Ultra-sensitive determination of cyanide in surface water by gas chromatography–tandem mass spectrometry after derivatization with 2-(dimethylamino)ethanethiol
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Add time:07/30/2019 Source:sciencedirect.com
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 r2 = 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−, SO42−, PO43−, K+, Na+, NH4+, Ca2+, Mg2+, Ba2+, Mn4+, Mn2+, Fe3+, Fe2+ 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.
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