High-Throughput Analysis from Complex Matrices: Acoustic Ejection Mass Spectrometry from Phase-Separated Fluid Samples

Acoustic ejection mass spectrometry is a novel high-throughput analytical technology that delivers high reproducibility without carryover observed. It eliminates the chromatography step used to separate analytes from matrix components. Fully-automated liquid–liquid extraction is widely used for sample cleanup, especially in high-throughput applications. We introduce a workflow for direct AEMS analysis from phase-separated liquid samples and explore high-throughput analysis from complex matrices. We demonstrate the quantitative determination of fentanyl from urine using this two-phase AEMS approach, with a LOD lower than 1 ng/mL, quantitation precision of 15%, and accuracy better than ±10% over the range of evaluation (1–100 ng/mL). This workflow offers simplified sample preparation and higher analytical throughput for some bioanalytical applications, in comparison to an LC-MS based approach.

Recent Applications of Derivatization Techniques for Pharmaceutical and Bioanalytical Analysis through High-Performance Liquid Chromatography

Background: Derivatization of analytes is a quite convenient practice from an analytical perspective. Its vast prevalence is accounted by the availability of distinct reagents, primarily pragmatic for obtaining desired modifications in an analyte structure. Another reason for its handiness is typically to overcome limitations such as lack of sensitive methodology or instrumentation.The past decades have witnessed various new derivatization techniques including in-situ, enzymatic, ultrasound-assisted, microwave-assisted, and photochemical derivatization which have gain popularity recently. Methods: The online literature available on the utilization of derivatization as prominent analytical tools in recent years with typical advancements is reviewed. The illustrations of the analytical condition together with the structures of different derivatizing reagents (DRs) are provided to acknowledge the vast capability of derivatization to resolve analytical problems. Results: The derivatization techniques have enabled analytical chemists throughout the globe to develop an enhanced sensitivity method with the simplest of the instrument like High-Performance Liquid Chromatography (HPLC). The HPLC, compared to more sensitive Liquid chromatography coupled to tandem mass spectrometer, is readily available and can be readily utilized for routine analysis in fields of pharmaceuticals, bioanalysis, food safety, and environmental contamination. A troublesome aspect of these fields is the presence of a complex matrix with trace concentrations for analyses. Liquid chromatographic methods devoid of MS detectors do not have the desired sensitivity for this. A possible solution for overcoming this is to couple HPLC with derivatization to enable the possibility of detecting trace analytes with a less expensive instrument. Running cost, enhanced sensitivity, low time consumption, and overcoming the inherent problems of analyte are critical parameters for which HPLC is quite useful in high throughput analysis. Conclusion: The review critically highlights various kinds of derivatization applications in different fields of analytical chemistry. The information primarily focuses on pharmaceutical and bioanalytical applications in recent years. The various modes, types, and derivatizing reagents with brief mechanisms have been ascribed briefly Additionally, the importance of HPLC coupled to fluorescence and UV detection is presented as an overview through examples accompanied by their analytical conditions.

Cost Effective Silver Nanowire-Decorated Graphene Paper for Drop-on SERS Biodetection

The use of SERS for real-world bioanalytical applications represents a concrete opportunity, which, however, is being largely delayed by the inadequacy of existing substrates used to collect SERS spectra. In particular, the main bottleneck is their poor usability, as in the case of unsupported noble metal colloidal nanoparticles or because of the need for complex or highly specialized fabrication procedures, especially in view of a large-scale commercial diffusion. In this work, we introduce a graphene paper-supported plasmonic substrate for biodetection as obtained by a simple and rapid aerosol deposition patterning of silver nanowires. This substrate is compatible with the analysis of small (2 μL) analyte drops, providing stable SERS signals at sub-millimolar concentration and a detection limit down to the nanogram level in the case of hemoglobin. The presence of a graphene underlayer assures an even surface distribution of SERS hotspots with improved stability of the SERS signal, the collection of well-resolved and intense SERS spectra, and an ultra-flat and photostable SERS background in comparison with other popular disposable supports.