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Comparison of conventional and supported liquid extraction methods for the determination of sitagliptin and simvastatin in rat plasma by LC–ESI–MS/MS

机译:LC-ESI-MS / MS测定大鼠血浆中西他列汀和辛伐他汀的传统方法和支持液提取方法的比较

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Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC–MS/MS, including (1) liquid–liquid extraction (LLE), (2) solid phase extraction (SPE) and (3) supported liquid extraction (SLE). Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring (MRM) in a positive ion mode with ESI. The transitions monitored were m/z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification (LLOQ) was 0.2ng/mL for sitagliptin and 0.1ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.
机译:比较了三种提取方法通过LC-MS / MS分析大鼠血浆中西他列汀和辛伐他汀的效率,包括(1)液-液提取(LLE),(2)固相提取(SPE)和(3)负载液体提取(SLE)。比较不同萃取方法的分析物回收率表明,SLE是最佳萃取方法。离子阱质谱仪通过正离子模式下的ESI多反应监测(MRM)促进了检测。对于辛伐他汀,监测的转变为m / z 441.1→325.2,对于西他列汀为408.2→235.1,对于IS为278.1→260.1。西他列汀的定量下限(LLOQ)为0.2ng / mL,辛伐他汀为0.1ng / mL。有效的SLE提供增强的色谱选择性,因此有利于该方法对生物样品的常规分析以及药代动力学研究的潜在效用。

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