School of Municipal and Environmental Engineering, Harbin Institute of Technology, Harbin 150090, China; State Key Laboratory of Urban Water Resource and Environment, Harbin Institute of Technology, Harbin 150090, China.
School of Environmental Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China.
Anal Chim Acta. 2018 Jul 12;1013:36-42. doi: 10.1016/j.aca.2018.01.052. Epub 2018 Feb 3.
A simple method by coupling a spray capillary with pressurized photoreactor for on-line monitoring of photolysis reactions was reported. In this method, only an inert gas is used to transfer the reaction solution, which avoids potential sample loss and contamination. The photolysis reaction is online quenched, and therefore, it has advantages of on-line detection and characterization of photolysis reaction intermediates. The assembly is easy to achieve, low-cost, and robust. Different from off-line methods, the photolysis reaction solution is directly transferred to a capillary tip for ionization, avoiding the delay in the detection of reactive intermediates. With this setup, this technique has been applied for on-line monitoring of degradation of cyclophosphamide (CP) in HO/UV for which two new intermediates were intercepted and structurally characterized for the first time by tandem mass spectrometry. In HO/UV, the degradation of CP occurred via hydroxylation, dehydrogenation, chlorine substitution reaction, and cleavage of the chloroethyl group. These results indicate that the coupling of electrospray ionization mass spectrometry with pressurized photoreactor can detect and characterize the key photolysis reaction intermediates, which render it a potential tool for elucidating the mechanism of water remediation.
本文报道了一种将喷雾毛细管与加压光反应器偶联，用于在线监测光解反应的简单方法。在该方法中，仅使用惰性气体来转移反应溶液，从而避免了潜在的样品损失和污染。光解反应在线猝灭，因此具有在线检测和表征光解反应中间体的优点。该组件易于实现、成本低且坚固耐用。与离线方法不同，将光解反应溶液直接转移到毛细管尖端进行电离，避免了对反应中间体检测的延迟。使用该装置，本技术已成功应用于在线监测 HO/UV 中环磷酰胺（CP）的降解，首次通过串联质谱拦截并结构表征了两种新的中间体。在 HO/UV 中，CP 的降解通过羟化、脱氢、氯取代反应和氯乙基基团的裂解发生。这些结果表明，电喷雾电离质谱与加压光反应器的耦合可以检测和表征关键的光解反应中间体，这使其成为阐明水修复机制的潜在工具。
