Development and validation of a GC-FID assay for determination of fluvastatin in pharmaceutical preparations

Abstract

Recebido em 1/12/08; aceito em 24/5/09; publicado na web em 30/10/09 A gas chromatographic method has been developed for the assay of fluvastatin sodium (FLU). FLU was silylated with N,Obis(trimethylsilyl)trifluoroacetamide-1% trimethylchlorosilane at 90 ºC for 30 min and analysed in a DB-1 column by capillary gas chromatograph with a flame ionization detector. The method was validated. The assay was linear over the concentration range at 10.0 to 50.0 mg mL -1. The limit of detection and the limit of quantitation were 1.0 and 3.0 mg mL -1 , respectively. The recoveries of FLU derivatives were in the range of 99.25-99.80%. In inter-day and intra-day analysis, the values of relative standard deviation (%) and the relative mean error (%) were found between 0.20-0.80% and -0.20-0.75%, respectively. The developed method was succesfully applied to analyze the FLU content in tablet formulation. The results were statistically compared with those obtained by the official method, and no significant difference was found between the two methods. Therefore, it can be recommended for the quality control assay of FLU in pharmaceutical industry.

Determination of Ethanol in Vinegar and Beverage by Gas Chromatography: A Validated Method for Halal Verification

“…The results of this validation have been tested to determine the ethanol content in vinegar containing 1.17x10 -2 -2.28x10 -2 % v/v ethanol [13]. Validation of the method with a concentration range of 12.5-75 µg/mL obtained a correlation coefficient of 0.9995 [15]. Validation of the method with a concentration range of 0.2-3.5 mg/mL resulted in a linearity of 0.993 and a limit detection of 0.13 mg/mL [16].…”