Analytica chimica acta

Ultra-sensitive determination of cyanide in surface water by gas chromatography-tandem mass spectrometry after derivatization with 2-(dimethylamino)ethanethiol.

PMID 25441894


A gas chromatography-tandem mass spectrometric (GC-MS/MS) method has been established for the determination of cyanide in surface water. This method is based on the derivatization of cyanide with 2-(dimethylamino)ethanethiol in surface water. The following optimum reaction conditions were established: reagent dosage, 0.7 g L(-1) of 2-(dimethylamino)ethanethiol; pH 6; reaction carried out for 20 min at 60°C. The organic derivative was extracted with 3 mL of ethyl acetate, and then measured by using GC-MS/MS. Under the established conditions, the detection and quantification limits were 0.02 μg L(-1) and 0.07 μg L(-1) in 10-mL of surface water, respectively. The calibration curve had a linear relationship relationship with y=0.7140x+0.1997 and r(2)=0.9963 (for a working range of 0.07-10 μg L(-1)) and the accuracy was in a range of 98-102%; the precision of the assay was less than 7% in surface water. The common ions Cl(-), F(-), Br(-), NO3(-), SO4(2-), PO4(3-), K(+), Na(+), NH4(+), Ca(2+), Mg(2+), Ba(2+), Mn(4+), Mn(2+), Fe(3+), Fe(2+) and sea water did not interfere in cyanide detection, even when present in 1000-fold excess over the species. Cyanide was detected in a concentration range of 0.07-0.11 μg L(-1) in 6 of 10 surface water samples.