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A Paper Chromatographic Method for Determination of Vanillin and Ethyl Vanillin in Vanilla Flavorings¹

Department of Dairy Technology, The Ohio State University, Columbus

ABSTRACT

In conjunction with a vanilla ice cream flavor study, attention was given to analysis for vanillin and ethyl vanillin. The method of ter Heide and Lemmens (2) was modified by changing the petroleum ether, using aniline-phthalate for color development, and using infrared spectrophotometry for quantitative analysis.

Qualitative procedure. A 5-µl sample was spotted 2 in. from the edge of an 11 by 18-in. sheet of Whatman No. 1 chromatographic paper. Five-µl portions of a dilute (1%) alcoholic or chloroform solution of vanillin and ethyl vanillin were spotted on the same paper for reference. The paper was placed in a cylindrical chromatography jar and developed in ascending fashion with a solvent system composed of benzene, petroleum ether (B.P. 30–60), and methanol in a 2:10:1 ratio by volume. After a developing time of 4 hr, the chromatogram was air-dried and sprayed with an aniline-phthalate reagent (0.93 g reagent grade aniline and 1.66 g phthalic anhydride to 100 ml of butanol saturated with water) previously used for color development of carbohydrates (1).

¹ Technical Paper 10-62. The Department of Dairy Technology, The Ohio State University. Study supported by a grant from the American Dairy Association.