SENSITIVE FLUORESCENCE LABELING FOR ANALYSIS OF ORGANOTIN COMPOUNDS WITH MORIN

Analytical procedures based on reversed-phase high-performance liquid chromatography combined with post-column derivatization with morin for the determination of organotin compounds in peanut oil, water samples or diet mixtures are described. A mixture of the isooctylesters of monooctyl tin and dioctyl tin thioglycolic acid (ZK 30434), a mixture of the isooctylesters of monododecyl tin and didodecyl tin thioglycolic acid (ZK 32283) or dibutyl tin difluoride (ZK 38 068) had to be analysed. The data obtained from validation and during routine analysis show that the post-column derivatization with morin is a powerful tool for the selective and sensitive detection of organotin compounds in complicated matrices. Interferences of peaks related to the organotins and the matrix constituents were not found. The values of the limit of detection were 10-mu-g ZK 30434 or ZK 32283/ml peanut oil, 60 ng ZK 38068/ml water and 2.5 mg ZK 30434/kg rodent diet mixture. Regarding to the repeatability, the methods described are characterized by values of the relative standard deviation of mostly less than 5%. In case of the determination of ZK 30434 dissolved in peanut oil atomic absorption spectrometry was used to investigate the accuracy of the HPLC method. A good correlation between the HPLC and AAS data was found. The limits of quantitation were 0.25 mg ZK 30434/ml peanut oil, 0.22 mg ZK 32283/ml peanut oil and 1.0-mu-g ZK 38068/ml water. The analytical procedures were applied within the framework of the analytical service for validation of toxicological studies according to the guidelines of good laboratory practices (G.L.P.). Both the correct preparation of the formulations and the homogeneity or stability could be checked.