Abstract
A new gas chromatographic method was developed for the determination of thiocyanate ion in biological fluids. Fluid sample solutions deproteinized with acetone or methanol were centrifuged. After evaporation of the organic solvent of the supernatant by a rotary evaporator, thiocyanate ion was ethylated with ethyl iodide in an immiscible aqueous phase-organic phase system by using an immobilized phase-transfer catalyst. The resulting ethyl thiocyanate was determined by gas chromatography on a 20% polyethylene glycol 20M column. Either a flame ionization detector (FID) or a flame thermionic detector (FTD) was used. Thee method was capable of detemining thiocyanate ion concentrations in the range of 5 to 40μg/ml with the FID and 0.05 to 20μg/ml with the FTD. The detection limits were 1μg/ml with the FID and 0.01μg/ml with the FTD. The recoveries of thiocyanate ion added to cow′s milk, human saliva, and human urine samples were over 92% with good repeatability.
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