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Fluorous and Fluorogenic Derivatization for Selective Liquid Chromatographic Analysis of Cyanide in Human Plasma.
Analytical Sciences ( IF 1.8 ) Pub Date : 2020-10-10 , DOI: 10.2116/analsci.20p103
Ryoko Tomita 1 , Tadashi Hayama 1 , Nao Nishijo 1 , Toshihiro Fujioka 1
Affiliation  

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.

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中文翻译:

用于人血浆中氰化物选择性液相色谱分析的氟和荧光衍生化。

描述了一种采用氟衍生化的液相色谱(LC)方法测定人血浆中的氰化物。该方法利用2,3-萘二醛和全氟烷基胺试剂在温和的反应条件下(室温反应时间5 min)将氰化物转化为含氟荧光化合物。流动相中使用高浓度有机溶剂,所得衍生物成功保留在全氟烷基修饰LC柱上,而非氟衍生物几乎没有保留,随后在激发和发射波长420和490处进行荧光检测纳米,分别。在优化条件下,5μL进样量中氰化物的检出限和定量限分别为1.3μg/L(S/N =3)和4.4μg/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%。通过将其应用于人血浆样本的分析,进一步评估了该方法的可行性。

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更新日期:2020-10-28
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