A modified micro-solid phase extraction device for in-port elution and injection into portable liquid chromatography: A proof-of-concept study.

A micro-solid phase extraction (micro-SPE) device packed with a C18 sorbent (10 mg) has been developed for the enrichment and purification of organic water pollutants prior to their analysis using a portable liquid chromatograph with a dual UV detector. To this end, the sorbent was immobilized at the inlet of a 4 mm syringe filter (0.20 µm), which was modified to reduce its internal volume.

Study of the degradation of diphenyl-ether herbicides aclonifen and bifenox in different environmental waters.

The degradation of the diphenyl-ether herbicides aclonifen (ACL) and bifenox (BF) in water samples has been studied under different laboratory conditions, using in-tube solid-phase microextraction (IT-SPME) coupled to capillary liquid chromatography (capLC). The working conditions were selected in order to detect also bifenox acid (BFA), a compound formed as a result of the hydroxylation of BF. Samples (4 mL) were processed without any previous treatment, which allowed the detection of the herbicides at low ppt levels.

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.

Determination of caffeine in dietary supplements by miniaturized portable liquid chromatography.

In this study three miniaturized liquid chromatography (LC) instruments have been evaluated and compared for the analysis of caffeine in dietary supplements, namely a benchtop capillary LC (capLC) system, a benchtop nano LC (nanoLC)system and a portable LC system. Commercial products derived from different sources of caffeine have been analyzed. Under optimized conditions, the methods based on benchtop systems were superior in terms of sensitivity.

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.

Scopolamine analysis in beverages: Bicolorimetric device vs portable nano liquid chromatography.

Scopolamine (SCP) is often involved in sexual assaults and robberies, particularly in recreational environments. Therefore, analytical tools are required for the analysis of this compound amenable for the field. In this work, a sensor for SCP is described based on the entrapment of KMnO into polydimethylsiloxane (PDMS).

Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case.

Analytical performance and optimization of figures of merit of a portable nano liquid chromatograph (NanoLC) with UV detection at 255 nm have been established for in place analysis. Methylxanthines: caffeine, theophylline and theobromine were selected as target analytes. A fast lab method based on IT-SPME coupled on line with capillary liquid chromatograph (CapLC) with diode array detection (DAD) was employed for comparative studies.

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.

Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography for the monitoring of tribenuron methyl in environmental waters.

The degradation kinetics and residual levels of the sulfonylurea herbicide tribenuron-methyl (TBM) in different environmental waters were studied using in tube-solid phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nanoLC) and UV diode array detection (DAD). This approach combines the high extraction efficiency of IT-SPME using polymeric coatings reinforced with metal oxide nanoparticles and the high sensitivity attainable by nanoLC, making possible the determination of TBM at low ppb levels (limit of detection, 0.25 ppb) without altering the sample matrix.

Bimodal copper oxide nanoparticles doped phase for the extraction of highly polar compounds by in-tube solid-phase microextraction coupled on-line to nano-liquid chromatography.

Polymers obtained from tetraethyl orthosilicate (TEOS) and triethoxymethylsilane (MTEOS) have been functionalized with different metal and metal oxide nanoparticles (NPs), and used as coatings of extractive capillaries for the extraction of polar compounds by in-tube solid-phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nano-LC). The extraction capabilities of the new phases have been studied using several triazinic herbicides with log of octanol/water partition coefficients (K) ranging from -0.7 to 3.

Quantitative Analysis of Terpenic Compounds in Microsamples of Resins by Capillary Liquid Chromatography.

A method has been developed for the separation and quantification of terpenic compounds typically used as markers in the chemical characterization of resins based on capillary liquid chromatography coupled to UV detection. The sample treatment, separation and detection conditions have been optimized in order to analyze compounds of different polarities and volatilities in a single chromatographic run. The monoterpene limonene and the triterpenes lupeol, lupenone, β-amyrin, and α-amyrin have been selected as model compounds.

Establishing the occurrence and profile of polycyclic aromatic hydrocarbons in marine sediments: The eastern Mediterranean coast of Spain as a case study.

Sampling, cost-effective analysis, diagnosis of sources of pollution and assessment of potential toxicological effects were included in the case study. Marine sediments collected from 24 points along the eastern Mediterranean coast of Spain (Comunitat Valenciana region) in 2010, 2011, 2012 and 2015 have been analysed for polycyclic aromatic hydrocarbons. Fluoranthene, pyrene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene were the most found.

Stabilization of formaldehyde into polydimethylsiloxane composite: application to the in situ determination of illicit drugs.

The Marquis test is the most frequently used spot color assay for the screening of unknown drugs such as amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-metilenedioxymethamphetamine, and morphine. However, this test involves the use of the toxic reagent formaldehyde, as well as the manipulation of concentrated sulfuric acid. Here, we report a new format of this test that improves the sustainability and safety for the operator by immobilizing formaldehyde into a polydimetylsiloxane composite.

Modifying the reactivity of copper (II) by its encapsulation into polydimethylsiloxane: A selective sensor for ephedrine-like compounds.

This paper demonstrates that the reactivity of copper (II) can be modified through its entrappment in a polymeric matrix of polydimethylsiloxane (PDMS), which makes possible the reaction into the support instead of in solution. Amino-containing compounds such as amino acids, proteins and sugars, which react with Cu (II) in solution, do not react inside the polymer. As a prove of concept, a highly specific Cu (II) PDMS-based sensor for ephedrines has been developed in this work.

