Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Dec 1;940:142-9. doi: 10.1016/j.jchromb.2013.09.035. Epub 2013 Oct 3.
A one-step derivatization and microextraction technique for the determination of amantadine in the human plasma and urine samples is presented. An appropriate mixture of methanol (disperser solvent), 1,2-dibromoethane (extraction solvent), and butylchloroformate (derivatization agent) is rapidly injected into samples. After centrifuging, the sedimented phase is analyzed by gas chromatography-flame ionization detection (GC-FID). The kind of extraction and disperser solvents and their volumes, amount of derivatization agent and reaction/extraction time which are effective in derivatization/dispersive liquid-liquid microextraction (DLLME) procedure are optimized. Under the optimal conditions, the enrichment factor (EF) of the target analyte was obtained to be 408 and 420, and limit of detection (LOD) 4.2 and 2.7ngmL(-1), in plasma and urine respectively. The linear range is 14-5000 and 8.7-5000ng/mL for plasma and urine, respectively (squared correlation coefficient≥0.990). The relative recoveries obtained for the spiked plasma and urine samples are between 72% and 93%. Moreover, the inter- and intra-day precisions are acceptable at all spiked concentrations (relative standard deviation <7%). Finally the method was successfully applied to determine amantadine in biological samples.
本文提出了一种一步衍生化和微萃取技术，用于测定人血浆和尿液中的金刚烷胺。将适量的甲醇（分散溶剂）、1,2-二溴乙烷（萃取溶剂）和丁基氯甲酸酯（衍生化剂）快速注入样品中。离心后，对沉淀相进行气相色谱-火焰离子化检测（GC-FID）分析。优化了萃取和分散溶剂的种类及其体积、衍生化剂的用量以及衍生化/分散液-液微萃取（DLLME）过程中的反应/萃取时间，以获得最佳条件。在最佳条件下，目标分析物在血浆和尿液中的富集因子（EF）分别为 408 和 420，检测限（LOD）分别为 4.2 和 2.7ngmL(-1)。血浆和尿液的线性范围分别为 14-5000 和 8.7-5000ng/mL（相关系数≥0.990）。在所有加标浓度下，血浆和尿液中加标样品的相对回收率均在 72%至 93%之间。此外，日内和日间精密度在所有加标浓度下均可接受（相对标准偏差<7%）。最后，该方法成功应用于生物样品中金刚烷胺的测定。
