The potential of lignocellulosic biomass for magnetic solid phase extraction of naproxen from saliva samples.

This paper presents a study on the application of magnetic biochars derived from three distinct biomass sources: almond (AMBC), walnut (WMBC), and peanut (PMBC) shells for magnetic solid-phase extraction (MSPE) of naproxen, a non-steroidal anti-inflammatory drug, from human saliva prior to LC-MS analysis. The three magnetic biochars were synthesized and characterized through IR, XRD, SEM, and EDX analyses. This work explored the factors influencing extraction efficiency using these three bioadsorbents through experimental design.

An ICP-MS-Based Analytical Strategy for Assessing Compliance with the Ban of E 171 as a Food Additive on the EU Market.

A method was developed for the determination of total titanium in food and food supplements by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted acid digestion of samples. Five food supplements, including one certified reference material, and 15 food products were used for method development. Key factors affecting the analytical results, such as the composition of the acid mixture for sample digestion and the bias from spectral interferences on the different titanium isotopes, were investigated.

Advanced oxidation and a metrological strategy based on CLC-MS for the removal of pharmaceuticals from pore & surface water.

In this work, it is studied the photolysis, electrolysis, and photo-electrolysis of a mixture of pharmaceutics (sulfadiazine, naproxen, diclofenac, ketoprofen and ibuprofen) contained in two very different types of real water matrices (obtained from surface and porewater reservoirs), trying to clarify the role of the matrix on the degradation of the pollutants. To do this, a new metrological approach was also developed for screening of pharmaceuticals in waters by capillary liquid chromatography mass spectrometry (CLC-MS). This allows the detection at concentrations lower than 10 ng mL.

Rapid determination of malondialdehyde in serum samples using a porphyrin-functionalized magnetic graphene oxide electrochemical sensor.

An electrochemical sensor based on a screen-printed carbon electrode (SPCE) modified with porphyrin-functionalized magnetic graphene oxide (TCPP-MGO) was developed for the sensitive and selective determination of malondialdehyde (MDA), an important biomarker of oxidative damage, in serum samples. The coupling of TCPP with MGO allows the exploitation of the magnetic properties of the material for separation, preconcentration, and manipulation of analyte, which is selectively captured onto the TCPP-MGO surface. The electron-transfer capability in the SPCE was improved through derivatization of MDA with diaminonaphthalene (DAN) (MDA-DAN).

SERS-Based Methodology for the Quantification of Ultratrace Graphene Oxide in Water Samples.

The extensive use of graphene materials in real-world applications has increased their potential release into the environment. To evaluate their possible health and ecological risks, there is a need for analytical methods that can quantify these materials at very low concentrations in environmental media such as water. In this work, a simple, reproducible, and sensitive method to detect graphene oxide (GO) in water samples using the surface-enhanced Raman spectroscopy (SERS) technique is presented.

Detection of Porphyrins in Hair Using Capillary Liquid Chromatography-Mass Spectrometry.

Unlike humans, some animals have evolved a physiological ability to deposit porphyrins, which are pigments produced during heme synthesis in cells, in the skin and associated integument such as hair. Given the inert nature and easiness of collection of hair, animals that present porphyrin-based pigmentation constitute unique models for porphyrin analysis in biological samples. Here we present the development of a simple, rapid, and efficient analytical method for four natural porphyrins (uroporphyrin I, coproporphyrin I, coproporphyrin III and protoporphyrin IX) in the Southern flying squirrel Glaucomys volans, a mammal with hair that fluoresces and that we suspected has porphyrin-based pigmentation.

Rapid Sample Screening Method for Authenticity Controlling of Vanilla Flavours Using Liquid Chromatography with Electrochemical Detection Using Aluminium-Doped Zirconia Nanoparticles-Modified Electrode.

A rapid and sensitive technique for frauds determination in vanilla flavors was developed. The method comprises separation by liquid chromatography followed by an electrochemical detection using a homemade screen-printed carbon electrode modified with aluminium-doped zirconia nanoparticles (Al-ZrO-NPs/SPCE). The prepared nanomaterials (Al-ZrO-NPs) were characterized by using X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray (EDX).

Surface Polymers on Multiwalled Carbon Nanotubes for Selective Extraction and Electrochemical Determination of Rhodamine B in Food Samples.

In this study, we combine magnetic solid phase extraction (MSPE), with the screen-printed carbon electrode (SPCE) modified by a molecular imprinted polymer (MIP) for sensitive and selective extraction and electrochemical determination of Rhodamine B in food samples. A magnetic solid phase extraction (MSPE) was carried out using magnetic poly(styrene-co-divinylbenzene) (PS-DVB) and magnetic nanoparticles (MNPs) synthetized on the surface of multiwalled carbon nanotubes (MWCNTs). An MIP was prepared on the surface of MWCNTs in the presence of titanium oxide nanoparticles (TiONPs) modifying the SPCE for the rapid electrochemical detection of Rhodamine B.