Analysis of Contact Traces of Cannabis by In-Tube Solid-Phase Microextraction Coupled to Nanoliquid Chromatography.

Because of its inherent qualities, in-tube solid-phase microextraction (IT-SPME) coupled on-line to nanoliquid chromatography (nanoLC) can be a very powerful tool to address the new challenges of analytical laboratories such as the analysis of traces of complex samples. This is the case of the detection of contact traces of drugs, especially cannabis. The main difficulties encountered in the analysis of traces of cannabis plants on surfaces are the low amount of sample available (typically < 1 mg), the complexity of the matrix, and the low percentages of cannabinoic compounds in the samples.

A new tool for direct non-invasive evaluation of chlorophyll a content from diffuse reflectance measurements.

Chlorophyll is a key biochemical component that is responsible for photosynthesis and is an indicator of plant health. The effect of stressors can be determined by measuring the amount of chlorophyll a, which is the most abundant chlorophyll, in vegetation in general. Nowadays, invasive methods and vegetation indices are used for establishing chlorophyll amount or an approximation to this value, respectively.

A solid colorimetric sensor for the analysis of amphetamine-like street samples.

A solid sensor obtained by embedding 1,2-naphthoquinone-4-sulfonate (NQS) into polydimethylsiloxane/tetraethylortosilicate/silicon dioxide nanoparticles composite has been developed to identify and determine amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxymetamphetamine (MDMA) and 3,4-methylenedioxyamphetamine (MDA). The analytes are derivatized inside the composite for 10 min to create a colored product which can be then quantified by measuring the diffuse reflectance or the color intensity after processing the digitalized image. Satisfactory limits of detection (0.

Determination of amphetamines in hair by integrating sample disruption, clean-up and solid phase derivatization.

The utility of matrix solid phase dispersion (MSPD) for the direct analysis of amphetamines in hair samples has been evaluated, using liquid chromatography (LC) with fluorescence detection and precolumn derivatization. The proposed approach is based on the employment of MSPD for matrix disruption and clean-up, followed by the derivatization of the analytes onto the dispersant-sample blend. The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization.

Microextraction with phases containing nanoparticles.

In this article, the state of the art of microextraction techniques that involve nanoparticles or nanomaterials (NPs) is reviewed, with special emphasis on the applications described in the biomedical field. The uses and advantages of the different types of NPs such as carbon nanotubes (either single- and multi-walled) and other carbon-based materials, metallic NPs, including gold, silver and magnetic NPs, and silica NPs are summarized. The main strategies used to modify the selectivity, extractive capacity and/or the stability of NPs through a chemical reaction are also reviewed.

Selective and sentivive method based on capillary liquid chromatography with in-tube solid phase microextraction for determination of monochloramine in water.

Due to the difficulties of working with chloramines, a critical examination of monochloramine standard preparation has been performed in order to select the best synthesis conditions. The analyte has been determined by in-tube solid phase extraction coupled to capillary liquid chromatography with UV detection (IT-SPME Capillary LC DAD). Potential factors affecting the response of monochloramine such as the pH of mobile phase and the volume of sample processed by IT-SPME Capillary LC DAD have been investigated and optimized.

Analysis of polar triazines and degradation products in waters by in-tube solid-phase microextraction and capillary chromatography: an environmentally friendly method.

This paper describes a new method for the determination of polar triazines, including some degradation products, which combines online in-tube solid-phase microextraction (IT-SPME) and capillary liquid chromatography with UV-diode array detection (DAD). Different extractive coatings have been evaluated for IT-SPME, a capillary column with a polydimethylsiloxane (PDMS) coating, and the same coating modified with carboxylated single-wall carbon nanotubes (c-SWCNTs) and carboxylated multiwall carbon nanotubes (c-MWCNTs). On the basis of the results obtained, a new method is presented for the identification and determination of triazines in water samples.

Development of a polydimethylsiloxane-thymol/nitroprusside composite based sensor involving thymol derivatization for ammonium monitoring in water samples.

This report describes a polydimethylsiloxane (PDMS)-thymol/nitroprusside delivery composite sensor for direct monitoring of ammonium in environmental water samples. The sensor is based on a PDMS support that contains the Berthelot's reaction reagents. To prepare the PDMS-thymol/nitroprusside composite discs, thymol and nitroprusside have been encapsulated in the PDMS matrix, forming a reagent release support which significantly simplifies the analytical measurements, since it avoids the need to prepare derivatizing reagents and sample handling is reduced to the sampling step.

On-line in-tube solid phase microextraction-capillary liquid chromatography method for monitoring degradation products of di-(2-ethylhexyl) phthalate in waters.

The main di-(2-ethylhexyl) phthalate (DEHP) degradation products, (2-ethylhexyl) phthalate (MEHP), diethyl phthalate (DEP) and dibutyl phthalate (DBP), have been tested. The proposed cost-effective method combines on-line, in-tube solid-phase micro extraction (IT-SPME) in in-valve configuration and capillary liquid chromatography with UV diode array detection (Cap-LC-DAD). Acidification of the samples at pH 3 improved markedly the estimation of MEHP.