Electroosmotic flow in fused deposition modeling (FDM) 3D-printed microchannels.

Electroosmotic flow (EOF) was determined in tridimensional (3D)-printed microchannels with dimensions smaller than 100 µm. Fused deposition modeling 3D printing using thermoplastic filaments of PETG (polyethylene terephthalate glycol), PLA (polylactic acid), and ABS (acrylonitrile butadiene styrene) were used to fabricate the microchannels. The current monitoring method and sodium phosphate solutions at different pH values (3-10) were used for the EOF mobility (µEOF ) measurements, which ranged from 2.00 × 10-4 to 12.52 × 10-4  cm2  V-1  s-1 . The highest and the smallest µEOF were obtained for the PLA and PETG microchannels, respectively. Adding the cationic surfactant cetyltrimethylammonium bromide to the sodium phosphate solution caused EOF direction reversion in all the studied microchannels. The obtained results can be interesting for developing 3D-printed microfluidic devices, in which EOF is relevant.

Microfluidic devices based on textile threads for analytical applications: state of the art and prospects.

Microfluidic devices based on textile threads have interesting advantages when compared to systems made with traditional materials, such as polymers and inorganic substrates (especially silicon and glass). One of these significant advantages is the device fabrication process, made more cheap and simple, with little or no microfabrication apparatus. This review describes the fundamentals, applications, challenges, and prospects of microfluidic devices fabricated with textile threads. A wide range of applications is discussed, integrated with several analysis methods, such as electrochemical, colorimetric, electrophoretic, chromatographic, and fluorescence. Additionally, the integration of these devices with different substrates (e.g., 3D printed components or fabrics), other devices (e.g., smartphones), and microelectronics is described. These combinations have allowed the construction of fully portable devices and consequently the development of point-of-care and wearable analytical systems.

Ready-to-use 3D-printed electrochemical cell for in situ voltammetry of immobilized microparticles and Raman spectroscopy.

We report in this communication a ready-to-use fused deposition modeling (FDM) based 3D-printed spectroelectrochemical cell to perform for the first time voltammetry of immobilized microparticles (VIMP) and Raman spectroscopy in situ using acrylonitrile butadiene styrene (ABS) as the filament material for printing. The 3D-printed cell was applied to evaluate solid state electrochemical behavior of tadalafil as a proof-of-concept. Several advantages were achieved in the use of the developed device, such as less manipulation of the working electrode, monitoring the same region of the solid microparticles before and after electrochemical measurements, better control of the laser incidence, low-cost and low-time production. Furthermore, the device was printed in a single-step, without handling to assembly and it has an estimated material cost of approximately 2 $. The use of 3D-printing technology was significantly important to integrate Raman spectroscopic method with VIMP measurements and to support mechanism elucidation and characterization of the compounds with less manipulation of the working electrode, avoiding loss of solid products formed from electrochemical reactions.

Microchip Electrophoresis Containing Electrodes for Integrated Electrochemical Detection.

Microchip electrophoresis is a versatile separation technique. Electrochemical detection is suitable to apply to microdevices due to its easy integration to the fabrication process and good sensitivity and selectivity. Here we describe the procedures to prepare Pt band electrodes deposited on glass to couple to polydimethylsiloxane (PDMS) microchips aiming the separation and detection of nitrite using an isolated potentiostat.

Electromembrane extraction and preconcentration of carbendazim and thiabendazole in water samples before capillary electrophoresis analysis.

Electromembrane extraction using a polypropylene hollow fiber impregnated with 1-ethyl-2-nitrobenzene was evaluated for the extraction and preconcentration of the fungicides thiabendazole and carbendazim from water samples before capillary electrophoresis analysis. The composition of the supported liquid membrane, the HCl concentration in the acceptor solution, and the stirring rate (of the donor solution) were optimized using the one-variable-at-a-time method. In contrast, a face-centered central composition design was used for optimization of voltage, extraction time, and concentration of HCl in the donor solution. After optimization, electromembrane extraction provided enrichment factors of 50 and 26 for thiabendazole and carbendazim that allowed us to achieve limits of detection of 1.1 and 2.3 µg/L, respectively. Repeatability (intraday precision) expressed as the relative standard deviation varied from 2.5 to 2.8%, while the interday precision ranged from 3.1 to 3.3%. The proposed method was applied for analysis of samples of tap and river water, and acceptable precision and accuracy were attained.

