Tomita Ryoko, Hayama Tadashi, Nishijo Nao, Fujioka Toshihiro
Faculty of Pharmaceutical Sciences, Fukuoka University, 8-19-1 Nanakuma, Johnan, Fukuoka, 814-0180, Japan.
Anal Sci. 2020 Oct 10;36(10):1251-1254. doi: 10.2116/analsci.20P103. Epub 2020 May 29.
A liquid chromatographic (LC) method with fluorous derivatization for the determination of cyanide in human plasma is described. In this method, the cyanide was transformed to a fluorous and fluorogenic compound by derivatizing with 2,3-naphthalenedialdehyde and perfluoroalkylamine reagent under mild reaction conditions (a reaction time of 5 min at room temperature). The obtained derivative was successfully retained on the perfluoroalkyl-modified LC column with the use of a high concentration of organic solvent in the mobile phase, whereas non-fluorous derivative was hardly retained, followed by fluorometric detection at excitation and emission wavelengths of 420 and 490 nm, respectively. Under the optimized conditions, the limit of detection and the limit of quantification for cyanide in a 5-μL injection volume were 1.3 μg/L (S/N = 3) and 4.4 μg/L (S/N = 10), respectively. The recovery from spiked human plasma was achieved in the range of 54 - 90% within a relative standard deviation of 3.5%. The feasibility of this method was further evaluated by applying it to the analysis of human plasma samples.
描述了一种用于测定人血浆中氰化物的含氟衍生化液相色谱（LC）方法。在该方法中，在温和的反应条件下（室温下反应5分钟），氰化物通过与2,3-萘二醛和全氟烷基胺试剂衍生化转化为含氟且具荧光的化合物。使用流动相中高浓度有机溶剂时，所得衍生物成功保留在全氟烷基修饰的LC柱上，而非含氟衍生物几乎不被保留，随后分别在激发波长420 nm和发射波长490 nm下进行荧光检测。在优化条件下，进样体积为5 μL时，氰化物的检测限和定量限分别为1.3 μg/L（S/N = 3）和4.4 μg/L（S/N = 10）。加标人血浆的回收率在54 - 90%范围内，相对标准偏差为3.5%。通过将该方法应用于人血浆样品分析进一步评估了其可行性。
