Anna Hogan

Timely detection of organophosphates in outdoor environments remains a critical challenge for forensic and environmental monitoring. Traditional methods often require transporting samples to centralised laboratories, delaying essential response actions. In this study, we present a novel mobile analytical chemistry workstation that integrates capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C4D) on low-cost polydimethylsiloxane (PDMS) microfluidic chips, enabling rapid and accurate on-site analysis of organophosphates. The system features a streamlined workflow that includes in-field sample collection, microfluidic analysis, and the wireless transmission of data to a central command centre for immediate decision-making. The detection system demonstrates a linear range of 2.5 mM to 20 mM for dimethyl methylphosphonate (DMMP), with an estimated limit of detection (LOD) of 2.5 mM. We evaluate the feasibility of combining CE and C4D under field conditions, highlighting both the strengths and limitations of this integrated platform.

Polychlorinated biphenyls (PCBs) have been found in soil, which has typically been the result of industrial pollution in the past two decades. Although they are banned, PCBs can still be found in soils and other environmental media. For this reason, it is critical to develop an analytical method that can reliably identify and monitor their sources. This study describes a gas chromatography with mass spectrometry (GC-MS) technique, which was used to detect PCBs in soil samples by using a fast extraction method. Using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, PCBs were more effectively extracted from soil. Different related parameters, such as time of shaking and centrifuging, type of solvent, and clean-up adsorbents, were compared and optimized. As the extraction solvent, acetonitrile/water produced the best results, and as the dispersive solid-phase extraction sorbent, diatomaceous earth produced the best results. Procedures allowed recovery values between 95.3% and 103.2%. A limit of detection of 1.9 µg/kg was determined with relative standard deviations (n = 3) of 2.1–4.0% for intra-day assays and 3.6–5.8% for inter-day assays. It was demonstrated that the method was simple, sensitive, efficient, and environmentally friendly when applied to soil samples. To our knowledge, an integrated approach based on QuEChERS for the determination of Aroclor 1254 in soil has not been published before. It is believed that this approach will eliminate the significant challenge of sample extraction in GC-MS processing, which was considered to be a procedural challenge in previous analyses.

A rapid, sensitive method for the separation of catecholamine biomarkers (CAs), of importance in traumatic brain injury (TBI) and in Parkinson’s disease (PD), has been successfully developed using hydrophilic interaction liquid chromatography (HILIC). Dopamine (DA), epinephrine (EPI), and norepinephrine (NE) are known to be three to fivefold elevated above normal in traumatic brain injury (TBI) patients. HILIC facilitates the rapid and efficient separation of these polar biomarkers, which can be poorly retained by reversed-phase liquid chromatography (RPLC), while electrochemical detection (ECD) at the boron-doped diamond (BDD) electrode provides enhanced nanomolar detection. Three HILIC columns were compared, namely the superficially porous (core-shell) Z-HILIC column and the Z-cHILIC and Z-HILIC fully porous columns. The core-shell Z-HILIC showed the highest efficiency with a rapid separation within 60 s. The HILIC method utilizing the core-shell Z-HILIC column was initially optimized for the simultaneous analysis of DA, EPI, and NE using UV detection. The advantages of using the BDD electrode over UV detection were explored, and the improved limits of detection (LODs, S/N = 3) measured were 40, 50, and 50 nM for DA, EPI, and NE, respectively. Method validation is reported in terms of the linearity, repeatability, reproducibility, and LODs. Furthermore, the proposed method was successfully applied to the real sample analysis of urinary CAs following phenylboronic acid (PBA) solid phase extraction (SPE) pretreatment.

Capillary electrochromatography (CEC) is a separation technique that hybridizes liquid chromatography (LC) and capillary electrophoresis (CE). The selectivity offered by LC stationary phase results in rapid separations, high efficiency, high selectivity, minimal analyte and buffer consumption. Chip-based CE and CEC separation techniques are also gaining interest, as the microchip can provide precise on-chip control over the experiment. Capacitively coupled contactless conductivity detection (C⁴D) offers the contactless electrode configuration, and thus is not in contact with the solutions under investigation. This prevents contamination, so it can be easy to use as well as maintain. This study investigated a chip-based CE/CEC with C⁴D technique, including silicon-based microfluidic device fabrication processes with packaging, design and optimization. It also examined the compatibility of the silicon-based CEC microchip interfaced with C⁴D. In this paper, the authors demonstrated a nanofabrication technique for a novel microchip electrochromatography (MEC) device, whose capability is to be used as a mobile analytical equipment. This research investigated using samples of potassium ions, sodium ions and aspirin (acetylsalicylic acid).

Alkaline phosphatase (ALP) is one of the main biomarkers that is clinically detected in bone and liver disorders using optical assays. The electrochemical principle is important because point-of-care testing is increasing dramatically and absorbance techniques hardly compete with the medical revolution that is occurring. The detection of ALP using electrochemical detection is contributing to the integration systems field, and hence enhancing the detection of biological targets for pharmaceutical research and design systems. Moreover, in vitro electrochemical measurements use cost effective materials and simple techniques. Graphite screen-printed electrodes and linear sweep voltammetry were used to optimize the electrochemistry of the enzymatic product p-aminophenol using the enzyme kinetic assay. ALP release from embryonic and cancer cells was determined from adhesion cell culture. Additionally, capillary electrophoresis and colorimetric methods were applied for comparison assays. The resulting assays showed a dynamic range of ALP ranging from 1.5 to 1500 U/L, and limit of detection of 0.043 U/L. This was achieved by using 70 μL of the sample and an incubation time of 10 min at an optimal substrate concentration of 9.6 mM of p-aminophenol phosphate. A significant difference (p < 0.05) was measured between the absorbance assays. This paper demonstrates the advantages of the electrochemical assay for ALP release from cells, which is in line with recent trends in gene expression systems using microelectrode array technologies and devices for monitoring electrophysiological activity.