Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection
Determination of amantadine in biological fluids using simultaneous derivatization and dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection
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DOI：
10.1016/j.jchromb.2013.09.035
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发表时间：
2013-12-01
影响因子：
3
通讯作者：
Nabil, Ali Akbar Alizadeh
中科院分区：
文献类型：
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作者：
Farajzadeh, Mir Ali;Nouri, Nina;Nabil, Ali Akbar Alizadeh
建立了一步衍生化-微萃取法测定人血浆和尿样中金刚烷胺的方法。将甲醇(分散剂溶剂)、1，2-二溴乙烷(萃取剂)和氯甲酸丁酯(衍生剂)的适当混合物快速注入样品中。离心后，用气相色谱-火焰离子化检测(GC-FID)对沉淀相进行分析。对影响衍生化/分散液-液微萃取(DLLME)过程的萃取剂和分散剂种类及其用量、衍生化试剂用量和反应/萃取时间进行了优化。在最佳条件下，目标分析物在血浆和尿液中的富集度(EF)分别为408和420，检出限(LOD)分别为4.2和2.7 ng mL(-1)。血浆和尿液的线性范围分别为14~5 000和8 7~5 000 ng/m L(相关系数平方=0.990)。血浆和尿样加标回收率在72%~93%之间。此外，日内和日间精密度在所有添加浓度(相对标准差)下都是可接受的
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 2.7 ng mL(-1), in plasma and urine respectively. The linear range is 14-5000 and 8.7-5000 ng/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