Online Monitoring of Small Volume Reactions Using Compact Liquid Chromatography Instrumentation.
Online Monitoring of Small Volume Reactions Using Compact Liquid Chromatography Instrumentation.
复制标题
使用紧凑的液相色谱仪器在线监测小体积反应。
DOI：
10.1002/sscp.202200012
复制
发表时间：
2022-06
影响因子：
1.1
通讯作者：
Grinias, James P
中科院分区：
文献类型：
--
作者：
Foster, Samuel W;Xie, Xiaofeng;Hellmig, Jacob M;Moura-Letts, Gustavo;West, W Raymond;Lee, Milton L;Grinias, James P
多种分析技术已用于监测化学反应，与离线分析相比，在线仪器提供了额外的好处。过去在线监测的一个挑战是将监测仪器放置在尽可能靠近反应容器的位置，以最大限度地提高采样时间分辨率并保持样品成分的完整性。此外，能够从实验室规模的反应中取样非常小的体积，允许使用小型反应容器并节省昂贵的试剂。在本研究中，紧凑型毛细管液相色谱仪器用于在线监测小至 1 mL 总体积的化学反应混合物，并直接从用于分析的反应容器自动采样 nL 级体积。分别使用串联毛细管上紫外吸光度、随后的在线 MS 检测或单独的紫外吸光度检测来进行证明短期（约 2 小时）和长期（约 50 小时）反应的分析。对于短期和长期反应（分别进样 10 次和 250 次），使用注射泵的采样方法将总体样品损失降至总反应体积的约 0.2%。
A wide variety of analytical techniques have been employed for monitoring chemical reactions, with online instrumentation providing additional benefits compared to offline analysis. A challenge in the past for online monitoring has been placement of the monitoring instrumentation as close as possible to the reaction vessel to maximize sampling temporal resolution and preserve sample composition integrity. Furthermore, the ability to sample very small volumes from bench-scale reactions allows the use of small reaction vessels and conservation of expensive reagents. In this study, a compact capillary LC instrument was used for online monitoring of as small as 1 mL total volume of a chemical reaction mixture, with automated sampling of nL-scale volumes directly from the reaction vessel used for analysis. Analyses to demonstrate short term (~2 h) and long term (~ 50 h) reactions were conducted using tandem on-capillary ultraviolet absorbance followed by in-line MS detection or ultraviolet absorbance detection alone, respectively. For both short term and long term reactions (10 and 250 injections, respectively), sampling approaches using syringe pumps minimized the overall sample loss to ~0.2% of the total reaction volume.