Single Crystal FLIM Characterization of Clofazimine Loaded in Silica-Based Mesoporous Materials and Zeolites
Abstract
:1. Introduction
2. Results and Discussion
2.1. Steady-State Absorption and Diffuse Transmittance Spectra
2.2. CLZ Loading
2.3. Steady-State Emission Spectra
2.4. TCSPC Decays in DCM Suspensions
2.5. Solid State Scanning Confocal Fluorescence Microscopy
2.5.1. Single Particle Emission Spectra
2.5.2. TCSPC Decays of Solid Composites
3. Materials and Methods
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
Abbreviations
CLZ | Clofazimine |
TCSPC | Time-correlated single-photon counting |
FLIM | fluorescence lifetime imaging microscopy |
MSPs | Mesoporous silica particles |
DCM | Dichloromethane |
DTS | Diffuse transmittance spectra |
THF | Tetrahydrofuran |
τi | Time constant |
ai | Pre-exponential factor |
ci | Fractional contributions |
σ | Standard deviation |
IRF | Instrumental response function |
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Host Material | CLZ Loading (%) | CLZ Content Capacity (% w/w) | Pore Size (Å) | Pore Volume (cm3 g−1) | Ratio Si/Al |
---|---|---|---|---|---|
SBA-15 | >99% | 4 | 60 | 0.7–0.9 a | 0 |
MCM-41 | 81 | 3.1 | 25 | 0.98 b | 0 |
Al-MCM-41 | 84 | 3.3 | 25 | 1 b | 30 |
NaX | 40 | 1.6 | 13 | 0.29 c | 1.24 |
NaY | 51 | 1.2 | 13 | 0.34 c | 2.45 |
HY | 46 | 1.8 | 7.4 | 0.33 d | 2.47 |
Host Material | λ obs (nm) | τ1 (ns) 1 | a1 (%) | τ2 (ns) 1 | a2 (%) |
---|---|---|---|---|---|
SBA-15 | 525 | 0.1 | 89 | 1.4 | 11 |
550 | 0.1 | 93 | 1.6 | 7 | |
575 | 0.2 | 93 | 1.8 | 7 | |
600 | 0.2 | 91 | 1.5 | 9 | |
MCM-41 | 550 | 0.2 | 45 | 0.9 | 55 |
600 | 0.2 | 44 | 0.9 | 56 | |
650 | 0.2 | 46 | 0.9 | 54 | |
Al-MCM-41 | 550 | 0.2 | 60 | 1.1 | 40 |
600 | 0.3 | 57 | 1.1 | 43 | |
650 | 0.2 | 52 | 1.0 | 48 | |
NaX | 525 | 0.1 | 94 | 1.8 | 6 |
550 | 0.1 | 63 | 1.8 | 37 | |
575 | 0.1 | 64 | 1.7 | 36 | |
600 | 0.1 | 60 | 1.7 | 40 | |
NaY | 525 | 0.1 | 97 | 1.7 | 3 |
550 | 0.1 | 85 | 2.0 | 15 | |
575 | 0.1 | 88 | 1.9 | 12 | |
600 | 0.1 | 86 | 2.0 | 14 | |
HY | 525 | 0.4 | 50 | 2.2 | 50 |
550 | 0.3 | 49 | 2.2 | 51 | |
575 | 0.3 | 50 | 2.2 | 50 | |
600 | 0.2 | 55 | 2.2 | 45 |
Host Material | τ11 (ns) | a1 (%) | c1 (%) | τ22 (ns) | σ2 | a2 (%) | c2 (%) | τ32 (ns) | σ3 | a3 (%) | c3 (%) |
---|---|---|---|---|---|---|---|---|---|---|---|
SBA-15 | 0.1 | 45 | 9 | 0.6 | 0.08 | 49 | 58 | 2.6 | 0.32 | 6 | 33 |
MCM-41 | 0.1 | 45 | 7 | 0.7 | 0.09 | 46 | 50 | 3.2 | 0.57 | 8 | 43 |
Al-MCM-41 | 0.1 | 57 | 12 | 0.7 | 0.12 | 36 | 46 | 3.4 | 0.40 | 7 | 42 |
NaX | 0.1 | 63 | 16 | 0.6 | 0.07 | 33 | 52 | 3.1 | 0.37 | 4 | 32 |
NaY | 0.1 | 81 | 36 | 0.4 | 0.07 | 17 | 36 | 3.3 | 0.74 | 2 | 28 |
HY | 0.1 | 87 | 52 | 0.5 | 0.09 | 12 | 32 | 3.6 | 1.03 | 1 | 16 |
Host Material | τ11 (ns) | a1 (%) | c1 (%) | τ22 (ns) | σ2 | a2 (%) | c2 (%) | τ32 (ns) | σ3 | a3 (%) | c3 (%) |
---|---|---|---|---|---|---|---|---|---|---|---|
SBA-15 | 0.1 | 40 | 8 | 0.9 | 0.12 | 45 | 53 | 1.8 | 0.15 | 15 | 39 |
MCM-41 | 0.1 | 43 | 6 | 0.9 | 0.19 | 44 | 52 | 2.2 | 0.43 | 13 | 42 |
Al-MCM-41 | 0.1 | 41 | 9 | 0.8 | 0.17 | 51 | 65 | 2.0 | 0.67 | 8 | 26 |
NaX | 0.1 | 49 | 15 | 0.5 | 0.04 | 46 | 64 | 1.6 | 0.22 | 5 | 21 |
NaY | 0.1 | 47 | 16 | 0.4 | 0.03 | 50 | 72 | 1.3 | 0.38 | 3 | 12 |
HY | 0.1 | 46 | 18 | 0.4 | 0.02 | 52 | 76 | 1.3 | 0.30 | 2 | 6 |
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Angiolini, L.; Cohen, B.; Douhal, A. Single Crystal FLIM Characterization of Clofazimine Loaded in Silica-Based Mesoporous Materials and Zeolites. Int. J. Mol. Sci. 2019, 20, 2859. https://doi.org/10.3390/ijms20122859
Angiolini L, Cohen B, Douhal A. Single Crystal FLIM Characterization of Clofazimine Loaded in Silica-Based Mesoporous Materials and Zeolites. International Journal of Molecular Sciences. 2019; 20(12):2859. https://doi.org/10.3390/ijms20122859
Chicago/Turabian StyleAngiolini, Lorenzo, Boiko Cohen, and Abderrazzak Douhal. 2019. "Single Crystal FLIM Characterization of Clofazimine Loaded in Silica-Based Mesoporous Materials and Zeolites" International Journal of Molecular Sciences 20, no. 12: 2859. https://doi.org/10.3390/ijms20122859