Coupling microextraction techniques with substrate spray mass spectrometry, towards a faster analysis of biological samples.

Direct coupling sample preparation with mass spectrometry has risen as a reliable analytical strategy in bioanalysis as it provides a high sample throughput. This approach avoids an exhaustive separation step, thus being cost-effective compared to the traditional analytical workflow. The selectivity and sensitivity levels rely on the mass spectrometric analysis and the appropriate selection of the sample preparation.

Effect of silver nanoparticles on donkey sperm parameters and ultrastructure.

The aim of this study was to determine the effect of silver nanoparticles (AgNPs) on donkey sperm parameters and ultrastructure. AgNPs were synthesized, purified and resuspended in the extender. Nine frozen-thawed donkey sperm samples were exposed to different concentrations of AgNPs (0, 1.

Humic acid-coated paper: An affordable mixed-mode weak-cation exchanger for isolating cocaine, codeine, and methadone from saliva samples for their direct infusion mass spectrometric analysis.

The use of natural materials as precursors for synthesizing sorptive phases can reduce the environmental impact of the sample preparation step. In this article, two natural materials, i.e.

On-site extraction of benzophenones from swimming pool water using hybrid tapes based on the integration of hydrophilic-lipophilic balance microparticles and an outer magnetic nanometric domain.

An on-site extraction device is presented consisting of scotch tape modified with concentric domains of micrometric hydrophilic-lipophilic balance (HLB) particles surrounded by a ring of nanometric magnetic ones. On the one hand, HLB microparticles are readily available at the surface of the tape, exposed to interact with the target analytes, being responsible for the extraction capacity of the sorptive phase. On the other hand, the presence of magnetic nanoparticles enables the attachment of the modified tape onto a metallic screw via a magnet, which is then coupled to a wireless drill, enabling the stirring of the microextraction device.

Coupling Miniaturized Stir Bar Sorptive Dispersive Microextraction to Needle-Based Electrospray Ionization Emitters for Mass Spectrometry: Determination of Tetrahydrocannabinol in Human Saliva as a Proof of Concept.

Direct coupling of sample preparation with mass spectrometry (MS) can speed up analysis, enabling faster decision-making. In such combinations, where the analysis time is mainly defined by the extraction procedure, magnetic dispersive solid-phase extraction emerges as a relevant technique because of its rapid workflow. The dispersion and retrieval of the magnetic sorbent are typically uncoupled stages, thus reducing the potential simplicity.

Sustainable beeswax modified cellulose paper for the determination of tricyclic antidepressants in biofluids.

This article describes the synthesis of sorptive phases for bioanalysis based on the modification of cellulose paper with natural beeswax as sorbent, resulting in a substrate completely renewable and sustainable. The preparation of the sorptive phases consisted of the dissolution of beeswax in hexane, followed by its drop-casting on cellulose paper and subsequent evaporation of the solvent. The beeswax modification of paper renders it hydrophobic, enabling the extraction of the target analytes, i.

Bioinspired composite packed in blunt needles, integrated microextraction and determination of oxycodone and naloxone in saliva by substrate spray mass spectrometry.

Background: Opioids are effective painkillers used for medical purposes. Their prolonged ingestion can provoke some side effects (including overdose or constipation) that are minimized by using opioid antagonists (e.g.

Sorptive tape-spray tandem mass spectrometry using aluminum foil coated with mixed-mode microparticles.

Direct mass spectrometry (MS) is an exciting strategy in bioanalysis, enabling rapid decision-making in different scenarios. Its application is usually hindered by matrix effects and the typically low concentration of the target compounds in the biofluids. In this sense, combining a previous sample preparation step minimizes or removes these shortcomings.

Nylon 6-cellulose composite hosted in a hypodermic needle: Biofluid extraction and analysis by ambient mass spectrometry in a single device.

This study proposes a hypodermic needle (HN) as a sorbent holder and an electrospray (ESI) emitter, thus combining extraction and analysis in a single device. A novel nylon 6-cellulose (N6-Cel) composite sorbent is proposed to extract methadone from oral fluid samples. The cellulosic substrate provides the composite with high porosity, permitting the flow-through of the sample, while the polyamide contributes to the extraction of the analyte.

The role of sustainable materials in sample preparation.

Sample preparation is a constantly evolving step in the measurement process with a positive effect on its performance. Its evolution has been marked by an underlying environmental commitment, with simplification, miniaturization, and automation being three of its driving forces. This trends article deepens how the sample preparation can go sustainable through the efficient design of new sorptive materials, either liquid or solid.

Volumetric absorptive microsampling for the therapeutic drug monitoring of psychiatric patients treated with cariprazine.

Psychiatric disorders are usually treated with antipsychotic agents belonging to different pharmacological and chemical classes, the most recent ones collectively known as "third-generation antipsychotics", such as cariprazine, approved in 2015 for the treatment of patients affected by schizophrenia. For these patients, a frequent therapeutic drug monitoring (TDM) becomes essential to assess compliance and to optimise and personalise their therapy, also due to cariprazine interindividual variability and narrow therapeutic range. In this study, a bioanalytical method featuring miniaturised sampling and pretreatment was developed, based on volumetric absorptive microsampling (VAMS) for TDM of psychiatric patients under cariprazine treatment and compared to a reference method based on fluid plasma analysis.

Mixed-mode cationic exchange sorptive tapes combined with direct infusion mass spectrometry for determining opioids in saliva samples.

