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CORESTA Congress, Kyoto, 2004, SSPT 09

Development of multi-residue methods for pesticide residues on tobacco

IZAWA K.; DOI K.; TOMARI I.; SUZUKI Y.; FUKUHARA Y.; YOSHIDA Y.; SHIBATA Y.
Japan Tobacco Inc., Product Quality Research Division, Yokohama, Kanagawa, Japan.

As shown in the presentation of CORESTA Guide No. 1, the need for Good Agricultural Practice of tobacco cultivation is being increasingly recognized. In preparing for the future, analysis methods for pesticide residues on tobacco leaves have been under development and the 90 pesticides in CORESTA Guide No. 1 were selected as the primary targets. As a result of this development, more than 78 of the 90 pesticides can now be anlysed and further development is under way. Currently, multi-residue methods are applied mostly to organochlorines, pyrethroids, 2,6-dinitroanilines, organophosphorous compounds, N-methylcarbamates and organonitrogens. To achieve good test efficiency and recovery rates between 70 to 120% at the same time, the analytical procedures consist of two extraction/ purification processes and 6 types of of detection systems. Organochlorines, pyrethroids and 2,6-dinitroanilines are extracted with acetonitrile and purified by liquid-liquid partition with n-hexane and by solid phase extraction (SPE). GC/ECD and GC/MS are used for the detection. Organophosphorous compounds, N-methylcarbamates, organonitrogens and other pesticides are extracted with acetone/water solution and purified with SPE using diatomaceous earth. This is followed by a further purification processes to obtain the solutions for detections by GC/FPD(P), HPLC and GC/MS. The following are important points for analysis method development. For method validation, recovery rates should be between 70 to 120% and limits of quantification should be lower than the Guideline Residue Level of CORESTA Guide No. 1. Moreover, solvent consumption should be kept to a minimum from safety and environment perspectives.