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β-cyclodextrin derivative and its preparation method, preparation method and application of β-cyclodextrin derivative-gold nanocomposite material
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A composite material and cyclodextrin technology, applied in the preparation of beta-cyclodextrin derivatives-gold nanocomposite materials, beta-cyclodextrin derivatives and their preparation fields, can solve the problem of high detection limit and low concentration. Problems such as the inability of accurate detection in the field
Inactive Publication Date: 2021-09-14
XIAN UNVERSITY OF ARTS & SCI
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So far, the composite materials of cyclodextrin and gold nanoparticles are only limited to natural cyclodextrin. When used for the detection of tetracycline and other antibiotics, the detection limit is high, and it is impossible to accurately detect low concentration areas.
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Embodiment 1
[0031] A kind of β-cyclodextrin derivative, described β-cyclodextrin derivative is 3-succinic acid monoamide-β-cyclodextrin, and its structural formula is as follows:
[0032] ;
[0033] The preparation method of the β-cyclodextrin derivative, the preparation method is:
[0034] 1.0 mmol 3-NH 2 - Mix β-cyclodextrin and 1.1 mmol succinic anhydride, add to 30 mL DMF, react at room temperature for 12 hours, then concentrate under reduced pressure at 60°C to a constant volume, that is, concentrate under reduced pressure to a constant volume, then add excess acetone, and The separated precipitate was filtered and dried in vacuum at 50°C for 5 hours;
[0035] The reaction equation is as follows:
[0036] .
Embodiment 2
[0038] The β-cyclodextrin derivatives described in Example 1 can also be prepared by the following method: 1.0 mmol 3-NH 2 - Mix β-cyclodextrin and 2 mmol succinic anhydride, add to 30 mL DMF, react at room temperature for 12 hours, then concentrate under reduced pressure at 60°C to a constant volume, that is, concentrate under reduced pressure until the volume remains constant, and then add excess acetone to precipitate The precipitate was filtered and dried under vacuum at 60 °C for 4 h.
[0039] The β-cyclodextrin derivatives prepared in Example 1 were respectively used for protonnuclear magnetic resonance spectrum and mass spectrum, and the results are shown in figure 1 and figure 2 ;Depend on figure 1 It can be seen that 1 H NMR (400 MHz, D2O) δ= 8.03-7.33 (m, 4H), 5.07-4.70 (m,7H), 4.11-3.26 (m, 42H); by figure 2 It can be seen that the mass spectrum (ESI) molecular formula C 42 h 75 NO 37 , m / z calculated value 1233.40[M-H] - , measured value 1233.51 [M-H] -...
Embodiment 3
[0042]The preparation method of β-cyclodextrin derivative-gold nanocomposites: clean the utensils used for the reaction, and add 1 mL, 0.01 MHAuCl 4 solution and 10 mL, 0.01M β-cyclodextrin derivative solution, react at 100°C until the solution turns from purple red to wine red, stop heating and stirring, and then cool naturally to room temperature, then at 12000 rpm Centrifuge for 10 min, and wash the precipitate obtained by centrifugation; wherein, the β-cyclodextrin derivative is prepared by the preparation method of Example 1.
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technical field [0001] The invention belongs to the technical field of beta-cyclodextrin modification, and specifically relates to a beta-cyclodextrin derivative and a preparation method thereof, a preparation method of a beta-cyclodextrin derivative-gold nanocomposite material and an application thereof. Background technique [0002] Residues of pharmaceutical and personal care products (PPCPs) in environmental water bodies are the focus of attention in the current environmental field. Antibiotics are one of the most common PPCPs, especially tetracyclines (TCs), which are cheap and one of the most widely used drugs at present. Their long-term, large and continuous discharge leads to Environmental pollution and ecological risks are very serious. At present, common antibiotic analysis methods mainly include gas chromatography, liquid chromatography and its combination technology, electrochemical analysis method and enzyme-linked immunosorbent method, etc. Chromatography and...
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