A gas chromatographic method is described for the determination of CCRL583 (1,1,1,3,3,4,4,4-octafluoro-2-(trifluoromethyl)-2-butanol). The sample is extracted with acetonitrile and cleaned up by liquid-liquid extraction, first with a basic aqueous solution and finally with an acid aqueous solution. The final organic layer is injected into a gas chromatograph equipped with a column packed with terephthalic acid-terminated Carbowax 20M. Recovery of CCRL583 from fortified wheat and peanuts was 91-108%.

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