首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Generic on-line solid phase extraction sample preparation strategies for the analysis of drugs in biological matrices by LC-MS/MS
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Generic on-line solid phase extraction sample preparation strategies for the analysis of drugs in biological matrices by LC-MS/MS

机译:通过LC-MS / MS分析生物基质中药物的通用在线固相萃取样品制备策略

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摘要

In the present work we investigate the integration of a single hardware platform (Prospekt-2) allowing on-line SPE with pre-/post-trapping dilution and direct injection of plasma extracts, and also compare the benefits and challenges of the different approaches for pharmaceutical drugs with heterogeneous physicochemical properties. In the first part, the generic use of on-line SPE with direct plasma injection or after protein precipitation was investigated for the quantitative analysis of talinolol. In the second part, pre-trapping and post-trapping dilution for on-line SPE is discussed for generic method development on an oxadiazole and its major metabolite. Finally, the difference of performance between direct plasma injection vs. off-line liquid liquid extraction is also described for the quantification of buprenorphine and naltrexone down to 50 and 100 pg/ml using a 0.25 ml plasma aliquot. All assays were in human plasma and detection was performed by mass spectrometry detection either on simple or triple stage quadrupoles. Regardless of the tested strategy, assays were found linear, with precision and accuracy with <15% for all quality controls samples and <20% for lower limit of quantitation. (C) 2014 Elsevier B.V. All rights reserved.
机译:在目前的工作中,我们研究了单个硬件平台(Prospekt-2)的集成,该平台允许在线SPE进行捕集前/捕集后稀释和血浆提取物的直接注射,并且还比较了不同方法在制备和纯化中的优势和挑战具有异构理化特性的药物。在第一部分中,对直接血浆注射或蛋白质沉淀后在线SPE的一般用途进行了研究,以用于他尼洛尔的定量分析。在第二部分中,讨论了在线SPE的捕集前和捕集后稀释,以开发恶二唑及其主要代谢物的通用方法。最后,还描述了直接血浆注射与离线液体提取之间的性能差异,用于使用0.25 ml血浆等分试样定量降到50和100 pg / ml的丁丙诺啡和纳曲酮。所有测定均在人血浆中,并通过质谱检测在简单或三级四极杆上进行。无论采用何种测试策略,都发现测定呈线性,准确度和准确性对所有质量控制样品而言均小于15%,对定量下限而言均小于20%。 (C)2014 Elsevier B.V.保留所有权利。

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