Carbonyl compounds responsive 2,4-dinitrophenylhydrazine doped polydimethylsiloxane based membrane as alternative derivatizing strategy prior to in-tube solid phase microextraction coupled with capillary liquid chromatography analysis.

In this work, a DNPH doped PDMS based membrane was developed to facilitate carbonyl compound derivatization. This membrane delivers DNPH in presence of carbonyl compounds to form hydrazones. Subsequently, the resulting hydrazones are preconcentrated, separated and detected by in-tube solid phase microextraction (IT-SPME) coupled on-line with capillary liquid chromatography (CapLC) with Uv-Vis diode array detection (DAD).

Assessing the size transformation of nanoplastics in natural water matrices.

Understanding the stability of NPs in different aqueous environments, related with their size is crucial for assessing their potential risks. This is influenced by several factors, including pH, ionic strength, and the presence of biomolecules, or dissolved organic matter (DOM). In this study, dispersions of NPs derived from common plastic waste materials, including polystyrene (PS), polyethylene terephthalate (PET), polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), and polycarbonate (PC), were synthesized by a nanoprecipitation method with sizes: 189 ± 7, 58 ± 3, 123 ± 4, 151 ± 7 and 182 ± 6 nm, respectively.

Volatile sulfur compounds in asthmatic children and adolescents: A cross-sectional study in breath and saliva.

Background: Halitosis in children implies psychosocial repercussions. Risk factors associated with this condition are unclear, and detection methods are inaccurate.

Aim: To quantify the levels of sulfur-like compounds in children with asthma and healthy children from a novel validated assay, and to establish the risk factors related to halitosis.

Isolation of Carbon Black from Soils by Dispersion for Analysis: Quantitation and Characterization by Field Flow Fractionation Techniques.

In the present work, a procedure based on a dispersive medium for carbon black (CB) isolation from soil samples for analysis was proposed for the first time. Polymeric and biological dispersants and a sequential use of both dispersants were assayed. Asymmetrical flow field flow fractionation with dynamic light scattering detector (AF4-DLS) and sedimentation field flow fractionation with multi-angle light scattering detector (SdF3-MALS) were used for CB quantitation and characterization in the achieved dispersions.

Determination of antioxidant activity by in situ synthesis of AgNPs using in-tube SPME coupled on-line to capillary liquid chromatography.

A chromatographic system based on in-tube SPME coupled to capillary LC-DAD has been used to study the synthesis of silver nanoparticles using polyphenols in different scenarios: excess of the reducing agent or of the silver salt, addition of the cationic surfactants, and thermal synthesis. The optimized synthesis conditions allowed to quantify the polyphenols used as reducing agents, such as Trolox and chlorogenic acid. Two chromatographic peaks with different absorption spectrum were monitored during the syntheses.

Reliable assessment of carbon black nanomaterial of a variety of cell culture media for in vitro toxicity assays by asymmetrical flow field-flow fractionation.

Carbon black nanomaterial (CB-NM), as an industrial product with a large number of applications, poses a high risk of exposure, and its impact on health needs to be assessed. The most common testing platform for engineered (E)NMs is in vitro toxicity assessment, which requires prior ENM dispersion, stabilization, and characterization in cell culture media. Here, asymmetric flow field-flow fractionation (AF4) coupled to UV-Vis and dynamic light scattering (DLS) detectors in series was used for the study of CB dispersions in cell culture media, optimizing instrumental variables and working conditions.

On-Site Multisample Determination of Chlorogenic Acid in Green Coffee by Chemiluminiscent Imaging.

The potential of antioxidants in preventing several diseases has attracted great attention in recent years. Indeed, these products are part of a multi-billion industry. However, there is a lack of scientific information about safety, quality, doses, and changes over time.

A Colorimetric Method for the Rapid Estimation of the Total Cannabinoid Content in Cannabis Samples.

A colorimetric method for the estimation of the total content of cannabinoids in cannabis samples is proposed. The assay is based on the reaction of these compounds with the reagent Fast Blue B (FBB), which has been immobilized into polydimethylsiloxane (PDMS). The reaction and detection conditions have been established according to the results obtained for the individual cannabinoids Δ-tetrahydrocannabidiol (THC), cannabidiol (CBD), and cannabinol (CBN), as well as for ethanolic extracts obtained from cannabis samples after ultrasonication.

Hand-Portable Miniaturized Liquid Chromatography for the Determination of Chlorogenic Acids in Dietary Supplements.

With the explosive growth of the dietary supplements industry, new demands have emerged that cannot be faced with the sophisticated instrumentation available in well-equipped laboratories. In particular, there is a demand for simplified and easy-to-use instruments, capable of providing results in short times of analysis. In this study, a hand-portable miniaturized liquid chromatograph (portable LC) has been tested for the determination of chlorogenic acids (CGAs) in products intended to supplement the diet and elaborated with green coffee extracts.

