Abstract: A gas chromatography-mass spectrometry (GC-MS) method has been developed for the determination of dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPhT) in textile auxiliaries. The sample was first extracted with n-hexane in acetate buffer solution (pH 4.0) under ultrasonication (for hydrophobic sample) or oscillation extraction (for hydrophilic sample) and then derivatized with sodium tetraethylborate in tetrahydrofuran. The derivative was determined by GC-MS in selected ion monitoring (SIM) mode. The separation and quantification were achieved using a Rxi-5ms silica capillary column (30 m×0.25 mm×0.25 μm). The linear ranges were 0.1~8.0 mg/L for both DBT and TBT, and 0.1~4.0 mg/L for TPhT. There were good linear relationships between the peak area and concentration in the linear ranges and the correlation coefficients (r2) were 0.9994~0.9998. The detection limits (LOD) were from 0.003 mg/L to 0.005 mg/L. The average recoveries of these organotin compounds at the three spiked levels of 4.0, 10.0 and 40.0 mg/kg were 92.6%~108.0% with the relative standard deviations (RSDs) of 2.5%~10.2%. The method is simple and accurate for simultaneous analysis of the DBT, TBT and TPhT in textile auxiliaries.

Key words: gas chromatography-mass spectrometry (GC-MS), organotin, textile auxiliary