FORCED DEGRADATION OF FERULIC ACID: DEVELOPMENT AND VALIDATION OF THE INDICATIVE METHOD OF STABILITY BY UHPLC-DAD
Ferulic Acid. UHPLC-DAD. Forced Degradation Products. Experimental
design. Cosmetic formulations.
Ferulic acid (FA) is a phenolic acid widely distributed in the plant kingdom and
deriving from the secondary metabolism of these. It is formed from the metabolism
of amino acids phenylalanine and tyrosine in vegetables, being abundant and
found in whole grains, spinach, parsley, grapes and rhubarb. This study is due to
the wide pharmacological applicability of FA and its extremely high antioxidant
potential. Some tests and studies are required by international and national
regulatory bodies, including the research of forced degradation products. The
objective of this research was to identify and characterize FA degradation products
and to develop a UHPLC-DAD method capable of quantifying impurities and
degradation products efficiently in raw materials, formulations and other
pharmaceutical forms. In this study, indicative stability studies were performed,
which include: forced hydrolysis, oxidation and photostability in solution and solid,
which were identified and quantified by a UHPLC-DAD method. The results
obtained are very promising. What calls most attention is the stability of the active
hydrolysis and the very strong light instability when in solution, having degradation
from the first 5 min. The optimization of the method developed by UHPL-DAD was
done using a factorial planning tool. Response-surface and Pareto graphs
revealed the variables with the greatest influence on all dependent variables, the
concentration of acetonitrile in the mobile phase and the flow. The best method to
identify the AF and impurity with good resolution and selectivity was: mobile
phase, water acidified to 2% acetic acid: acetonitrile (88:12), flow rate of 0.25 mL /
min, oven temperature 30ºC. The final concentration of the sample was 25 ppm
and detection was performed at 322 nm. The fast method was developed with
analysis time less than 5 min. Factorial planning proved to be a very important tool
for the rational and optimized development of the method.