Validation of a gas chromatographic method for determining fatty acids that compose D003 in 10 mg film-coated tablets

Farmaco. 2004 Jul;59(7):543-7. doi: 10.1016/j.farmac.2003.11.020.

Abstract

D003 is a new product composed of a mixture of aliphatic fatty acids (C(24:0) to C(36:0)), which shows antiplatelet, antithrombotic, antioxidant, and cholesterol-lowering effects in experimental models and human beings. A gas chromatographic method using a DB-5 wide-bore column and 1-nonadecanoic acid as internal standard was developed and validated in order to determine D003 in 10 mg film-coated tablets. The acids were analysed as methyl esters derivatives, prepared using 5% aqueous HCl-methanol. Developed method was specific for the active principle, even when samples were subjected to stress conditions. Good linearity (correlation coefficient > 0.99) and accuracy (total average recovery = 100.29%) were proven over a range 50-150% of the nominal concentration. Within-day and intermediate precisions at the nominal dose (100%) were < 1.5%. Robustness was examined through an intralaboratory study, quantification and resolution were only affected by the injection volume increase and no other of the 7 operational changes evaluated affected the results. The method was suitable for quality control and stability studies of these tablets.

MeSH terms

  • Animals
  • Anticholesteremic Agents / analysis*
  • Anticholesteremic Agents / chemistry
  • Chromatography, Gas / methods*
  • Chromatography, Gas / standards
  • Drug Stability
  • Fatty Acids / analysis*
  • Fatty Acids / chemistry
  • Humans
  • Quality Control
  • Reproducibility of Results
  • Tablets, Enteric-Coated / analysis*
  • Tablets, Enteric-Coated / chemistry

Substances

  • Anticholesteremic Agents
  • D003 preparation
  • Fatty Acids
  • Tablets, Enteric-Coated