A simple method for determination of erythritol, maltitol, xylitol, and sorbitol in sugar-free chocolates by capillary electrophoresis with capacitively coupled contactless conductivity detection.

In this work, a novel and simple analytical method using capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C4 D) is proposed for the determination of the polyols erythritol, maltitol, xylitol, and sorbitol in sugar-free chocolate. CE separation of the polyols was achieved in less than 6 min, and it was mediated by the interaction between the polyols and the borate ions in the background electrolyte, forming negatively charged borate esters. The extraction of the polyols from the samples was simply obtained using ultra-pure water and ultrasonic energy. Linearity was assessed by calibration curves that showed R2 varying from 0.9920 to 0.9976. The LOQs were 12.4, 15.9, 9.0, and 9.0 µg/g for erythritol, maltitol, xylitol, and sorbitol, respectively. The accuracy of the method was evaluated by recovery tests, and the obtained recoveries varied from 70 to 116% with standard deviations ranging from 0.2 to 19%. The CE-C4 D method was successfully applied for the determination of the studied polyols in commercial samples of sugar-free chocolate.

Determination of tetrakis(hydroxymethyl)phosphonium sulfate in commercial formulations and cooling water by capillary electrophoresis with contactless conductivity detection.

A novel capillary electrophoresis method using capacitively coupled contactless conductivity detection is proposed for the determination of the biocide tetrakis(hydroxymethyl)phosphonium sulfate. The feasibility of the electrophoretic separation of this biocide was attributed to the formation of an anionic complex between the biocide and borate ions in the background electrolyte. Evidence of this complex formation was provided by (11) B NMR spectroscopy. A linear relationship (R(2) = 0.9990) between the peak area of the complex and the biocide concentration (50-900 µmol/L) was found. The limit of detection and limit of quantification were 15.0 and 50.1 µmol/L, respectively. The proposed method was applied to the determination of tetrakis(hydroxymethyl)phosphonium sulfate in commercial formulations, and the results were in good agreement with those obtained by the standard iodometric titration method. The method was also evaluated for the analysis of tap water and cooling water samples treated with the biocide. The results of the recovery tests at three concentration levels (300, 400, and 600 µmol/L) varied from 75 to 99%, with a relative standard deviation no higher than 9%.

Recent advances in low-cost microfluidic platforms for diagnostic applications.

The use of inexpensive materials and cost-effective manufacturing processes for mass production of microfluidic devices is very attractive and has spurred a variety of approaches. Such devices are particularly suited for diagnostic applications in limited resource settings. This review describes the recent and remarkable advances in the use of low-cost substrates for the development of microfluidic devices for diagnostics and clinical assays. Thus, a plethora of new and improved fabrication methods, designs, capabilities, detections, and applications of microfluidic devices fabricated with paper, plastic, and threads are covered.

Toner and paper-based fabrication techniques for microfluidic applications.

The interest in low-cost microfluidic platforms as well as emerging microfabrication techniques has increased considerably over the last years. Toner- and paper-based techniques have appeared as two of the most promising platforms for the production of disposable devices for on-chip applications. This review focuses on recent advances in the fabrication techniques and in the analytical/bioanalytical applications of toner and paper-based devices. The discussion is divided in two parts dealing with (i) toner and (ii) paper devices. Examples of miniaturized devices fabricated by using direct-printing or toner transfer masking in polyester-toner, glass, PDMS as well as conductive platforms as recordable compact disks and printed circuit board are presented. The construction and the use of paper-based devices for off-site diagnosis and bioassays are also described to cover this emerging platform for low-cost diagnostics.

Fast determination of ethambutol in pharmaceutical formulations using capillary electrophoresis with capacitively coupled contactless conductivity detection.

