Validation of the HS-GC-FID method for the determination of ethanol residue in tablets

This paper describes the validation of a HSGCFID method (based on the Pharmacopeia's method) for the determination of ethanol content in tablets. A general view of the procedure development/optimization process is presented. The main point of this study is the calculation of validation parameters. Selectivity of the method was determined. Linearity (r > 0.997) was observed in the range from 9.0 to 3,040 mu g of ethanol per sample (because the mass of the tablets used was around 200 mg, this corresponds to 45-15,200 mu g g(-1)). The method showed good recoveries (average 99.0%), and a relative standard deviation for repeatability and intermediate precision of 4.5% and 5.5% respectively. The limit of detection was calculated to be 3.0 mu g of ethanol per sample (15 mu g g(-1)). The uncertainty budget was done according to the "Guide to the Expression of Uncertainty in Measurement'' (GUM)[1], and a relative expanded uncertainty was estimated as 4.8%. This paper describes the validation of a HS-GC-FID method (based on the Pharmacopeia's method) for the determination of ethanol content in tablets. A general view of the procedure development/optimization process is presented. The main point of this study is the calculation of validation parameters. Selectivity of the method was determined. Linearity (r > 0.997) was observed in the range from 9.0 to 3,040 mu g of ethanol per sample (because the mass of the tablets used was around 200 mg, this corresponds to 45-15,200 mu g g(-1)). The method showed good recoveries (average 99.0%), and a relative standard deviation for repeatability and intermediate precision of 4.5% and 5.5% respectively. The limit of detection was calculated to be 3.0 mu g of ethanol per sample (15 mu g g(-1) stop). The uncertainty budget was done according to the "Guide to the Expression of Uncertainty in Measurement" (GUM)[1], and a relative expanded uncertainty was estimated as 4.8%.