Advances in the Measurement of Polymeric Colorimetric Sensors Using Portable Instrumentation: Testing the Light Influence.

Sustainable and green sensors based on polydimethyl siloxane (PDMS) or cellulose polymers, as a case of study of the use of portable instrumentation joined to a smartphone, have been tested. A smartphone camera was used to obtain images and was also coupled to a minispectrometer, without and with an optical fiber probe to register spectra. To study light influence on the analytical signal, light-emitting diode (LED), halogen light and daylight have been assayed.

Improving Sustainability of the Griess Reaction by Reagent Stabilization on PDMS Membranes and ZnNPs as Reductor of Nitrates: Application to Different Water Samples.

A new approach based on the use of polydimethylsiloxane (PDMS) membranes doped with Griess reagents for in situ determination of NO2- and NO3- in real samples is proposed. The influence of some doping compounds, on the properties of the PDMS membranes, such as tetraethyl orthosilicate (TEOS), or/and ionic liquids (OMIM PF) has been studied. Membrane characterization was performed.

Combining high performance thin layer chromatography with minispectrometer-fiber optic probe-coupled to smartphone for in place analysis: Lactose quantification in several matrices.

An in place colorimetric method has been proposed for estimation of the quantity of lactose in several matrix (milk, water effluents and surfaces). Analyzing the amount of this carbohydrate it can be control the product, the cleanliness of the parts of the dairy companies and it can avoid contamination of milk products produced there. This method combines the use of HPTLC for sugars separation with novel analytical devices as minispectrophotometer with fiber optic coupled to a smartphone.

Characterization and Quantitation of Carbon Black Nanomaterials in Polymeric and Biological Aqueous Dispersants by Asymmetrical Flow Field Flow Fractionation.

Characterization of carbon black (CB) nanomaterials is required in industrial and research areas. Hence, in this study, asymmetrical flow field flow fractionation coupled to UV-vis and DLS detectors in series (AF4-UV-vis-DLS) was studied to evaluate the CB dispersion behavior in polymeric and biological dispersants, given the relevance of these media in practical applications. Under the experimental conditions, the results indicated that polymeric and biological dispersions showed size distributions with hydrodynamic diameters of 404 and 175 nm, respectively, for a particle core diameter of 40 nm.

A Colorimetric Membrane-Based Sensor with Improved Selectivity towards Amphetamine.

Due to their simplicity, speed and low cost, chemical spot tests are increasingly demanded for the presumptive identification of illicit drugs in a variety of contexts such as point-of-care assistance or prosecution of drug trafficking. However, most of the colorimetric reactions used in these tests are, at best, drug class selective. Therefore, the development of tests based on chemical reactions with improved discrimination power is of great interest.

Capillary Liquid Chromatography for the Determination of Terpenes in Botanical Dietary Supplements.

Dietary supplements of botanical origin are increasingly consumed due to their content of plant constituents with potential benefits on health and wellness. Among those constituents, terpenes are gaining attention because of their diverse biological activities (anti-inflammatory, antibacterial, geroprotective, and others). While most of the existing analytical methods have focused on establishing the terpenic fingerprint of some plants, typically by gas chromatography, methods capable of quantifying representative terpenes in herbal preparations and dietary supplements with combined high sensitivity and precision, simplicity, and high throughput are still necessary.

Corneal Biomechanical Parameters and Central Corneal Thickness in Glaucoma Patients, Glaucoma Suspects, and a Healthy Population.

Purpose: To evaluate and compare corneal hysteresis (CH), corneal resistance factor (CRF), and central corneal thickness (CCT), measurements were taken between a healthy population (controls), patients diagnosed with glaucoma (DG), and glaucoma suspect patients due to ocular hypertension (OHT), family history of glaucoma (FHG), or glaucoma-like optic discs (GLD). Additionally, Goldmann-correlated intraocular pressure (IOPg) and corneal-compensated IOP (IOPcc) were compared between the different groups of patients.

Methods: In this prospective analytical-observational study, a total of 1065 patients (one eye of each) were recruited to undergo Ocular Response Analyzer (ORA) testing, ultrasound pachymetry, and clinical examination.

NQS-Doped PDMS Solid Sensor: From Water Matrix to Urine Enzymatic Application.

The development of in situ analytical devices has gained outstanding scientific interest. A solid sensing membrane composed of 1,2-naphthoquinone-4-sulfonate (NQS) derivatizing reagent embedded into a polymeric polydimethylsiloxane (PDMS) composite was proposed for in situ ammonium (NH) and urea (NHCONH) analysis in water and urine samples, respectively. Satisfactory strategies were also applied for urease-catalyzed hydrolysis of urea, either in solution or glass-supported urease immobilization.

Monofunctional pyrenes at carbon nanotube electrodes for direct electron transfer HO reduction with HRP and HRP-bacterial nanocellulose.