A method for the determination of ethambutol (EMB), a first-line drug against tuberculosis, based on CE with capacitively coupled contactless conductivity detection is proposed. The separation of EMB and its main product of degradation were achieved in less than 3 min with a resolution of 2.0 using a BGE composed of 50 mmol/L histidine and 30 mmol/L MES, pH 6.30. By raising the pH to 8.03, the analysis time was reduced to 1.0 min, but with a significant loss of resolution (0.7). Using the best separation conditions, linearity of 0.9976 (R(2), five data points), sensitivity of 1.26x10(-4) V min mumol(-1) L, and LOD and quantification of 23.5 and 78.3 mumol/L, respectively, were obtained. Recoveries at four levels of concentration ranged from 95 to 102% and the concentration range studied ranged from 100 to 500 mumol/L. The results obtained for the determination of EMB in pharmaceutical formulations were compared with those obtained by using CE with photometric detection.

Fabrication of a multichannel PDMS/glass analytical microsystem with integrated electrodes for amperometric detection.

The fabrication process of novel multichannel microfluidic devices with integrated electrodes for amperometric detection is described. Soft-lithography, lift-off and O(2) plasma surface activation sealing techniques were employed for rapid prototyping of cost effective PDMS/glass microchips. The capabilities of the proposed microdevices were demonstrated by the electrooxidation of hydroquinone and N-acetyl-p-aminophenol (APAP) on a Au working electrode at +800 mV and +700 mV, respectively, against a Au pseudo reference electrode, and of thiocyanate on a Cu working electrode at +700 mV against a Ag/AgCl (KCl saturated) reference electrode. Linear response over the range up to 1.0 mmol L(-1) for APAP and up to 4.0 mmol L(-1) for hydroquinone and thiocyanate were verified through calibration curves with correlation coefficients greater than 0.97 (minimum of five data points). The sensitivities for hydroquinone, thiocyanate, and APAP were 28, 19, and 78 microA mol(-1) L, respectively. Under the experimental conditions used, the estimated limits of detection were 0.21, 0.95, and 0.12 mmol L(-1) for hydroquinone, thiocyanate and APAP, respectively. The geometries of the devices were designed to allow fast calibration procedures and reliable results for in-field applications. Exerting a strong influence over the device performance, the sealing process was greatly enhanced by depositing auxiliary TiSiO(2) thin-films. The general performance of the system was verified by amperometric assays of N-acetyl-p-aminophenol standard solutions, and the influences exerted by the present fabrication methods regarding reproducibility and reliability are addressed. The proposed device was successfully applied in the determination of the concentration of APAP in two commercial formulations.

Extending the lifetime of the running electrolyte in capillary electrophoresis by using additional compartments for external electrolysis.

The use of two additional reservoirs to accommodate the electrodes of the power source is proposed to improve the stability of the running electrolyte in capillary electrophoresis. The basic idea is to use salt bridges to connect those reservoirs to the ones containing the capillary ends. Although simple, there are several issues that can be considered in the design and implementation of such system in order to prevent undesired transference of material between the electrolysis and the main reservoirs. The use of a sealed electrolysis reservoir without a gas phase, the use of materials that ensure volume stability, and the use of bridges as long as possible are three basic directions. A compromise is involved in the dimensions of the sectional area of the bridge, because a small area diminishes the amount of a species transferred by diffusion but leads to an undesirable increase of the electrical field during the electrophoretic running. Thus, a bridge composed of a main wide-bore tube connected to a small-bore capillary seems to give the best performance for practical use. A simple electrolysis-separated system was adapted to a preexisting capillary electrophoresis system, and its performance was evaluated with a mixture of tartaric, malic, and succinic acids that was separated in sodium benzoate solution (pH 5.5) using the original equipment and the modified one. Due to the water electrolysis and the small buffering capacity of the electrolyte, there was a significant pH change and consequently changes in the effective mobilities of the analytes and loss of resolution after a few runs using the original equipment. Using the electrolysis-separated system, no significant change in the migration time and resolution was observed even after 15 runs. Besides the freedom to prepare running electrolytes with electroactive species or unbuffered solution, high throughput and the use of small reservoirs, such as the ones used in microfluidic devices, are the main advantages of the system.