6
5. The resulting solution at a molar ratio of 1:2 (IRB:2-HP-β-CD)
(see Notes 4–6) is thereafter frozen at −80 °C and freeze-dried
[15] to remove the water and obtain the white solid irbesartan–
2-HP-β-CD lyophilized product (see Note 7).
1. Accurately weigh 3445.6 mg of 2-HP-β-CD.
2. Transfer in a glass vessel with 300 mL of purified water and set
under magnetic stirring.
3. When the cyclodextrin is completely dissolved, add 500 mg of
LOS potassium (accurately weighed) in the vessel and continue
the magnetic stirring (LOS:CD molar ratio 1:2, see Notes 4–6).
4. Adjust the pH at approximately 10.5 with ammonium hydroxide solution 5% v/v to facilitate the reaction of inclusion complex formation (see Notes 1–3).
5. When the mixture turns to a clear and colorless solution, fix the
final volume at 500 mL with purified water.
6. Immediately freeze the solution at −80 °C for lyophilization to
follow and obtain the white solid LOS-2-HP-β-CD inclusion
complex (see Note 7).
1. Accurately weigh 30 mg of CAN or CC and 198.85 mg or
143.37 mg of 2-HP-β-CD, respectively.
2. Mix the weighed amounts of CAN (or CC) and 2-HP-β-CD in
a glass beaker along with 20 mL of purified water.
3. Add small amounts of the ammonium hydroxide solution 5%
v/v under continuous magnetic stirring.
4. Adjust pH at approximately 10.5 (see Notes 1–3).
5. Adjust the final volume at 30 mL with purified water and mix
thoroughly.
6. Freeze the resulting solution immediately after preparation at
−80 °C (see Note 7).
7. Freeze-dry the iced preparation in a lyophilizer (e.g., Kryodos- 50
model Telstar) to obtain a white amorphous solid.
1. Weigh accurately 60 mg of CA and 0.964 g of 2-HP-β-CD.
2. Transfer the weighed amounts of CA and 2-HP-β-CD in a
100 mL beaker and suspend with 50 mL of water.
3. Add small amounts of ammonium hydroxide 5% v/v aqueous
solution and adjust the pH at approximately 9–10 under magnetic stirring (see Notes 1–3).
4. Continue magnetic stirring under pH monitoring until a clear
solution is obtained.
5. Fix the final volume at 60 mL with purified water.
3.2 Steps to Follow
for the Preparation
of Solid-State LOS–2HP- β-CD Inclusion
Complex
3.3 Steps to Follow
for the Preparation
of Solid-State CAN–2HP- β-CD and CC–2HP- β-CD Inclusion
Complexes [27]
3.4 Steps to Follow
for the Preparation
of Solid-State RA–2HP- β-CD and CA–2HP- β-CD Inclusion
Complexes
3.4.1 CA–2-HP-b-CD
Inclusion Complex
Eirini Christodoulou et al.
5. The resulting solution at a molar ratio of 1:2 (IRB:2-HP-β-CD)
(see Notes 4–6) is thereafter frozen at −80 °C and freeze-dried
[15] to remove the water and obtain the white solid irbesartan–
2-HP-β-CD lyophilized product (see Note 7).
1. Accurately weigh 3445.6 mg of 2-HP-β-CD.
2. Transfer in a glass vessel with 300 mL of purified water and set
under magnetic stirring.
3. When the cyclodextrin is completely dissolved, add 500 mg of
LOS potassium (accurately weighed) in the vessel and continue
the magnetic stirring (LOS:CD molar ratio 1:2, see Notes 4–6).
4. Adjust the pH at approximately 10.5 with ammonium hydroxide solution 5% v/v to facilitate the reaction of inclusion complex formation (see Notes 1–3).
5. When the mixture turns to a clear and colorless solution, fix the
final volume at 500 mL with purified water.
6. Immediately freeze the solution at −80 °C for lyophilization to
follow and obtain the white solid LOS-2-HP-β-CD inclusion
complex (see Note 7).
1. Accurately weigh 30 mg of CAN or CC and 198.85 mg or
143.37 mg of 2-HP-β-CD, respectively.
2. Mix the weighed amounts of CAN (or CC) and 2-HP-β-CD in
a glass beaker along with 20 mL of purified water.
3. Add small amounts of the ammonium hydroxide solution 5%
v/v under continuous magnetic stirring.
4. Adjust pH at approximately 10.5 (see Notes 1–3).
5. Adjust the final volume at 30 mL with purified water and mix
thoroughly.
6. Freeze the resulting solution immediately after preparation at
−80 °C (see Note 7).
7. Freeze-dry the iced preparation in a lyophilizer (e.g., Kryodos- 50
model Telstar) to obtain a white amorphous solid.
1. Weigh accurately 60 mg of CA and 0.964 g of 2-HP-β-CD.
2. Transfer the weighed amounts of CA and 2-HP-β-CD in a
100 mL beaker and suspend with 50 mL of water.
3. Add small amounts of ammonium hydroxide 5% v/v aqueous
solution and adjust the pH at approximately 9–10 under magnetic stirring (see Notes 1–3).
4. Continue magnetic stirring under pH monitoring until a clear
solution is obtained.
5. Fix the final volume at 60 mL with purified water.
3.2 Steps to Follow
for the Preparation
of Solid-State LOS–2HP- β-CD Inclusion
Complex
3.3 Steps to Follow
for the Preparation
of Solid-State CAN–2HP- β-CD and CC–2HP- β-CD Inclusion
Complexes [27]
3.4 Steps to Follow
for the Preparation
of Solid-State RA–2HP- β-CD and CA–2HP- β-CD Inclusion
Complexes
3.4.1 CA–2-HP-b-CD
Inclusion Complex
Eirini Christodoulou et al.