Ionic liquid and magnetic multiwalled carbon nanotubes for extraction of N-methylcarbamate pesticides from water samples prior their determination by capillary electrophoresis.

A simple and rapid microextraction procedure is reported on the use of ionic liquid (IL) in combination with magnetic multiwalled carbon nanotubes (MMWCNTs). The procedure is based on temperature-controlled IL dispersive liquid phase microextraction (DLPME) and MMWCNTs, for selective preconcentration of N-methylcarbamate pesticides in water samples, followed by their hydrolysis in alkaline buffer, prior to being analyzed by capillary electrophoresis. The extraction procedure uses small volume of organic solvents, and there is no need for centrifugation.

Contributions of Capillary Electrophoresis in Analytical Nanometrology: A Critical View.

An overview on the increasing role of capillary electrophoresis in characterization and direct analysis of nanomaterials is herein presented. The niche of electrophoretic approaches in nanometrology is so relevant that nonmetallic, metal, metal oxide nanoparticles, and quantum dots have been analyzed to be targeted via capillary electrophoresis with conventional detection systems or coupling arrangements aimed at increasing selectivity and sensitivity toward either pristine or conjugated nanoparticles. Moreover, parameters altering intrinsic properties of nanoparticles may be optimized to gather the desired results and identify nanomaterials according to their size, shape, or associations with binding agents.

A new nanometrological strategy for titanium dioxide nanoparticles screening and confirmation in personal care products by CE-spICP-MS.

A new nanometrological approach was developed for screening of titania nanoparticles by capillary electrophoresis after adsorption of a target analyte namely l-cysteine onto the nanoparticles in a sodium phosphate buffer, followed by titanium elemental analysis by means of inductively-coupled plasma-mass spectrometry and size distribution measurements by single-particle mode. This analytical strategy involved a first screening of nanotitania in actual samples by electrophoresis, sensitivity being enhanced by cysteine which acts as a nanoparticles stabiliser. Detection and quantitation limits were 0.

LC-MS determination of catecholamines and related metabolites in red deer urine and hair extracted using magnetic multi-walled carbon nanotube poly(styrene-co-divinylbenzene) composite.

A novel analytical methodology for the extraction and determination of catecholamines (dopamine, epinephrine and norepinephrine) and their metabolites DL-3,4-dihydroxyphenyl glycol and DL-3,4-dihydroxymandelic acid by LC-MS is developed and validated for its application to human and animal urine and hair samples. The method is based on the preliminary extraction of the analytes by a magnetic multi-walled carbon nanotube poly(styrene-co-divinylbenzene) composite. This is followed by a <9 min chromatographic separation of the target compounds in an Onyx Monolithic C column using a mixture of 0.

Analytical control of Rhodamine B by SERS using reduced graphene decorated with copper selenide.

A novel approach for the decoration of reduced graphene oxide with copper selenide (CuSe-rGO), using supercritical carbon dioxide (sc-CO) as a medium, was developed and proposed as a new substrate for surface-enhanced Raman spectroscopy (SERS) to determine Rhodamine B in chili powder. The synthesized materials graphene oxide (GO), reduced graphene oxide (rGO) and CuSe-rGO were characterized by Raman spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). All SERS spectra were obtained by using a portable Raman spectrometer.

Graphene quantum dots for enhancement of fluorimetric detection coupled to capillary electrophoresis for detection of ofloxacin.

A new CE method with fluorescence detection is reported on the determination of ofloxacin in milk samples using graphene quantum dots (GQDs) for sensitivity enhancement. Injection of GQDs prior the standards/sample is crucial to increase the antibiotic fluorescence response. Clean-up and preconcentration steps allowed for a good linear correlation in a concentration range between 50 and 1000 ng/mL for the ofloxacin, detection and quantification limits being 10.

Unique evolution of vitamin A as an external pigment in tropical starlings.

Pigments are largely responsible for the appearance of organisms. Most biological pigments derive from the metabolism of shikimic acid (melanins), mevalonic acid (carotenoids) or levulinic acid (porphyrins), which thus generate the observed diversity of external phenotypes. Starlings are generally dark birds despite iridescence in feathers, but 10% of species have evolved plumage pigmentation comprising bright colors that are known to be produced only by carotenoids.

Analytical nanometrological approach for screening and confirmation of titanium dioxide nano/micro-particles in sugary samples based on Raman spectroscopy - Capillary electrophoresis.

