In this paper, an approach to fabricate epoxy or polystyrene microdevices with encapsulated tubing and electrodes is described. Key features of this approach include a fixed alignment between the fluidic tubing and electrodes, the ability to polish the device when desired, and the low dead volume nature of the fluidic interconnects. It is shown that a variety of tubing can be encapsulated with this approach, including fused silica capillary, polyetheretherketone (PEEK), and perfluoroalkoxy (PFA), with the resulting tubing/microchip interface not leading to significant band broadening or plug dilution. The applicability of the devices with embedded tubing is demonstrated by integrating several off-chip analytical methods to the microchip. This includes droplet transfer, droplet desegmentation, and microchip-based flow injection analysis. Off-chip generated droplets can be transferred to the microchip with minimal coalescence, while flow injection studies showed improved peak shape and sensitivity when compared to the use of fluidic interconnects with an appreciable dead volume. Importantly, it is shown that this low dead volume approach can be extended to also enable the integration of conventional capillary electrophoresis (CE) with electrochemical detection. This is accomplished by embedding fused silica capillary along with palladium (for grounding the electrophoresis voltage) and platinum (for detection) electrodes. With this approach, up to 128,000 theoretical plates for dopamine was possible. In all cases, the tubing and electrodes are housed in a rigid base; this results in extremely robust devices that will be of interest to researchers wanting to develop microchips for use by non-experts.
Interfacing of microfluidic devices to mass spectrometry has challenges including dilution from sheath liquid junctions, fragile electrodes, and excessive dead volumes which prevent optimum performance and common use. The goal of this work is to develop a stable nanospray chip-MS interface that contains easily integrated electrodes and an embedded capillary emitter to mitigate current chip-MS problems. This system uses a hybrid polystyrene-poly(dimethylsiloxane) (PS-PDMS) microfluidic platform with an embedded electrode and integrated capillary emitter used as the nanospray interface. Two chip designs were used to evaluate the performance, illustrate on-chip reaction capabilities. By direct infusion, this system showed good performance with LODs of GSH and caffeine of 9 nM and 1 nM, R2 of 0.996 and 0.992 and sensitivity of 12 counts/nM and 332 counts/nM over a linear dynamic range of 40 nM to 50 μM and 1 to 50 μM respectively. A reaction was performed on the chip with syringe pumps showing the oxidation of glutathione (GSH) to oxidized glutathione (GSSG) using H2O2. The on-chip reaction of GSH oxidation to GSSG, with online-MS detection, successfully demonstrate the stability and robustness of the nanospray interface.
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