Kage S, Nagata T, Kudo K
Department of Forensic Medicine, Faculty of Medicine, Kyushu University, Fukuoka, Japan.
J Chromatogr B Biomed Appl. 1996 Jan 12;675(1):27-32. doi: 10.1016/0378-4347(95)00344-4.
We devised a sensitive and simple method for determining cyanide and its major metabolite, thiocyanate, in blood using an extractive alkylation technique. Pentafluorobenzyl bromide was used as the alkylating agent, and tetradecyldimethylbenzylammonium chloride was used as the phase-transfer catalyst. The derivatives obtained were analyzed qualitatively by gas chromatography-mass spectrometry and quantitatively by gas chromatography with an electron-capture detection. The detection limits of cyanide and thiocyanate were 0.01 and 0.003 mumol/ml, respectively, while the gross recovery of both compounds was 80%. The calibration curve was linear over the concentration range from 0.02 to 1.0 mumol/ml for cyanide and from 0.01 to 1.0 mumol/ml for thiocyanate. The accuracy and precision of the method were evaluated, and the coefficients of variation were found to be within 10%. Using the method, the blood levels of two victims who had died from cyanide poisoning were determined.
我们设计了一种灵敏且简便的方法，利用萃取烷基化技术测定血液中的氰化物及其主要代谢产物硫氰酸盐。五氟苄基溴用作烷基化试剂，十四烷基二甲基苄基氯化铵用作相转移催化剂。所得衍生物通过气相色谱 - 质谱联用法定性分析，通过带有电子捕获检测的气相色谱法定量分析。氰化物和硫氰酸盐的检测限分别为0.01和0.003μmol/ml，而两种化合物的总回收率为80%。氰化物的校准曲线在0.02至1.0μmol/ml浓度范围内呈线性，硫氰酸盐的校准曲线在0.01至1.0μmol/ml浓度范围内呈线性。对该方法的准确性和精密度进行了评估，发现变异系数在10%以内。使用该方法测定了两名死于氰化物中毒受害者的血液水平。
