Supercritical Fluid Nanospray Mass Spectrometry
Supercritical Fluid Nanospray Mass Spectrometry
复制标题
超临界流体纳喷雾质谱法
DOI：
10.1021/jasms.2c00134
复制
发表时间：
2022
影响因子：
3.2
通讯作者：
Edwards, James L.
中科院分区：
文献类型：
--
作者：
Mostafa, Mahmoud Elhusseiny;Grinias, James P.;Edwards, James L.
超临界流体通常使用有机溶剂补充流进行电喷雾，以促进连续电连接和电喷雾稳定性的增强。这导致样品稀释、灵敏度损失和潜在的相分离。将超临界流体与有机溶剂预混合已经显示出对电喷雾效率和增加的分析物电荷状态的实质性益处。本文介绍了一种用于超临界流体的纳米喷雾质谱系统（nSF-MS）。该分流系统使用小的i.d.毛细管，加热界面，在线玻璃料，和亚微米发射器尖端电喷雾季烷基胺溶剂化在超临界CO2与10%甲醇改性剂。分析物信号响应作为总系统流速（0.5-1.5 mL/min）的函数进行评价，该总系统流速被分成纳米喷雾超临界流体，线性流速在0.07和0.42 cm/sec之间，压力范围（15-25 MPa）。NSF系统显示出基于增加的信号强度的质量敏感检测，以增加毛细管内径。和分析物注射体积。这些效果表明，有效的溶剂蒸发季胺的分析。载体添加剂通常降低信号强度。nSF-MS系统与常规SF补充流ESI的比较显示，在所有毛细管内径上信号强度增强10倍。nSF-MS系统可能在发射点实现SF的快速溶剂蒸发。所开发的系统结合了纳米发射体、sCO 2和低改性剂百分比的益处，这引起MS检测灵敏度的增强。
Supercritical fluids are typically electrosprayed using an organic solvent makeup flow to facilitate continuous electrical connection and enhancement of electrospray stability. This results in sample dilution, loss in sensitivity, and potential phase separation. Premixing the supercritical fluid with organic solvent has shown substantial benefits to electrospray efficiency and increased analyte charge state. Presented here is a nanospray mass spectrometry system for supercritical fluids (nSF-MS). This split flow system used small i.d. capillaries, heated interface, inline frit, and submicron emitter tips to electrospray quaternary alkyl amines solvated in supercritical CO2with a 10% methanol modifier. Analyte signal response was evaluated as a function of total system flow rate (0.5–1.5 mL/min) that is split to nanospray a supercritical fluid with linear flow rates between 0.07 and 0.42 cm/sec and pressure ranges (15–25 MPa). The nSF system showed mass-sensitive detection based on increased signal intensity for increasing capillary i.d. and analyte injection volume. These effects indicate efficient solvent evaporation for the analysis of quaternary amines. Carrier additives generally decreased signal intensity. Comparison of the nSF-MS system to the conventional SF makeup flow ESI showed 10-fold signal intensity enhancement across all the capillary i.d.s. The nSF-MS system likely achieves rapid solvent evaporation of the SF at the emitter point. The developed system combined the benefits of the nanoemitters, sCO2, and the low modifier percentage which gave rise to enhancement in MS detection sensitivity.