Studies on azaspiracid biotoxins. I. Ultrafast high-resolution liquid chromatography/mass spectrometry separations using monolithic columns.
Studies on azaspiracid biotoxins. I. Ultrafast high-resolution liquid chromatography/mass spectrometry separations using monolithic columns.
复制标题
氮杂螺酸生物毒素的研究。
DOI：
--
复制
发表时间：
2002
影响因子：
2
通讯作者：
Bob Whitehead
中科院分区：
文献类型：
--
作者：
D. Volmer;S. Brombacher;Bob Whitehead
在本研究中，评估了整体柱的超快液相色谱/质谱 (LC/MS) 分析和几种氮杂螺酸生物毒素类似物的高分辨率分离性能。由于其高渗透性，整体柱比传统填充柱具有许多优点；即，在高流速下具有非常低的背压和相对平坦的范第姆特曲线。也就是说，非常高的流速可用于超快分析，或者通过使用比普通色谱柱更长的色谱柱，可以实现高分辨率分离。在一系列实验中，我们在 1 至 8 mL/min 之间改变流动相流速，并研究了它们对色谱参数（如保留时间、分辨率、板数和压力）的影响。色谱运行时间可以减少到大约。 30 s 分离效率无明显变化。信号强度比较揭示了大气压化学电离 (APCI) 和电喷雾电离 (ESI) 在流量依赖性方面的有趣差异。本文给出了关于质量流或浓度相关装置的行为的解释。此外，柱长在 10 至 70 厘米之间变化。结果，理论塔板数大幅增加。在报告中所示的示例中，展示了从 10 厘米色谱柱的 13,000 个塔板增加到 70 厘米色谱柱的 80,000 个塔板。此外，整体柱对于复杂生物毒素混合物的高分辨率 LC/MS 分离也具有潜力，该混合物在 40 厘米长的柱上进行分离。
In this study, the performance of monolithic columns was evaluated for ultrafast liquid chromatography/mass spectrometry (LC/MS) analyses and for high-resolution separations of several azaspiracid biotoxin analogs. Because of their high permeability, monolithic columns offer a number of advantages over conventional packed columns; viz., very low backpressures and relatively flat van Deemter curves at high flow rates. That is, very high flow rates can be used for ultrafast analyses or, by using longer than normal columns, high-resolution separations are possible. In a series of experiments, we varied the mobile phase flow rates between 1 and 8 mL/min, and studied their impact on chromatographic parameters such as retention time, resolution, number of plates and pressure. The chromatographic run times could be reduced to ca. 30 s without a significant change in the separation efficiency. A signal intensity comparison revealed interesting differences between atmospheric-pressure chemical ionization (APCI) and electrospray ionization (ESI) in their flow-rate dependency. An explanation with respect to the behavior as of a mass-flow or a concentration-dependent device is given in the paper. Additionally, the column length was varied between 10 and 70 cm. As a result, the number of theoretical plates increased substantially. In the example shown in the report, an increase from 13 000 plates for a 10-cm column to 80 000 for a 70-cm column is demonstrated. In addition, the potential of the monolithic columns for high-resolution LC/MS separations is shown for a complex biotoxin mixture, which was separated on a 40-cm-long column.