Abstract
Ethylcellulose microspheres containing tolnaftate (I) were prepared by the emulsion-solvent evaporation technique. An X-ray powder diffractometric method was developed to quantify the content of crystalline I in these microspheres. X-ray lines of I with d-spacings of 5.5 and 4.2 Å were chosen for the quantitative analyses. Physical mixtures containing various weight fractions of I and blank (empty) microspheres were prepared and lithium fluoride (20% w/w) was added as the internal standard. The 5.5 and 4.3 Å lines of I and the 2.3 Å line of lithium fluoride were used for the quantitative analysis. A plot of the intensity ratio (intensity of the 5.5 Å line of I/intensity of 2.3 Å line of lithium fluoride) as a function of the weight percent of I in the mixture, resulted in a straight line. The crystalline content of I in the tolnaftate-loaded microspheres was determined using this standard curve. A second independent determination of the content of I was possible from the intensities of the 4.3 Å line. The enthalpy of fusion of I, determined by differential scanning calorimetry (DSC), was also used as a measure of the crystalline content of I in the microspheres. The X-ray and DSC methods measure the content of crystalline I in the microspheres at room temperature (∼25°C) and at the melting point of I (111°C), respectively. The total content of I in the microspheres was determined by HPLC. The DSC and X-ray results indicated that a substantial fraction of the incorporated I was dissolved in the ethylcellulose matrix.
Original language | English (US) |
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Pages (from-to) | 983-990 |
Number of pages | 8 |
Journal | Journal of Pharmaceutical Sciences |
Volume | 91 |
Issue number | 4 |
DOIs | |
State | Published - 2002 |
Bibliographical note
Funding Information:This work was supported by AAPS, Health Future Foundation, and PhRMA Foundation. We thank Mr. Rahul Surana for his numerous contributions and Ms. Smita Debnath for her helpful comments.
Copyright:
Copyright 2017 Elsevier B.V., All rights reserved.
Keywords
- DSC
- HPLC
- Microspheres
- Solubility
- Tolnaftate
- X-ray powder diffractometry