A rapid procedure involving high-performance liquid chromatography with fluorometric detection is described which is capable of analyzing tangerines and oranges, as well as their processed fractions, for residues of NAA as low as 0.008 ppm. Sulfuric acid is used to release conjugates for extraction with methylene chloride, followed by partitioning between ethyl ether and potassium hydrogen phosphate for cleanup. The insensitivity of the fluorometer to pulsatile flow allows the use of an economical single piston solvent pump for chromatography. Residues were measured in ' Dancy ' tangerines and processed fractions in one disappearance experiment and in ' Pineapple ' orange in another.
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