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Comprehensive Summary: A monolithic column‐based mass spectrometry (MS) analysis kit was prepared for whole blood analysis with MS. The kit is disposable and can be used for purification, storage, transportation and direct analysis of whole blood. The kit mainly consists of a capillary for quantitative microsampling, a cation exchange monolithic column for purification and storage, and a syringe for loading sample. This kit is very friendly to various users that one can easily siphon the blood in the kit followed by rapid clean‐up. We established a quantitative method using the kit with a limit detection as low as 0.33 nmol/L, and achieved more than five orders of magnitude enhancement in sensitivity compared to direct nanoelectrospray ionization MS analysis. The column can avoid analyte exposure to environment, which helps the storage of the sample for laboratory analysis. The relative standard deviation of immediate blood analysis and storage blood analysis within 10 d was less than 10%. This method has been successfully applied to the quantitative analysis of procainamide hydrochloride in 2 μL rat blood. These results indicate that this disposable kit does have the potential to achieve highly sensitive quantitative MS analysis in biological samples, which is expected to become a cost‐effective and powerful tool for in vitro diagnostics. [ABSTRACT FROM AUTHOR]

The in‐depth study of electrochemical (EC) synthesis can require a powerful mass spectrometry (MS) analytical platform which can discover and identify fleeting intermediates in EC reactions. Here we report a floating electrolytic electrospray ionization (FE‐ESI) strategy that can perform EC processes in a floating electrolytic cell and monitor intermediates by high‐resolution MS. Compared with previous EC‐MS methods, a significant advantage of FE‐ESI‐MS is that it allows one to modulate the electrolytic and electrospray process individually, ensuring its high sensitivity in discovering intermediates and universality to investigate redox reactions in different scenarios. This powerful platform has been successfully used to investigate the EC reductive coupling of p‐tolylboronic acid and p‐nitrotoluene. A series of nitrene intermediates were discovered and identified by FE‐ESI‐MS, indicating that a hidden mechanism involving nitrene formation might play a key role in EC reductive coupling process. [ABSTRACT FROM AUTHOR]

Comprehensive Summary: A monolithic column‐based mass spectrometry (MS) analysis kit was prepared for whole blood analysis with MS. The kit is disposable and can be used for purification, storage, transportation and direct analysis of whole blood. The kit mainly consists of a capillary for quantitative microsampling, a cation exchange monolithic column for purification and storage, and a syringe for loading sample. This kit is very friendly to various users that one can easily siphon the blood in the kit followed by rapid clean‐up. We established a quantitative method using the kit with a limit detection as low as 0.33 nmol/L, and achieved more than five orders of magnitude enhancement in sensitivity compared to direct nanoelectrospray ionization MS analysis. The column can avoid analyte exposure to environment, which helps the storage of the sample for laboratory analysis. The relative standard deviation of immediate blood analysis and storage blood analysis within 10 d was less than 10%. This method has been successfully applied to the quantitative analysis of procainamide hydrochloride in 2 μL rat blood. These results indicate that this disposable kit does have the potential to achieve highly sensitive quantitative MS analysis in biological samples, which is expected to become a cost‐effective and powerful tool for in vitro diagnostics. [ABSTRACT FROM AUTHOR]