This article describes the synthesis of mixed-mode cationic exchange (MCX) tapes as sorptive phases in bioanalysis, and it faces the determination of methadone and tramadol in saliva as the model analytical problem. The tapes are synthesized using aluminum foil as substrate, which is subsequently covered with double-sided adhesive tape where the MCX particles (ca. 1.

Deep eutectic solvent coated paper: Sustainable sorptive phase for sample preparation.

Paper-based sorptive phases have gained attention recently due to the low-cost and sustainable character of the cellulosic substrate. However, the sustainability of the resulting phase can be limited by type of coating used for analytes isolation. In this article, this limitation is overcome by using deep eutectic solvents (DES) as coating.

Icosahedral gold nanoparticles decorated with hexon protein: a surrogate for adenovirus serotype 5.

The development of synthetic particles that emulate real viruses in size, shape, and chemical composition is vital to the development of imprinted polymer-based sorbent materials (molecularly imprinted polymers, MIPs). In this study, we address surrogates for adenovirus type 5 (Adv 5) via the synthesis and subsequent modification of icosahedral gold nanoparticles (iAuNPs) decorated with the most abundant protein of the Adv 5 (i.e.

Polydopamine inner wall-coated hypodermic needle as microextraction device and electrospray emitter for the direct analysis of illicit drugs in oral fluid by ambient mass spectrometry.

In this article, polydopamine inner wall-coated hypodermic needles (PDA-HNs) are evaluated as both microextraction devices and electrospray ionization (ESI) emitters for determining selected illicit drugs (methamphetamine, cocaine, and methadone) in oral fluid samples. The PDA film, located in the inner wall of the needle, allows the extraction of the analytes at alkaline pH, where their hydrophobic character is promoted. The extracted analytes are finally eluted in a methanol/formic acid mixture that also acts as ESI solution.

Potential of hydrophobic paper-based sorptive phase prepared by in-situ thermal imidization for the extraction of methadone from oral fluid samples.

Paper-based sorptive phases (PSPs) are functional planar materials with a demonstrated potential in analytical sample preparation. This article describes the synthesis of a polyimide coated paper by an in-situ imidization at a high temperature. Polyimides (PI) are synthesized in two subsequent steps where a hydrophilic polymer, in this case, poly(amic acid) (PAA), is formed as an intermediate product.

Advanced polymeric solids containing nano- and micro-particles prepared via emulsion-based polymerization approaches. A review.

This review critically summarizes the latest contributions in the preparation of advanced nano/microparticle-contained polymers from emulsions. The nano- or micro-particles can be dispersed in the phase where the polymerization reaction takes place and, consequently, once the solid is formed, the particles are embedded in the final polymeric structure. This results in the formation of hybrid materials, which combine the unique properties of nano/micro-particles with the inherent properties of the polymers (which depend mainly on the selected monomers).

Polydopamine coated hypodermic needles as a microextraction device for the determination of tricyclic antidepressants in oral fluid by direct infusion MS/MS.

In-needle microextraction consists of the confinement of the sorbent, by coating or packing, inside a metallic needle. The size of the needles reduces the eluent requirements providing an efficient preconcentration of the analytes. In this work, hypodermic needles coated with polydopamine (PDA) are presented as microextraction devices to isolate six tricyclic antidepressants from oral fluid samples.

Pre-cleaned bare wooden toothpicks for the determination of drugs in oral fluid by mass spectrometry.

This article deepens the potential of pre-cleaned bare wooden toothpicks (pb-WTs) for extracting drugs (antidepressants and acetaminophen) from oral fluid samples. The leaching of the intrinsic compounds from the wood matrix is identified as the main challenge for the final determination of the targets, even when a very selective instrumental technique, such as mass spectrometry, is employed. The pre-cleaning of the WTs is proposed for improving the analytical performance.

Portable stirring device for the on-site extraction of environmental waters using magnetic hydrophilic-lipophilic balance tape.

The spatial heterogeneity of environmental systems makes sampling at multiple locations crucial to provide complete and representative information. The on-site application of an extraction technique simplifies the sampling logistics, increasing sample integrity during transportation and storage. This article presents a portable, simple, and low-cost device capable of performing the simultaneous on-site extraction of several environmental water samples.

A paper-based polystyrene/nylon Janus platform for the microextraction of UV filters in water samples as proof-of-concept.

A new mix-mode cellulose-based sorptive phase is described that combines two different polymeric domains (i.e., nylon and polystyrene), thus providing simultaneous hydrophilic and hydrophobic features as a result.

Wooden-based materials: Eco-friendly materials for direct mass spectrometric analysis and microextraction.

Lignocellulosic materials have arisen as a sustainable alternative in microextraction techniques during the last 10 years. As they are natural materials, their use fits into some of the principles of Green Analytical Chemistry. Their inherent porosity, narrow shape, and rigidity permit their use in ambient ionization mass spectrometry techniques.

Carbon fibers as green and sustainable sorbent for the extraction of isoflavones from environmental waters.

Isoflavones are a group of phytoestrogens of important environmental concern due to their endocrine disrupting effects. This article presents a rapid, green, and sustainable method for determining four isoflavones (daidzein, genistein, formononetin, and biochanin A) in environmental waters complying with current trends in Analytical Chemistry. The method consists of in-syringe dispersive solid-phase extraction (DSPE) as the extraction approach, using carbon fibers as extraction material.