19
10. Bubble gaseous HCl for 30 s in the dispersion of the BOCmodified CNHs (see Note 6).
11. Stir the reaction mixture under an inert atmosphere of nitrogen for 12 h.
12. Evaporate the solvent under reduced pressure (see Note 7).
13. Add fresh dichloromethane (10 mL), and filter the mixture
over a PTFE membrane filter with pore size of 0.2 μm.
14. Wash the solid residue obtained on top of the PTFE filter with
DMF and dichloromethane (50 mL).
15. Recover the amine-modified CNHs as powder and store it at
room temperature in the dark.
1. Treat pristine CNHs (50 mg) with molecular oxygen at
0.1 MPa for 10 min at 580° C.
2. Transfer the oxidized CNHs in a round-bottom flask and add
30% w/w solution of H 2 O 2 (60 mL).
3. Apply light irradiation and heat the reaction mixture at 120° C
for 3 h (see Note 8).
4. Filter the dispersion of the CNHs through a PTFE membrane
filter with pore size of 0.2 μm.
5. Wash the solid residue obtained on top of the PTFE filter with
a large amount of deionized water and methanol (50 mL).
6. Recover the carboxylic acid-modified CNHs as powder and
store it at room temperature in the dark.
1. Treat the carboxylic acid-modified CNHs (50 mg) with thionyl chloride, SOCl 2 (50 mL), at 70° C for 8 h under nitrogen
atmosphere (see Note 9).
2. Evaporate the SOCl 2 under reduced pressure. Then, add dry
THF (20 mL), bath-sonicate the mixture for 5 min, and then
evaporate the solvent to dryness. Repeat the latter twice and
keep the dry solid residue (acyl chloride-modified CNHs)
under nitrogen atmosphere (see Note 10).
3. Add dry THF (10 mL) to the acyl chloride-modified CNHs
and keep it under nitrogen atmosphere. Dissolve the hydroxylor amino-terminated drug/biomolecule (100 mg) in dry
THF (20 mL) and add dropwise to the dispersion of the acyl
chloride- modified CNHs. Stir all the mixture at room temperature for 24 h.
4. Filter the dispersion of the drug/biomolecule-functionalized
CNHs through a PTFE membrane filter with pore size of
0.2 μm.
3.4 Incorporation
of Carboxylic Acid
Moieties on CNHs
3.5 Conjugation
of Drugs/Biomolecules
on Pre-modified CNHs
Functionalized Carbon Nanohorns
10. Bubble gaseous HCl for 30 s in the dispersion of the BOCmodified CNHs (see Note 6).
11. Stir the reaction mixture under an inert atmosphere of nitrogen for 12 h.
12. Evaporate the solvent under reduced pressure (see Note 7).
13. Add fresh dichloromethane (10 mL), and filter the mixture
over a PTFE membrane filter with pore size of 0.2 μm.
14. Wash the solid residue obtained on top of the PTFE filter with
DMF and dichloromethane (50 mL).
15. Recover the amine-modified CNHs as powder and store it at
room temperature in the dark.
1. Treat pristine CNHs (50 mg) with molecular oxygen at
0.1 MPa for 10 min at 580° C.
2. Transfer the oxidized CNHs in a round-bottom flask and add
30% w/w solution of H 2 O 2 (60 mL).
3. Apply light irradiation and heat the reaction mixture at 120° C
for 3 h (see Note 8).
4. Filter the dispersion of the CNHs through a PTFE membrane
filter with pore size of 0.2 μm.
5. Wash the solid residue obtained on top of the PTFE filter with
a large amount of deionized water and methanol (50 mL).
6. Recover the carboxylic acid-modified CNHs as powder and
store it at room temperature in the dark.
1. Treat the carboxylic acid-modified CNHs (50 mg) with thionyl chloride, SOCl 2 (50 mL), at 70° C for 8 h under nitrogen
atmosphere (see Note 9).
2. Evaporate the SOCl 2 under reduced pressure. Then, add dry
THF (20 mL), bath-sonicate the mixture for 5 min, and then
evaporate the solvent to dryness. Repeat the latter twice and
keep the dry solid residue (acyl chloride-modified CNHs)
under nitrogen atmosphere (see Note 10).
3. Add dry THF (10 mL) to the acyl chloride-modified CNHs
and keep it under nitrogen atmosphere. Dissolve the hydroxylor amino-terminated drug/biomolecule (100 mg) in dry
THF (20 mL) and add dropwise to the dispersion of the acyl
chloride- modified CNHs. Stir all the mixture at room temperature for 24 h.
4. Filter the dispersion of the drug/biomolecule-functionalized
CNHs through a PTFE membrane filter with pore size of
0.2 μm.
3.4 Incorporation
of Carboxylic Acid
Moieties on CNHs
3.5 Conjugation
of Drugs/Biomolecules
on Pre-modified CNHs
Functionalized Carbon Nanohorns