Simultaneous quantification of an enantiomer and the racemic compound of ibuprofen by X-ray powder diffractometry

Neelima V. Phadnis, Raj Suryanarayanan

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16 Scopus citations

Abstract

Purpose. An X-ray powder diffractometric method was developed for the simultaneous quantification of the relative amounts of the racemic compound (±) of ibuprofen (I) and S(+)-ibuprofen (II), when they occur as a mixture. Method. The X-ray powder diffraction patterns of I and II show pronounced differences. This formed the basis for the determination of the relative amounts of I and II when they occur as a mixture. X-ray lines with d-spacings of 14.41 and 4.37 Å were unique to I and II, respectively. Mixtures containing different proportions of I and II were prepared which also contained lithium fluoride (III) as an internal standard. Results. A linear relationship was obtained when the intensity ratio (intensity of the 4.37 Å line of II/intensity of the 2.01 Å line of III) was plotted as a function of the weight fraction of II in the mixture. Similar results were obtained in the case of I. Using these standard curves, the weight fractions of I and II in 'unknown' mixtures were determined. The experimentally determined analyte concentration ranged between 98 and 104% of the true value. The relative error in the analyses of individual samples was <10%. The minimum detectable weight fraction of I in II and II in I were 0.032 (3.2% w/w) and 0.034 (3.4% w/w), respectively. The minimum quantifiable weight fractions were 0.136 for I and 0.112 for II. Since the X-ray diffraction patterns of S(+)-ibuprofen and R(-)-ibuprofen are identical, the conclusions drawn regarding mixtures of I and II will also hold true in the quantitative analyses of mixtures of I and R(-)-ibuprofen.

Original languageEnglish (US)
Pages (from-to)1176-1180
Number of pages5
JournalPharmaceutical research
Volume14
Issue number9
DOIs
StatePublished - Oct 21 1997

Keywords

  • (±)-ibuprofen
  • R(-)-ibuprofen
  • S(+)-ibuprofen
  • X-ray powder diffractometry

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