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Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

机译:用分散液 - 液微萃取,用气相色谱 - 质谱法测定人血浆中左旋乙酰胺

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摘要

Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.
机译:Levetiracetam(Lem)是一种抗癫痫药物,在普遍性和部分癫痫综合征中临床有效。这种药物的使用在临床实践中越来越大,并且对特殊人口表现出或 - internamidivialim的变异性。因此,在生物基质中药物监测需要生物分析方法。因此,该工作提出了一种分散液 - 液体微萃取方法,然后是气相色谱 - 质谱(DILLME-GC-MS),用于人血浆中的LEV定量。但是,由于基质复杂性,需要先前的纯化步骤。与文献中呈现的其他预处理技术不同,首次开发了使用超滤管AMICON®(10kDA多孔尺寸)而没有有机溶剂消耗的过程。使用线性温度程序,毛细管熔融二氧化硅柱和作为载气的氦气进行GC-MS分析。 DLLME优化参数是萃取和分散溶剂的类型和体积,盐添加和涡旋搅拌时间。在选择的参数下(提取溶剂:氯仿,130μl;分散溶剂:异丙醇,400μL;没有盐添加和无涡流时间),完全验证了该方法,所有参数都与文献建议一致。使用小于550μl的有机溶剂在患者的血浆样品中量化LeL。

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