The use of AOAC standard methods for the determination of nicotine in commercial tobacco products is shown to be inappropriate. The methods do not provide for suitable sample preparation of these products for the analysis and, in addition, they yield high results. Evidence is presented that the nicotine or total alkaloids measured includes artifact nicotine. The distillation method was developed at a time when the complex alkaloid chemistry of tobacco was unknown, and does not take into consideration the possible contribution of substances in tobacco capable of contributing falsely to the result. The Cundiff-Markunas method, developed more recently, also fails to account for this effect—probably because it was designed to produce results matching those of the distillation method. Replacement of the standard methods is proposed and some alternative procedures are suggested

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Platinum oxide (0.2 g.) was added and the mixture hydrogenated at 700 p.s.i. for two hours. The catalyst was removed, methanolic hydrogen chloride added until acid to congo red and the methanol evaporated in vacuo.The residue was shaken with 25 ml. of water giving a suspension of the rather insoluble hydrochloride of IV. It was converted to the base and after recrystallization once from ethanol-water and from methanol, 150 mg. of elongated plates of ¿Z-l 1-methoxyalloyohimbane (IV) was obtained. On the hot-stage it melted at 195-198°with a change to opaque crystals at 100°. The melting point in an evacuated capillary was 203-205°.

Because existing procedures for the analytical determination of the nitrogencontaining compounds in tobacco do not cover all its nitrogenous constituents, and because of the possible biochemical and industrial significance of these undetermined compounds, a scheme of analysis was devised to permit not only determination

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