Development and validation of a method by Gas Chromatography for the determination of D002 in tablets

Abstract

An analytical method for determining D002 in 50 and 100 mg
tablets was developed and validated. This method can be used as part of
the quality control and stability studies of these finished pharmaceutical
forms. This method is based on the extraction of the active principle with
cloroform and the addition of 1-eicosanol as internal standard and N-methyl-
N-(trimethylsilil)triflouroacetamide as derivatizing agent. Silanized glass
packed column (3 m, with 3 mm de internal diameter) filled with 3 % OV
101 on Cromosorb W AW-DMCS was used for the analysis. It was proved
that in the studied mass rage (between 50 and 150 % of the nominal doses),
the method is linear, with a correlation coeficient of 0.999. Relative standard
deviation of response factors of 0,875 % and standard deviation of slope
of 0.137 % fullfilled too the aceptance criteria. Accuracy was assessed
through a recovery study, values were between 99.72 y 100.39 %, which were
not significantly different form 100 %. The repeatability (n = 10) and
intermediate precision (n = 6, for 4 d) were assessed from 80 a 120 % of the
nominal concentration, in all cases the method was precise, according to
variation coeficient (CV) < 2 %, no significant differences were found in
either the precision or the means obtained in the different days, according
Fisher F and Student t tests for p = 0.05.