Norcantharidin/layered double hydroxide nano hybrid and preparation method thereof
A technology of norcanthin and nano-hybrids, which is applied in the direction of active ingredients of heterocyclic compounds, pharmaceutical formulations, drug combinations, etc., can solve the problems of ordinary preparations such as ineffective treatment, high toxicity, and skin irritation, and achieve good results. Sustained release effect, reduction of toxic and side effects, mild reaction effect
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Embodiment 1
[0030] Step a: 2.44g (0.012mol) MgCl 2 ·6H 2 O and 1.45g (0.006mol) AlCl 3 9H 2 O was dissolved in 36 mL of deionized water.
[0031] Step b: 1.01 g (0.006 mol) of solid norcantochelin was dissolved in 42 mL of NaOH solution with a concentration of 1 mol / L.
[0032] Step c: Add the solution of step b to the solution of step a, stir, control the pH to 9, and the reaction temperature to 65°C; then age the obtained slurry at 65°C for 3 hours, filter, wash with water until neutral, and age at 80°C After 24 hours, the norcanthin / LDHs nano-hybrid product was obtained; after drying, the powder product was obtained.
[0033] By XRD spectrum ( figure 1 a) It can be seen that the norcanthin / LDHs nano-hybrid has a layered crystal structure, and the interlayer spacing (d 003 ) shows that norcanthin has been inserted into the interlayer of LDHs.
[0034] From the IR spectrum ( figure 2 b) It was further confirmed that norcanchelin had intercalated into the interlayer.
[0035] Th...
Embodiment 2
[0038] Step a: 2.44g (0.012mol) MgCl 2 ·6H 2 O and 1.45g (0.006mol) AlCl 3 9H 2 O was dissolved in 36 mL of deionized water.
[0039] Step b: 2.02 g (0.012 mol) of solid norcantochelin was dissolved in 42 mL of NaOH solution with a concentration of 1 mol / L.
[0040] Step c: Add the solution of step b to the solution of step a, stir, control the pH to 9.5, and the reaction temperature to 65°C; then age the obtained slurry at 65°C for 6 hours, filter, wash with water until neutral, and age at 80°C After 28 hours, the norcanthin / LDHs nano-hybrid product was obtained; after drying, the powder product was obtained.
[0041] By XRD spectrum ( figure 1 b) shows that the norcanthin / LDHs nano-hybrid has a layered crystal structure, and the interlayer spacing (d 003 ) shows that norcanthin has been inserted into the interlayer.
[0042] From the IR spectrum ( figure 2 c) It was further confirmed that norcantochelin had intercalated into the interlayer.
[0043] For the results...
Embodiment 3
[0046] Step a: 2.44g (0.012mol) MgCl 2 ·6H 2 O and 1.45g (0.006mol) AlCl 3 9H 2 O was dissolved in 36 mL of deionized water.
[0047] Step b: 5.04 g (0.018 mol) of solid norcantharin was dissolved in 50 mL of NaOH solution with a concentration of 1 mol / L.
[0048] Step c: Add the solution of step b to the solution of step a, stir, control the pH to 9.5, and the reaction temperature to 70°C; then age the obtained slurry at 70°C for 3 hours, filter, wash with water until neutral, and age at 80°C After 26 hours, the norcanthin / LDHs nano-hybrid product was obtained; after drying, the powder product was obtained.
[0049] By XRD spectrum ( figure 1 c) It can be seen that the norcantochelin / LDHs nano-hybrid has a layered crystal structure, and from the interlayer distance (d003), it can be known that norcantochelin has been inserted into the interlayer of LDHs.
[0050] The sample was analyzed by ultraviolet spectrophotometry, and the content of norcantharin was determined to ...
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