In Japan, the addition of sorbic acid and sorbate to wine has been permitted since December, 1973, within the level not surpassing 0.2g/kg as sorbic acid, while neither dehydroacetate nor benzoate is allowed to use as preservatives of wines. Accordingly, it became necessary to establish a determination method of sorbate in wines. It was undertaken in this report to establish a gas chromatographic method for the simultaneous determination of sorbate and detection of dehydroacetate and benzoate in wines, being accompanied with satisfactory results.
A wine sample (50g) was alkalized by the addition of 5m
l of 10% NaOH, then 10g of NaCl and 50m
l of ether was added and the mixture was shaken vigorously. After separation, the upper layer was extracted again with 10m
l of 10% NaOH solution, two aqueous layers were combined together, and, after being acidified by the addition of 10% H
2SO
4, the combined solution was extracted twice with ether. The lower layer was discarded, and, after evaporation of the solvent on a water bath, the residue was dissolved in acetone containing
p-toluic acid and was injected into an FID gas chromatograph fitted with a 1.5m glass column packed with 2% DEGS+0.5% H
3PO
4. A recovery test of sorbate was carried out on two samples of imported wines spiked at 100ppm level with sorbic acid. About 100% of recovery was obtained. The detection limits of sorbic acid, dehydroacetic acid and benzoic acid were 5ppm, respectively. Three from 16 samples, imported in June 1973, were found to contain below 0.2g/kg of sorbic acid, while both dehydroacetic acid and benzoic acid could not be detected in them.
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