Fraction collection from capillary liquid chromatography and off-line electrospray ionization mass spectrometry using oil segmented flow.
Fraction collection from capillary liquid chromatography and off-line electrospray ionization mass spectrometry using oil segmented flow.
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DOI：
10.1021/ac100669z
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发表时间：
2010-06-15
影响因子：
7.4
通讯作者：
Kennedy, Robert T.
中科院分区：
文献类型：
--
作者：
Li, Qiang;Pei, Jian;Song, Peng;Kennedy, Robert T.
通过毛细管液相色谱法（LC）分离的样品的离线分析和表征使用常规方法收集级分是有问题的。我们展示了收集纳升馏分形成塞子的流出物从75 μm内径的LC柱分割的不混溶的油，如全氟萘烷。塞子储存在管道中，然后可以用于操作样品。离线电喷雾质谱（ESI-MS）用于表征样品。通过将分段的塞直接泵入纳米喷雾发射器尖端来进行ESI-MS。关键参数，包括油的选择，ESI电压，和流速，使成功的直接注入分析进行了研究。在油不形成电喷雾而是从尖端虹吸离开的条件下获得最佳信号。离线分析显示保留了色谱图，没有损失分辨率。证明该方法允许在分析期间改变流速。具体地，使用流速的降低以允许延长对所选级分的MS分析时间，类似于“峰停放”。
Off-line analysis and characterization of samples separated by capillary liquid chromatography (LC) has been problematic using conventional approaches to fraction collection. We demonstrate collection of nanoliter fractions by forming plugs of effluent from a 75 μm inner diameter LC column segmented by an immiscible oil such as perfluorodecalin. The plugs are stored in tubing that can then be used to manipulate the samples. Off-line electrospray ionization mass spectrometry (ESI-MS) was used to characterize the samples. ESI-MS was performed by directly pumping the segmented plugs into a nanospray emitter tip. Critical parameters including the choice of oils, ESI voltage, and flow rates that allows successful direct infusion analysis were investigated. Best signals were obtained under conditions in which the oil did not form an electrospray but was siphoned away from the tip. Off-line analysis showed preservation of the chromatogram with no loss of resolution. The method was demonstrated to allow changes in flow rate during the analysis. Specifically, decreases in flow rate were used to allow extended MS analysis time on selected fractions, similar to “peak parking”.
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影响因子：
7.4
作者：
Li, Qiang;Zubieta, Jon-Kar;Kennedy, Robert T.
通讯作者：
Kennedy, Robert T.
DOI：
10.1016/s1044-0305(97)00282-1
发表时间：
1998-03-01
影响因子：
3.2
作者：
Davis, MT;Lee, TD
通讯作者：
Lee, TD
影响因子：
3.9
作者：
Okushima, S;Nisisako, T;Higuchi, T
通讯作者：
Higuchi, T
DOI：
10.1016/j.jchromb.2006.05.031
发表时间：
2006-10-20
影响因子：
3
作者：
Kirchherr, H.;Kuehn-Velten, W. N.
通讯作者：
Kuehn-Velten, W. N.
影响因子：
7.4
作者：
Murphy, RE;Schure, MR;Foley, JP
通讯作者：
Foley, JP