A method for the preparation and purification of pentylated derivatives is described for nine organotin compounds that are relevant in environmental analysis (tributyltin acetate, dibutyltin dichloride, butyltin trichloride, triphenyltin chloride, diphenyltin dichloride, phenyltin trichloride, tricyclohexyltin hydroxide (cyhexatin), dicyclohexyltin dibromide and bis (trineophyltin) oxide (fenbutatinoxide)). The compounds are synthesized on a 100 mg scale and purified by column chromatography. Purity checks were performed with gas chromatography with mass selective detection. The mass spectrum of pentyltrineophyltin is presented.