OBJECTIVE: To establish a method for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil. METHODS: Capillary gas chromatography was performed on the column of DB-FFAP capillary column by temperature programmed, the inlet temperature was 150 ℃, flame ionization detector was chosen, detector temperature was 290 ℃, carrier gas was nitrogen at a flow rate of 1.0 ml/min, injection volume was 1.0 μl, and split ratio was 5 ∶ 1. RESULTS: 1,1-ethanediol diacetate and acetic acid were well-separated; and the linear ranges was 0.78-19.55 g/ml (r=0.999 7) and 7.69-64.11 μg/ml (r=0.999 3), respectively; the limits of quantification were 0.78 μg/ml and 7.69 μg/ml, and limits of detection were 0.23 μg/ml and 2.56 μg/ml for 1,1-ethanediol diacetate and acetic acid respectively; RSDs of precision and reprocudibility tests were lower than 3%, and stability test was lower than 5%; recoveries were 97.6%-100.4%(RSD=0.94%,n=9) and 93.6%-100.4%(RSD=0.94%,n=9); and the test results for 3 batches of flurbiprofen axetil were met the specification. CONCLUSIONS: The method is simple, accurate and reliable, and can be used for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil.
关键词
氟比洛芬酯原料药毛细管气相色谱法11-乙二醇二乙酸酯乙酸残留量
Keywords
Flurbiprofen axetilCapillary gas chromatography11-ethanediol diacetateAcetic acidResidual