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Analytical Quality by Design-based development and validation of ultra pressure liquid chromatography/MS/MS method for glycopeptide antibiotics determination in human plasma

机译:基于设计的开发和验证超压液相色谱/ MS / MS方法的分析质量,用于人血浆中的糖肽抗生素测定

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Aim: An ultra pressure liquid chromatography (UPLC)/MS/MS method for vancomycin and teicoplanin determination in human plasma was developed in accordance with analytical quality by design (AQbD) concept and fully validated. Materials & methods: Chromatographic separation was performed on ACQUITY UPLC C-18 charge surface hybrid (CSH) column (2.1 mm x 50 mm, 1.7 mu m particle size) in gradient mode and the mobile phase consisted of 0.1% formic acid in water and pure acetonitrile. The experimental design methodology was used for the definition of optimal chromatographic and protein precipitation conditions. Results: The linearity ranges were 0.05-10 mu g ml(-1) for vancomycin and 0.5-200 mu g ml(-1) for total teicoplanin. The relative standard deviations for precision estimation were below 15% and the accuracy was within 85-115% for all quality control levels. Conclusion: The method was utilized for glycopeptide antibiotics bioanalysis.
机译:目的:按照设计(AQBD)概念和完全验证,通过设计(AQBD)概念的分析质量开发了用于万古霉素和人血浆中的超压液相色谱(UPLC)/ MS / MS / MS方法。 材料和方法:在梯度模式下对诸如UPLC C-18电荷表面杂合(CSH)柱(CSH)柱(CSH)柱(2.1mm×50mm,1.7μm粒度)进行色谱分离,流动相在水中组成0.1%甲酸 纯乙腈。 实验设计方法用于定义最佳色谱和蛋白质沉淀条件。 结果:对于万古霉素,线性范围为0.05-10μgmml(-1),用于总Teicoplanin的0.5-200 mm g ml(-1)。 精度估计的相对标准偏差低于15%,对所有质量控制水平的精度不到85-115%。 结论:该方法用于糖肽抗生素生物分析。

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