Does alteration of crystal habit affects any drug properties??

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- K.LOHITHA
PA/2016/106

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 ROFECOXIB
 4-[4-(Methyl sulfonyl)phenyl(-3-phenyl-2(5H)-furanone]
 NSAID
 Active at low dose
 Less gastric toxicity
 inhibits COX enzymes involved in synthesis of PG’s
 Gift sample from Ipca Laboratories Ltd.,Mumbai
 CELECOXIB
 4-[5-(4-Methylphenyl)-3-(9trifluoromethyl]-1H-pyrazole-1-yl]benzene sulfonamide
 NSAID
 Gift sample from Aarti Drugs, Mumbai

4. PREPARATION OF CRYSTALS
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RESULTS AND DISCUSSION
Solvent used Melting point
Commercial
sample
203°c
Ethyl acetate 183°c
methanol 180°c
acetone 185°c
ethanol 184°c
IPA 178°c
Solvent used Melting point
Commercial
sample
169°c
ethanol 134°c
methanol 130°c
acetone 128°c
ROFECOXIB CELECOXIB
☻ primary indication of polymorphs
☻Polymorphic transitions -

6. FT-IR Spectroscopic analysis
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Celecoxib – FT-IR analysis

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X-ray diffractionROFECOXIB CELECOXIB

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DSC analysis
Rofecoxib
Celecoxib

10. SEM analysis10
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SOLUBILITY
BEHAVIOUR
DISSOLUTION
BEHAVIOUR
Rofecoxib –IPA>ethylacetate>acetone>methanol>cs>ethanol
Celecoxib – acetone>methanol>ethanol>cs

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 Melting points of rofecoxib & celecoxib crystals obtained from different solvents
were different, providing the prima facie evidence for differences in crystal habit or
polymorphism.
 FT-IR & XRD data provided further evidence for polymorphism.
 Crystals obtained from solvents (of different polarities) showed different crystal
habits and dissolution patterns. Hence IPA & Acetone – best solvents
 Moreover, DSC concluded that there was no occurrence of polymorphism in the
obtained

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