Simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry

A method for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables was developed by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). The samples were firstly digested by HC1/THF (1:10, v/v), then extracted by hexane and followed by the derivatization with Grignard reagent (EtMgBr). Then after purification using florisil SPE columns, the sample extracts were finally analyzed by GC-MS/MS. The qualitative and quantitative determinations of the three organotin pesticides were performed by the tandem mass in multiple reaction monitoring (MEM) mode. By using apple as a representative matrix, the limits of detection (LODs) obtained by the proposed method for cyhexatin, triphenyltin and fenbutatin oxide were 2. 0, 1. 5 and 3. 4 μg/kg (as Sn), respectively. The average recoveries for the three organotin pesticides were in the range of 72. 496-107. 1% at the spiked levels of 10, 20, 50 and 200μg/kg (as Sn) and the relative standard deviations (RSDs) ranged from 0. 4% to 14. 2%. The proposed method was validated to have good linearity, high sensitivity, selectivity and accuracy for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide in fruits and vegetables. The sensitivity of this method can meet the requirement, of the inspection for the three organotin pesticides at the level of maximum residue limit, (MRLs) set by China and some other countries.