Identificación por Cromatografía de Gases - Espectrometría de Masas y determinación cuantitativa por Cromatografía de Gases de los productos de degradación térmica de las tabletas de policosanol (20 mg) revestidas

Abstract

Identification of hexacosanyl, octacosanyl, and triacontanyl
stearates and palmitates as main thermal degradation products of policosanol
in film-coated tablets containing 20 mg of this active ingredient was achieved
by Gas Chromatography-Mass Spectrometry. In order to quantify these
degradation products, a Gas Chromatographic method with flame ionisation
detector, and docosanyl stearate as internal standard was developed and
validated. In this method it was used a BPX-5 wide-bore capillary column (25 m
X 0.53 mm d.i. X 1.0 µm of film thickness) in a temperature program from 300
to 350 °C . Validation of the method showed that it is accurate and linear in a
range from 2.5 to 30 % of degradation. Precision studies of this method:
repeatability and intermediate precision, assayed with tablets degraded in a
7.2 %, showed coefficients of variation lower than 2 %. Determined limits of
detection and quantification (0.006 and 0.022 mg, respectively), determined
for hexacosanyl palmitate, one of the minority degradation products, prove
that the method can be used even for tablets with less than 2 % of degradation.
Good accuracy and precision were obtained when tablets spiked with
concentrations of hexacosanyl palmitate that correspond to the quantification
limit were analyzed. The method is suitable in support of stability studies of
these tablets.