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Determination of amino acids and amines in mammalian decomposition fluid by direct injection liquid chromatography-electrospray ionisation-tandem mass spectrometry

机译:直接进样液相色谱-电喷雾电离-串联质谱法测定哺乳动物分解液中的氨基酸和胺

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摘要

A sensitive and selective analytical method utilising liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) operated in multiple reaction monitoring mode was developed for the semi-quantitative determination of 19 biogenic amines and amino acids in mammalian (porcine) decomposition fluid. The effect of the matrix on analyte response was initially investigated by diluting crude samples and by injecting various volumes in the LC-MS system. It was found that the matrix had little effect on analyte signal intensities when small volumes (0.1 to 1 μL) of crude samples or 1 : 10 diluted samples were injected into the LC-ESI-MS/MS system. The standard addition method was also investigated for quantitative assessment but proved unsuccessful, possibly due to poor ionisation of the electrospray interface at high analyte concentrations. Therefore a method using external calibration was used for semi-quantitative determination of the analytes in decomposition fluid. The LC-ESI-MS/MS method enabled identification of all target compounds as being present. In addition a 14-day cyclic trend in the concentrations of two amino acids, phenylalanine and tryptophan, was tentatively established. General increasing trends with respect to time and temperature were also observed for putrescine and indole.
机译:建立了一种以液相色谱-电喷雾电离-串联质谱(LC-ESI-MS / MS)进行多反应监测的灵敏且选择性的分析方法,用于半定量测定哺乳动物(猪)中的19种生物胺和氨基酸)分解液。最初通过稀释粗样品并通过在LC-MS系统中注入各种体积来研究基质对分析物响应的影响。发现将少量(0.1到1μL)粗样品或1:10稀释样品注入LC-ESI-MS / MS系统后,基质对分析物信号强度的影响很小。还对标准添加方法进行了研究,以进行定量评估,但证明不成功,这可能是由于在高分析物浓度下电喷雾界面的电离差所致。因此,使用外部校准的方法用于半定量测定分解液中的分析物。 LC-ESI-MS / MS方法能够鉴定所有存在的目标化合物。此外,初步确定了两个氨基酸(苯丙氨酸和色氨酸)浓度的14天循环趋势。还观察到腐胺和吲哚在时间和温度方面的总体增长趋势。

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