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. 2018 Apr;13(2):93-102.
doi: 10.4103/1735-5362.223775.

Synthesis, characterization, and stability study of desloratadine multicomponent crystal formation

Ahmad Ainurofiq  1   2 , Rachmat Mauludin  1 , Diky Mudhakir  1 , Sundani Nurono Soewandhi  1
Affiliations

Synthesis, characterization, and stability study of desloratadine multicomponent crystal formation

Ahmad Ainurofiq et al. Res Pharm Sci. 2018 Apr.

Abstract

This study describes the formation of multicomponent crystal (MCC) of desloratadine (DES). The objective of this study was to discover the new pharmaceutical MCC of DES using several coformers. The MCC synthesis was performed between DES and 26 coformers using an equimolar ratio with a solvent evaporation technique. The selection of the appropriate solvent was carried out using 12 solvents. The preview of the MCC of DES was performed using polarized light microscopy (PLM). The formation of MCC was confirmed using powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The accelerated stability of MCC at 40 °C and relative humidity of 75% was investigated using PXRD and FTIR. Depending on the prior evaluation, DES and benzoic acid (BA) formed the MCC. PLM and SEM results showed that crystal habit of combination between DES and BA differed from the constituent components. Moreover, the diffractogram pattern of DES-BA was distinct from the constituent components. The DSC thermogram showed a new peak which was distinct from both constituent components. The FTIR study proved a new spectrum. All characterizations indicated that a new solid crystal was formed, ensuring the MCC formation. In addition, DES-BA MCC had both chemical and physical stabilities for a period of 4 months.

Keywords: Characterization; Desloratadine; Multicomponent crystal; Stability.

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Figures

Scheme 1
Scheme 1
(a), Structure of desloratadine; (b) stereoview of zig-zag packing arrangement of two desloratadine chains (14).
Fig. 1
Fig. 1
Polarized light microscopic images of (a), desloratadine (DES); (b), benzoic acid (BA); and (c), mixture of DES:BA (1:1 mole ratio and after recrystallization using methanol as the solvent); (d), DES; (e), nicotinamide (NIC); and (f), mixture of DES:NIC (1:1 mol ratio and after recrystallization using acetone).
Fig. 2
Fig. 2
Diffractograms of desloratadine (DES); benzoic acid (BA); DES-BA; caffeine (CAF); DES-CAF; methionine (MET); DES-MET; glycine (GLY); DES-GLY; succinic acid (SA); and DES-SA.
Fig. 3
Fig. 3
Thermograms of desloratadine (DES), benzoic acid (BA), DES-BA, succinic acid (SA), and DES-SA.
Fig. 4
Fig. 4
FTIR spectra of desloratadine (DES), benzoic acid (BA), and DES-BA multicomponent crystal.
Fig. 5
Fig. 5
SEM photographs of (a), desloratadine (DES); (b), benzoic acid (BA); and (c), DES-BA multicomponent crystal.
Fig. 6
Fig. 6
Diffractograms of desloratadine-benzoic acid multicomponent crystal (a), before and (b), after the stability testing.
Fig. 7
Fig. 7
FTIR spectra of desloratadine-benzoic acid multicomponent crystal (a), before and (b), after the stability testing.
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