An analytical method for an insecticide Fipronil and its metabolite MB 46513 remaining in agricaitunil products has been established which uses GC-ECD and GC/MS for their determination and continuation, respectively. In this method, target compounds are extracted with acetone from agricultural products, concentated, and finally re-extracted with n-hexane. When the sample contains lipid in large quantity, it is first delipidated by partition with acetonitrile, cleaned up with Florisil column, and finally determined by GC-ECD. In the case of vegetables and fruits, which contain lipids in small quantity, the sample is cleaned up with a Florisil column and determined by GOECD. The detection limit of this method is 0.001 micro g/g for both of these kind of samples, the recovery of Fipronil is over 85%, and the C. V. of the recovery is less than 7%. For MB-46513. the recovery is over 63% and its C. V. is less than 9%. This method was applied to 17kinds of agricultural products and no Fipronil and MB46513 were detected.

A micro analytical method has been established for aliphatic lower primary and secondary amines in environmental water and sediment. Amines were distilled and allowed to react with benzenesulfonyl chloride under an alkaline condition. The derivatized compounds were extracted with benzene under an acidic condition and subjected to a determination by GC/MS. This method has been successfully applied for a simultaneous determination of primary and secondary amines with recovery over 80%, except for methylamine, and C.V. below 7%, except for methyl and dimethyl amines; moreover, the detection limit were 0.1 micro g/L for all of the amines determinated. This method is excelent also in sensitivity, is sufficiently applicable to environmental samples.