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Accurate and simple determination of oxcarbazepine in human plasma and urine samples using switchable-hydrophilicity solvent in GC-MS.
Biomedical Chromatography ( IF 1.8 ) Pub Date : 2020-06-11 , DOI: 10.1002/bmc.4915
Sezin Erarpat 1 , Süleyman Bodur 1 , Merve Fırat Ayyıldız 1 , Ömer Tahir Günkara 1 , Fatih Erulaş 2 , Dotse Selali Chormey 1 , Fatma Turak 1 , Türkan Börklü Budak 1 , Sezgin Bakırdere 1
Affiliation  

This work presents a sensitive and rapid analytical method for the determination of oxcarbazepine in human plasma and urine samples. A vortex‐assisted switchable hydrophilicity solvent‐based liquid phase microextraction (VA–SHS–LPME) was used to preconcentrate oxcarbazepine from the samples before the determination by gas chromatography mass spectrometry. The switchable hydrophilicity solvent was synthesized by protonating N,N‐dimethylbenzylamine with carbon dioxide to make it totally miscible with an equivalent volume of water. Parameters of the VA–SHS–LPME method including volume of switchable hydrophilicity solvent, concentration/volume of sodium hydroxide and vortex period were systematically optimized. Under the optimum conditions, good linearity ranging from 27.03 to 353.47 μg/kg was obtained for the analyte. Limit of detection and quantitation values were found to be 6.2 and 21 μg/kg (mass base), respectively. The relative standard deviation was calculated as 6.9% for six replicate measurements of the lowest concentration of the calibration plot. Satisfactory recovery results were calculated in the range of 97–100% for human plasma and urine samples spiked at five different concentrations.

中文翻译:

使用可切换的亲水性溶剂在GC-MS中准​​确,简单地测定人血浆和尿液中的奥卡西平。

这项工作为测定人血浆和尿液样品中的奥卡西平提供了一种灵敏而快速的分析方法。在气相色谱质谱法测定之前,使用涡流辅助可切换亲水性溶剂基液相微萃取(VA–SHS–LPME)对样品中的奥卡西平进行预浓缩。通过NN的质子化反应合成可切换的亲水性溶剂。-二甲基苄胺与二氧化碳的混合物,使其与等体积的水完全混溶。系统地优化了VA–SHS–LPME方法的参数,包括可切换亲水性溶剂的体积,氢氧化钠的浓度/体积和涡旋周期。在最佳条件下,分析物的线性良好,范围从27.03至353.47μg/ kg。检出限和定量值分别为6.2和21μg/ kg(质量基准)。六次重复测量校准曲线的最低浓度时,相对标准偏差计算为6.9%。对于以五种不同浓度加标的人体血浆和尿液样品,令人满意的恢复结果的计算范围为97-100%。
更新日期:2020-06-11
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