A method was developed for simultaneous determination of cyanide and thiocyanate in milk by gas chromatography-tandem quadrupole mass spectrometry (GC-MS/MS). Cyanide and thiocyanate were derivatized with pentafluorobenzyl bromide (PFBBr) as PFB-CN and PFB-SCN, respectively. Cetyltrimethylammonium bromide (CTAB) was employed both as a phase transfer catalyst and a protein precipitant in the sample pretreatment, which facilitates the separation of the organic and aqueous phases, and greatly simplifies the pretreatment procedures to achieve simultaneous and rapid determination of cyanide and thiocyanate. Under the optimized conditions, the limits of detection (LODs) of cyanide and thiocyanate in milk were 0.006 mg/kg and 0.015 mg/kg, and the spiked recoveries ranged from 90.1% to 98.2% and from 91.8% to 98.9% with relative standard deviations (RSDs) less than 18.9% and 15.2%, respectively. The proposed method was validated as a simple, fast and highly sensitive method for the determination of cyanide and thiocyanate in milk.
Keywords: Cyanide; cetyltrimethylammonium bromide (CTAB); gas chromatography-tandem mass spectrometry (GC-MS/MS); milk; pentafluorobenzyl bromide (PFBBr); thiocyanate.