Analytical nanometrology is a present challenge in today's analytical science, particularly from a practical point of view and when it is addressed to routine/control laboratories. In this way, a screening-confirmation approach is described for the characterization and distinction between titanium dioxide nano/micro-particles in sugary food samples. The first step involves the confirmation of the presence of TiO in the sample (used as additive E171 in sugary samples), using a portable Raman spectrometer, in which the crystalline structure of TiO (anatase or rutile) in the positive samples can be also obtained in this step.

Nanostructured hybrid surface enhancement Raman scattering substrate for the rapid determination of sulfapyridine in milk samples.

The fabrication of surface-enhanced Raman spectroscopy (SERS) substrates, which can offer the advantages of strong Raman signal enhancement with good reproducibility, is still a challenge for practical applications. In this work, a simple and reproducible SERS substrate combining the properties of multi-walled carbon nanotubes (MWCNTs) and gold nanoparticles (AuNPs), is proposed for the determination and quantification of sulfapyridine in milk samples with a concentration range of 10-100 ng mL. The Raman signals of sulfapyridine is enhanced at factor of 4394.

Magnetic multi-walled carbon nanotube poly(styrene-co-divinylbenzene) for propranolol extraction and separation by capillary electrophoresis.

Aim: The preparation of magnetic multi-walled carbon nanotube poly(styrene-co-divinylbenzene) for propranolol magnetic solid-phase extraction is described.

Materials & Methods: A study comparing propranolol adsorption and desorption was performed with only magnetic multi-walled carbon nanotubes, and different poly(styrene-co-divinylbenzene) with and without magnetic multi-walled carbon nanotubes. Enantiomeric separation of propranolol took place by cyclodextrin-modified capillary electrophoresis and the method was validated in spiked human urine samples.

Innovative coupling of supercritical fluid extraction with ion mobility spectrometry.

This paper describes a pioneer on-line hyphenation between a supercritical fluid extraction (SFE) and an ion mobility spectrometry (IMS) detector through a Tenax TA sorbent trap as retention interface. By means of a simple design, taking advantage of both techniques, this new coupling allows us to extract and preconcentrate analytes and in a second step to determine them. As result, an increase in the accuracy of the analytical process was achieved by elimination of sample transfer from one device to another.

Magnetic nanocellulose hybrid nanoparticles and ionic liquid for extraction of neonicotinoid insecticides from milk samples prior to determination by liquid chromatography-mass spectrometry.

A simple and rapid microextraction procedure is reported on the use of ionic liquid in combination with magnetic nanocellulose hybrid nanoparticles. The procedure is ultrasound-assisted and applicable to selective preconcentration of neonicotinoid insecticides from milk samples, prior to being analysed by liquid chromatography-mass spectrometry. The extraction procedure uses small volume of organic solvents (<1 mL), and there is no need for centrifugation.

Determination of antidepressants in human urine extracted by magnetic multiwalled carbon nanotube poly(styrene-co-divinylbenzene) composites and separation by capillary electrophoresis.

Poly(styrene-co-divinylbenzene)-coated magnetic multiwalled carbon nanotube composite synthesized by in-situ high temperature combination and precipitation polymerization of styrene-co-divinylbenzene has been employed as a magnetic sorbent for the solid phase extraction of antidepressants in human urine samples. Fluoxetine, venlafaxine, citalopram and sertraline were, afterwards, separated and determined by capillary electrophoresis with diode array detection. The presence of magnetic multiwalled carbon nanotubes in native poly(styrene-co-divinylbenzene) not only simplified sample treatment but also enhanced the adsorption efficiencies, obtaining extraction recoveries higher than 89.

Use of capillary electrophoresis for characterisation of vinyl-terminated Au nanoprisms and nanooctahedra.

It is described a simple, rapid and efficient methodology to characterise and separate gold nanoprisms and nanooctahedra by capillary electrophoresis. This technique is suitable to distinguish between morphologies and it can be used as a powerful separation tool after a customised synthesis of both structures. This synthesis was carried out by amending two parameters, temperature and pH, and a sharp decrease was found in nanotriangles when temperature was increased from 70 up to 95°C.

Capillary electrophoresis method for the discrimination between natural and artificial vanilla flavor for controlling food frauds.

A capillary electrophoresis method was developed for the determination of coumarin (COUM), ethyl vanillin (EVA), p-hydroxybenzaldehyde (PHB), p-hydroxybenzoic acid (PHBA), vanillin (VAN), vanillic acid (VANA) and vanillic alcohol (VOH) in vanilla products. The measured concentrations are compared to values obtained by liquid chromatography (LC) method. Analytical results, method precision, and accuracy data are presented and limits of detection for the method ranged from 2 to 5 μg/mL.