A rapid sample clean-up and chromatographic separation were developed to determine both furfural and 5-hydroxymetbylfurfural (HMF) in citrus juices. Furfural and HMF were isolated by using a C-18 cartridge, and quantified by isocratic elution with a&on&rile/water (lY85, v/v) as the mobile phase with a Radial-PAK C-18 column (100 x 8 mm i.d.). Detection was at 280 nm and the lower limit of detection for both compounds was 50 ppb. Recoveries between 94.0 and 101.2% were obtained for HMF added to orange juice. Recoveries of fmfural ranged between 96.8 and 103.9%.
INTRODUCTIONTHE OCCURRENCE of furfural and 5hydroxymethylfurfural (HMF) in stored citrus products is recognized as an indication of quality deterioration (Berry and Tatum, 1965;Nagy et al., 1972;Nagy and Randall, 1973;Maraulja et al., 1973). Dinsmore and Nagy (1972) employed a distillation procedure to remove furfural from aged citrus juices; distillation was followed by calorimetric determination of furfural in the distillate. This method produced low recoveries and wide statistical variations in furfural concentration because of the instability of the colored reaction product. Later, Dinsmore and Nagy (1974) described an improved calorimetric method, which was based on the Stenhouse color reaction of furfural with aniline in acetic acid. Although more specific for furfural, the recoveries were still less than 38%. Recently, a more precise HPLC method (Marcy and Rouseff, 1984) was developed for determination of furfural, but the HPLC method required the identical distillation step which suffered from low recoveries. Meydav and Berk (1978) proposed a calorimetric method for determination of HMF in citrus products based on the thiobarbituric acid color reaction. A direct solvent extraction with diethyl ether was utilized to determine the degradative metabolites by gas-liquid chromatography (Tatum et al., 1975) or by thin-layer chromatography (Shaw et al., 1970), but only qualitative identifications were made. The objective of this study was to develop a sample preparation method for the simultaneous determination of turfural and HMF in citrus juices using a disposable C-18 cartridge.