The non-covalent modification of carbon nanotube electrodes with pyrene derivatives is a versatile approach to enhance the electrical wiring of enzymes for biosensors and biofuel cells. We report here a comparative study of five pyrene derivatives adsorbed at multi-walled carbon nanotube electrodes to shed light on their ability to promote direct electron transfer with horseradish peroxidase (HRP) for HO reduction. In all cases, pyrene-modified electrodes enhanced catalytic reduction compared to the unmodified electrodes.

Study of the Stability of Citrate Capped AgNPs in Several Environmental Water Matrices by Asymmetrical Flow Field Flow Fractionation.

Asymmetrical flow field-flow fractionation (AF4) coupled to UV-Vis and dynamic light scattering (DLS) detectors in series, was tested for stability studies of dispersions of citrate-capped silver nanoparticles (AgNPs) in several water matrices. The main goal is to provide knowledge to understand their possible behavior in the environment for short times since mixturing (up to 180 min). Ultrapure (UPW), bottled (BW1, BW2), tap (TW), transitional (TrW) and sea water (SW) matrices were assayed.

Scaling the Analytical Information Given by Several Types of Colorimetric and Spectroscopic Instruments Including Smartphones: Rules for Their Use and Establishing Figures of Merit of Solid Chemosensors.

The analytical information given by different types of instruments was scaled in order to establish suitably the figures of merit of a given methodology based on color measurements. Different lab and portable instruments, including smartphones with and without a miniaturized spectrophotometer accessory, have been tested. In order to obtain broad information and using objective criteria, these instruments have been compared from (1) the analytical point of view, considering mainly the detection limit (limits of detection [LODs]), selectivity, accuracy and intra- and interday precision, size, components, and costs; and (2) the environmental point of view, based on their footprint as kilograms of CO.

Aqueous Dilution of Noble NPs Bulk Dispersions: Modeling Instability due to Dissolution by AF4 and Stablishing Considerations for Plasmonic Assays.

Among different nanomaterials, gold and silver nanoparticles (AuNPs and AgNPs) have become useful tools for a wide variety of applications in general, and particularly for plasmonic assays. Particle size and stability analysis are key elements for their practical applications since the NPs properties depend on these parameters. Hence, in the present work, asymmetrical flow field flow fractionation (AF4) coupled to UV-Vis and dynamic light scattering (DLS) detectors in series, has been evaluated for stability studies of citrate-capped AuNPs and AgNPs aqueous dispersions.

Rapid evaluation of ammonium in different rain events minimizing needed volume by a cost-effective and sustainable PDMS supported solid sensor.

The presence of ammonium ion in rainwater is due to atmospheric processes which involve its scavenging from gas phase and particulate matter. The fractionated samplings of rainwater can provide information about these processes and their potential sources. However, only a low sample volume may be available, which constrained the analysis in general and more particularly in situ mode.

Innovations in Extractive Phases for In-Tube Solid-Phase Microextraction Coupled to Miniaturized Liquid Chromatography: A Critical Review.

Over the past years, a great effort has been devoted to the development of new sorbents that can be used to pack or to coat extractive capillaries for in-tube solid-phase microextraction (IT-SPME). Many of those efforts have been focused on the preparation of capillaries for miniaturized liquid chromatography (LC) due to the reduced availability of capillary columns with appropriate dimensions for this kind of system. Moreover, many of the extractive capillaries that have been used for IT-SPME so far are segments of open columns from the gas chromatography (GC) field, but the phase nature and dimensions are very limited.

Portable solid sensor supported in nylon for silver ion determination: testing its liberation as biocide.

This paper reports the fabrication and utility of a new solid sensor, which allows the quantitation of silver ions acting as catalyst at the low micromolar level. The optical sensor was prepared by incorporating both reagents, pyrogallol red (PGR) and 1,10-phenanthroline (Phen), in a nylon membrane. The effect of parameters in determining silver-catalyzed oxidation of PGR by persulfate in the presence of Phen as an activator was studied and optimized for achieving suitable sensitivity.

New Reusable Solid Biosensor with Covalent Immobilization of the Horseradish Peroxidase Enzyme: In Situ Liberation Studies of Hydrogen Peroxide by Portable Chemiluminescent Determination.

Herein, we reported a chemiluminescent biosensor based on the covalent immobilization of the horseradish peroxidase (HRP) enzyme on a polydimethylsiloxane (PDMS) support to quantify in situ hydrogen peroxide (HO). The chemiluminescent reaction based on the use of luminol as an oxidizable substrate, with HRP as the catalyst, has been used in order to quantify HO as the oxidizing agent. The performance of the proposed biosensor has been demonstrated to determine HO liberated by cells in a culture medium and for evaluating the delivery of HO from denture cleaner tablets, as examples of application.