Digital microfluidics platform for interfacing solid-liquid extraction column with portable capillary electropherograph for analysis of soil amino acids.

In this work, the concept of a field-portable analyzer is proposed that operates with milliliter amounts of solvents and samples. The need to develop such an analyzer is not only driven by specific extraterrestrial analysis but also, for example, by forensics applications where the amount of liquid that can be taken to the field is severely limited. The prototype of the proposed analyzer consists of a solid-liquid extractor, the output of which is connected to the micropump, which delivers droplets of extracts to digital microfluidic platform (DMFP). In this way, world-to-chip interfacing is established. Further, the sample droplets are transported to CE capillary inlet port, separated and detected via a contactless conductivity detector. Working buffers and other solvents needed to perform CE analysis are also delivered as droplets to the DMFP and transported through the CE capillary. The performance of the analyzer is demonstrated by analysis of amino acids in sand matrices. The recovery of the spiked amino acids from the inert sand sample was from 34 to 51% with analysis LOD from 0.2 to 0.6 ppm and migration time RSD from 0.2 to 6.0%.

Digital microfluidic sampler for a portable capillary electropherograph.

A new sample introduction/analysis approach was developed by combining a digital microfluidic (DMF) device with a portable capillary electrophoresis (CE) analyzer based on short separation capillary and contactless conductivity detection. The DMF sample injection was performed by transporting sample and buffer droplets in succession under the CE capillary inlet end allowing the capillary to be immersed into the sample/buffer droplet, and CE separation was performed by applying a high voltage between the (grounded) buffer droplet and CE outlet reservoir. Electrowetting on dielectric (EWOD) phenomenon was used for droplets actuation. With the use of the DMF sampler, CE separation of a mixture of vitamins was achieved. A droplet evaporation process with simultaneous concentration of sample in the droplet was monitored. It was found that the concentration process closely followed the theoretically predicted function.

A portable capillary electropherograph equipped with a cross-sampler and a contactless-conductivity detector for the detection of the degradation products of chemical warfare agents in soil extracts.

A fully portable CE device equipped with a capacitively coupled contactless-conductivity detector and a cross-injection device is put to the test in laboratory conditions. The portable device is capable of working on batteries for at least 4 h. After that, its performance is strongly affected by the drop in the high-voltage output and analysis may be interrupted if its length exceeds a reasonable time. The concentration of the BGE affects both ionic strength and conductivity. Choosing an optimal concentration of BGE is therefore about finding a good compromise between selectivity and sensitivity. All experiments were performed using a mixture of histidine and MES with a concentration of 15 mM as BGE. The performance of the cross-injection device is optimized by the use of internal standards. Satisfactory reproducibility is gained as the RSD of peak areas is reduced to 8% or less. LODs for different phosphonic acids are in the range of 2.5-9.7 microM. For the analysis of adsorption of phosphonic acids in sand and loamy soil samples, calibration curves are constructed. Linearity in a measured concentration range of 10-100 microM is excellent, as the squares of correlation constants are approximately 1. The concentration analysis of phosphonic acids in soil extracts demonstrates that their adsorption curves in sand and loamy soil follow different adsorption isotherms.

Fraction collection in capillary electrophoresis for various stand-alone mass spectrometers.

A procedure for collecting fractions during capillary electrophoresis for their analysis using various stand-alone instruments is described. The results of a systematic study of the optimization and application of capillary electrophoresis (CE) in conjunction with a reverse-phase high-performance liquid chromatography electrospray ionization quadrupole time of flight-tandem mass spectrometry (RP-HPLC-ESI-Q-TOF-MS/MS) and inductively-coupled mass spectrometry (ICP-MS) to the analysis of the seed extract of the Japanese Pagoda Tree (Sophora japonica) are presented. The off-line coupling of CE to the matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF-MS) for the proteins mixture was applied. The cathode end of the capillary was placed inside a stainless steel needle using a coaxial liquid-sheath-flow configuration. The optimization of experimental parameters resulted in an efficient methodology for MS analysis of fractions. Several components contained in the extract of S. japonica were identified, some not previously known. It was demonstrated that low sensitivity, which is a real problem in off-line CE-MS analysis, could be tolerated because of a more flexible optimization of the CE separation conditions and the choice of independent stand-alone instruments for analysis of separated fractions. The estimated limit of detection for CE-RP-HPLC-ESI-Q-TOF-MS was 50 microM of polyphenols and for CE-ICP-MS, 1-100 microg/l.