Determination of cyanide ions in saliva using gas chromatography after derivatization with pentafluorobenzyl bromide
ZHUANG Xiao-zhou, YE Li-he, PENG Jian-mei, CAI Xiao-xuan, ZHOU Chang-xia, ZHONG Yuan-qin
Department of Physicochemical Laboratory, Dongguan Municipal Center for Occupational Disease Prevention and Treatment, Dongguan, Guangdong 523008, China
Abstract：Objective To establish an analytical method for quantitative determination of cyanide ion in saliva based on gas chromatography with electron capture detector (ECD) after derivatization with pentafluorobenzyl bromide (PFB-Br). Methods A small amount of saliva was diluted to volume with acetonitrile solution after being added buffer solution, then was added quantitative PFB-Br and shaken well. The samples which had been boiled 30 minutes for the derivative reaction were injected into the gas chromatograph directly to be separated after cooling, and then detected by ECD. Results The method showed that a good linearity range of cyanide ion mass concentration in saliva was 0.25-200.0 mg/L, and the linear correlation coefficient was 0.999,4. The detection limit was 0.07 mg/L and the minimum detection concentration was 0.25 mg/L when saliva volume was 100.0 μl. The between-run relative standard deviation (RSD) was in the range of 2.4%-5.3% (n=6), the within-run RSD was in the range of 1.1%-3.8% (n=6), and the recovery rate was between 100.7% and 102.1%. The common inorganic ions as Cl-, F- and SCN- in saliva had no interference to the determination results. The samples could be stored for at least 15 days in a refrigerator at 4 ℃. Conclusions This method is applicable for determination of cyanide ions in saliva and valuable for emergency detection of cyanide poisoning .
2018, Vol. 25 
