based on template, the interaction of size and function.In MoS2QDs@NIPs
In, because not adding template, do not form specific recognition site, therefore MoS2Suction of the QDs@NIPs to template molecule
Attached ability is far below MoS2QDs@MIPs, and there is no significant difference with the quenching ability of other similar antibiotic.
Embodiment 9:
Sample analysis
Using the MoS obtained by embodiment 12QDs@MIPs carrys out the amikacin in test sample.
Take 3 parts of river water sample, heating is boiled, with 0.22 μm membrane filtration 3 times.With 1 gained MoS of embodiment2QDs@MIPs,
According to MoS in embodiment 62The concentration of amikacin in linear equation counting system in the performance test of QDs@MIPs, according to
Scalar quantity and measured value calculate the rate of recovery, measure the rate of recovery of amikacin in 3 parts of samples respectively, the results are shown in Table 1.
The determination of recovery rates result of amikacin in 1 sample of table
As shown in Table 1, MoS2QDs@MIPs is to the rate of recovery of amikacin in 98.8%-103.5%, and RSD value is below
5.78%, illustrate that the accuracy of this method is higher, precision is preferable.
The above is only presently preferred embodiments of the present invention, the interest field being not intended to limit the invention.It is any with this
The technical solution or anyone skilled in the art that the interest field that claim is covered is implemented utilize
The method content of the disclosure above makes the scheme of many possible changes and modifications, all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of novel molecular engram polymer MoS2 The preparation method of QDs@MIPs, which comprises the following steps: first
First prepare quantum dot MoS2 Then QDs is wrapped in MoS by the way that amikacin to be embedded into silica shell again2 QDs core
On obtain quantum dot compound, finally amikacin in quantum dot compound is eluted to obtain and is printed with amikacin space
The molecularly imprinted polymer MoS in mark site2 QDs@MIPs。
2. a kind of novel molecular engram polymer MoS as described in claim 12The preparation method of QDs@MIPs, feature exist
In: the molecularly imprinted polymer MoS2 The preparation method of QDs@MIPs, which is characterized in that specifically includes the following steps:
S1. MoS2 The preparation of QDs
L-cysteine is dissolved in deionized water, ultrasound obtains solution A；
By Na2MoPO4·2H2O is dissolved in deionized water, ultrasound, adjusts pH to 5.8-6.5 with the HCl solution of 1mol/L, obtains molten
Liquid B；
Solution B is added dropwise in solution A, ultrasound obtains mixed liquor, then mixed liquor is transferred to polytetrafluoroethylene (PTFE) autoclave
In, 36 h are reacted at 200 oC；
It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of membrane filtration, is finally 2000 with the molecular weight that shuts off
Bag filter dialyse to obtain quantum dot MoS2 QDs；
S2. MoS2 The preparation of QDs@MIPs
By quantum dot MoS2 QDs 6mL is added in 100mL beaker, hexamethylene 15mL is added under mechanical stirring, Qula leads to X-
100 2.8-3.6 mL, 3- aminopropyl triethoxysilane 40 μ L, amikacin 10-15.0 mg, ammonium hydroxide 50-300 μ L and just
100 μ L of silester, sealing, is stirred overnight；
The solution obtained after stirring is demulsified with acetone, is centrifuged after removing impurity, discards supernatant liquid, obtained sediment is to measure
Son point compound washes quantum dot compound using the ethanol/acetonitrile solution that the volume ratio of Yi Chun ︰ acetonitrile is 4 ︰ 1 as eluent
It washs, is centrifuged at a high speed, the ethanol/acetonitrile solution that the volume ratio by the obtained sediment of centrifugation Yong Yi Chun ︰ acetonitrile again is 4 ︰ 1 is anti-
After backwashing is washed, and until supernatant can't detect amikacin, gained sediment is finally placed in 80 in baking oven by high speed centrifugation again
DEG C dry 12 h, can be obtained MoS2 QDs@MIPs powder.
3. a kind of novel molecular engram polymer MoS as claimed in claim 22The preparation method of QDs@MIPs, feature exist
In: the operation of step S1 is as follows:
S1. MoS2 The preparation of QDs
0.5 g of L-cysteine is dissolved in 50 mL of deionized water, 10 min of ultrasound obtain solution A；
By Na2MoPO4·2H20.25 g of O is dissolved in 25 mL of deionized water, 10 min of ultrasound, with the HCl of 1mol/L adjust pH to
5.8-6.5 obtaining solution B；
10 min of ultrasound in solution A are added dropwise in solution B, obtain mixed liquor, then that mixed liquor is transferred to polytetrafluoroethylene (PTFE) high pressure is anti-
It answers in kettle, 36 h is reacted at 200 oC；
It after solution natural cooling, is first filtered with filter paper, then with 0.22 μm of membrane filtration, is finally 2000 with the molecular weight that shuts off
Bag filter dialyse to obtain quantum dot MoS2 QDs。
4. a kind of novel molecular engram polymer MoS as claimed in claim 32The preparation method of QDs@MIPs, feature exist
In: in step s 2, the centrifugation is specially with 2000 turns of supercentrifuge 2 min of centrifugation.
5. a kind of novel molecular engram polymer MoS as claimed in claim 32The preparation method of QDs@MIPs, feature exist
In: in step s 2, the detection is specially to be detected with ultraviolet-uisible spectrophotometer.
6. a kind of novel molecular engram polymer MoS2QDs@MIPs, it is characterised in that: by MoS2 QDs nano particle is located at
It is constituted in MIPs ball.
7. a kind of novel molecular engram polymer MoS as claimed in claim 62QDs@MIPs, it is characterised in that: described
MoS2 The partial size of QDs nano particle is 1-10nm.
8. a kind of novel molecular engram polymer MoS as claimed in claim 62QDs@MIPs, it is characterised in that: the MIPs
The partial size of ball is 15-50 nm.
9. a kind of novel molecular engram polymer MoS as claimed in claim 62QDs@MIPs, it is characterised in that: wanted by right
Seek molecularly imprinted polymer MoS described in 1-52The preparation method of QDs@MIPs is made.
10. a kind of described in any item novel molecular engram polymer MoS of claim 6-92QDs@MIPs is in antibiotic Ah meter
Application in card star content detection.
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