Propylene carbonate quantification by its derivative 3,5-diacetyl-1,4-dihydro-2,6-lutidine

Talanta. 2016 May 1:151:75-82. doi: 10.1016/j.talanta.2016.01.022. Epub 2016 Jan 13.

Abstract

Propylene carbonate (PC) is a non-toxic solvent currently used in various pharmaceutical formulations. Consequently, a simple, cost-effective and most accurate analytical method for the quantification of this optical inert solvent is of major interest. Based on a consecutive three-step reaction 3,5-diacetyl-1,4-dihydro-2,6-lutidine was obtained from PC and used for quantification by either UV and fluorescent detection. Data were compared with results from LC-ESI-MS as a reference method. After using Mandel's test for linearity assessment of the calibration curves, linear fitting was used for LC-ESI-MS and spectrofluorimetry, while a polynomial 3rd order curve fitting was used for spectrophotometry. High intra- and inter-day precision as well as high accuracy were confirmed for all three analytical methods (spectrophotometry, spectrofluorimetry and LC-ESI-MS). The comparison of all three methods was assessed using correlation coefficients and Bland-Altman plots, both showing satisfying results with a high degree of agreement. The new method confirmed its applicability for PC quantification in two formulations, namely a PC-enriched cream and polyester microimplants. This new quantification method for PC is a reliable alternative to highly sophisticated chromatographic methods.

Keywords: Dihydropyridine condensation; LC-ESI-MS; Propylene carbonate; Residual solvent quantification.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Calibration
  • Chromatography, Liquid
  • Diacetyl / chemistry*
  • Hydrogen-Ion Concentration
  • Mass Spectrometry
  • Models, Chemical
  • Molecular Structure
  • Propane / analogs & derivatives*
  • Propane / analysis
  • Propane / chemistry
  • Pyridines / chemistry*
  • Reproducibility of Results
  • Spectrometry, Fluorescence
  • Temperature

Substances

  • Pyridines
  • 2,6-lutidine
  • propylene carbonate
  • Diacetyl
  • Propane