320
1. The peaks of 2-HP-β-CD are barely observable. The absence of
cross polarization between 2-HP-β-CD and phospholipid
DPPC presumably shows that the former molecule approaches
the surface of the lipid bilayers and that the distances between
the
1
H and
13
C nuclei of the two species are thus sufficiently
large or that the dynamics of the 2-HP-β-CD is sufficiently fast,
so that the
1
H–
13
C (residual) dipolar interaction is practically
negligible.
13
C MAS experiments lead to the conclusion that
this preposition as the peaks attributed to 2-HP-β-CD is eminent at low temperatures.
2. The presence of the drug in the lipid bilayers does not modify
significantly DPPC’s carbon chemical shifts.
4.2 Notes Related
to Subheading 3.2
(Figs. 4 and 5)
Table 1
Chemical shifts of irbesartan alone or complexed with 2-HP-β-CD in D 2 O and in SDS micelles
Hydrogen
atoms
IRB in D 2 O [ppm
(multiplicity)]
IRB in SDS
micelles [ppm
(multiplicity)]
Complex IRB-2-HPβ-CD in D2O [ppm
(multiplicity)]
Complex IRB-2-HPβ-CD in SDS micelles
[ppm (multiplicity)]
31
0.78 (triplet)
0.84 (triplet)
0.76 (triplet)
0.86 (triplet)
30
1.25 (sextet)
1.32 (sextet)
1.23 (sextet)
1.32 (sextet)
29
1.43 (pentet)
1.52 (pentet)
1.41 (pentet)
1.54 (pentet)
6a, 6b
9a, 9b
1.82
1.93–1.99
(multiplet and
multiplet)
1.91
1.97–2.01
(multiplet and
multiplet)
1.91–1.96
(multiplet and
multiplet)
1.97
(multiplet and
multiplet)
7a,7b
1.93–1.99
(multiplet)
1.91, 2.03–2.06
(multiplet)
1.77–2.02 (multiplet) 1.80, 1.98 (multiplet)
8a, 8b
1.93–1.99
(multiplet)
2.03–2.06
(multiplet)
1.77–2.02 (multiplet) 1.80, 1.98 (multiplet)
28
2.43 (triplet)
2.56 (triplet)
2.37 (triplet)
2.45 (triplet)
10
4.78 (singlet)
4.84 (triplet)
4.76 (singlet)
4.77 (singlet)
12/16
7.10 (doublet)
7.10 (doublet)
7.09 or 7.14
(doublet)
7.12 or 7.13 (doublet)
13/15
7.10 (doublet)
7.16 (doublet)
7.09, or 7.14
(doublet)
7.12 or 7.13 (doublet)
22
7.53–7.55
(multiplet)
7.41 (doublet)
7.48 (multiplet)
7.39 (doublet)
20
7.53–7.55
(multiplet)
7.52 (triplet)
7.49 (multiplet)
7.46 (triplet)
19
7.59 (doublet)
7.84 (doublet)
7.62 (doublet)
7.78 (doublet)
21
7.61 (triplet)
7.57 (triplet)
7.57 (triplet)
7.53 (triplet)
Dimitrios Ntountaniotis et al.
1. The peaks of 2-HP-β-CD are barely observable. The absence of
cross polarization between 2-HP-β-CD and phospholipid
DPPC presumably shows that the former molecule approaches
the surface of the lipid bilayers and that the distances between
the
1
H and
13
C nuclei of the two species are thus sufficiently
large or that the dynamics of the 2-HP-β-CD is sufficiently fast,
so that the
1
H–
13
C (residual) dipolar interaction is practically
negligible.
13
C MAS experiments lead to the conclusion that
this preposition as the peaks attributed to 2-HP-β-CD is eminent at low temperatures.
2. The presence of the drug in the lipid bilayers does not modify
significantly DPPC’s carbon chemical shifts.
4.2 Notes Related
to Subheading 3.2
(Figs. 4 and 5)
Table 1
Chemical shifts of irbesartan alone or complexed with 2-HP-β-CD in D 2 O and in SDS micelles
Hydrogen
atoms
IRB in D 2 O [ppm
(multiplicity)]
IRB in SDS
micelles [ppm
(multiplicity)]
Complex IRB-2-HPβ-CD in D2O [ppm
(multiplicity)]
Complex IRB-2-HPβ-CD in SDS micelles
[ppm (multiplicity)]
31
0.78 (triplet)
0.84 (triplet)
0.76 (triplet)
0.86 (triplet)
30
1.25 (sextet)
1.32 (sextet)
1.23 (sextet)
1.32 (sextet)
29
1.43 (pentet)
1.52 (pentet)
1.41 (pentet)
1.54 (pentet)
6a, 6b
9a, 9b
1.82
1.93–1.99
(multiplet and
multiplet)
1.91
1.97–2.01
(multiplet and
multiplet)
1.91–1.96
(multiplet and
multiplet)
1.97
(multiplet and
multiplet)
7a,7b
1.93–1.99
(multiplet)
1.91, 2.03–2.06
(multiplet)
1.77–2.02 (multiplet) 1.80, 1.98 (multiplet)
8a, 8b
1.93–1.99
(multiplet)
2.03–2.06
(multiplet)
1.77–2.02 (multiplet) 1.80, 1.98 (multiplet)
28
2.43 (triplet)
2.56 (triplet)
2.37 (triplet)
2.45 (triplet)
10
4.78 (singlet)
4.84 (triplet)
4.76 (singlet)
4.77 (singlet)
12/16
7.10 (doublet)
7.10 (doublet)
7.09 or 7.14
(doublet)
7.12 or 7.13 (doublet)
13/15
7.10 (doublet)
7.16 (doublet)
7.09, or 7.14
(doublet)
7.12 or 7.13 (doublet)
22
7.53–7.55
(multiplet)
7.41 (doublet)
7.48 (multiplet)
7.39 (doublet)
20
7.53–7.55
(multiplet)
7.52 (triplet)
7.49 (multiplet)
7.46 (triplet)
19
7.59 (doublet)
7.84 (doublet)
7.62 (doublet)
7.78 (doublet)
21
7.61 (triplet)
7.57 (triplet)
7.57 (triplet)
7.53 (triplet)
Dimitrios Ntountaniotis et al.