Highly sensitive serum volatolomic biomarkers for pancreatic cancer diagnosis.

The discovery of new diagnostic tools for the early detection of diseases with poor prognosis such as pancreatic adenocarcinoma (PAC) is of high importance. The results from a control-case study (20 PAC patients, 19 healthy controls) for the search of new biomarkers of pancreatic cancer based in differences in the serum volatolome are presented in this work. Volatolomics were performed following a non-targeted HS-SPME-GC/MS approach, and a total of 433 volatile organic compounds (VOCs) was detected in the human serum samples.

AuAg Nanoparticles Grafted on TiO@N-Doped Porous Carbon: Improved Depletion of Ciprofloxacin under Visible Light through Plasmonic Photocatalysis.

TiO2 nanoparticles (NPs) were modified to obtain photocatalysts with different composition sophistication and displaying improved visible light activity. All of them were evaluated in the photodegradation of ciprofloxacin. The band gap of TiO2 NPs was successfully tailored by the formation of an N-doped porous carbon (NPC)-TiO2 nanohybrid through the pyrolysis of melamine at 600 °C, leading to a slight red-shift of the absorption band edge for nanohybrid NPC-TiO2 1.

An organometallic approach for the preparation of Au-TiO and Au-g-CN nanohybrids: improving the depletion of paracetamol under visible light.

The photocatalytic degradation of paracetamol (a common analgesic also known as acetaminophen) in ultrapure water with different photocatalytic systems was performed under ultraviolet or visible irradiation. The photocatalysts employed were: commercial Degussa-P25 TiO and Au-TiO under UVA irradiation (365 nm) and g-CN and Au-g-CN under visible light irradiation (low-power (4 × 10 W) white light LEDs), improving the effectiveness of degradation rates when the gold nanoparticles (Au NPs) were combined with the semiconductors. The nanostructured photocatalysts were synthesised and characterised by transmission electron microscope (TEM), UV-vis diffuse reflectance spectroscopy and, in the case of g-CN photocatalysts by X-ray photoelectron spectroscopy (XPS).

Combination of Au-Ag Plasmonic Nanoparticles of Varied Compositions with Carbon Nitride for Enhanced Photocatalytic Degradation of Ibuprofen under Visible Light.

Au-Ag/g-CN nanohybrids - were synthesized by the one-pot self-reduction of the organometallic precursor [AuAg(CF)(OEt)] in the presence of graphitic carbon nitride (g-CN), leading to two populations of alloyed Au-Ag nanoparticles (NPs) of different size and composition on the surface of g-CN, i.e., Ag-enriched Au-Ag NPs of smaller size and Au-enriched Au-Ag NPs of larger size.

Study of intermediate by-products and mechanism of the photocatalytic degradation of ciprofloxacin in water using graphitized carbon nitride nanosheets.

The photocatalytic degradation of the antibiotic ciprofloxacin in water was carried out with nanosheets of graphitic carbon nitride (g-CN) as catalyst and visible light irradiation using low-power (4 × 10 W) white light LEDs. The aim of this study was to identify the intermediate by-products formed during the degradation and to propose a pathway for CIP degradation. To achieve this goal, photocatalytically degraded CIP solutions were analysed by liquid chromatography coupled to high-resolution mass spectrometry using a QTOF instrument.

Photocatalytic degradation of ibuprofen in water using TiO/UV and g-CN/visible light: Study of intermediate degradation products by liquid chromatography coupled to high-resolution mass spectrometry.

The photocatalytic degradation of ibuprofen with TiO nanoparticles (NPs) and UV light and with graphitic carbon nitride (g-CN) 2D nanosheets and visible light are proposed and compared as advanced oxidation treatments for the removal of ibuprofen in water. By-products formed with both photocatalytic systems have been tentatively identified based on the results of ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry, using a quadrupole-time of flight mass spectrometer in positive and negative ionization modes, which allowed to obtain the elementary composition of their precursors and fragment ions. The removal of ibuprofen and the by-product formation were studied at three pH values.

Determination of cinnamaldehyde, carvacrol and thymol in feedstuff additives by pressurized liquid extraction followed by gas chromatography-mass spectrometry.

Specific blends of essential oils (BEOs) are promising substitutes for antibiotics to promote livestock performance and to reduce the incidence of intestinal disorders. Microencapsulation of BEOs has shown to improve their stability, bioavailability and to control their release rate once they are added to the feedstuff. The development and validation of a method for determining essential oil components such as carvacrol, thymol and cinnamaldehyde in a microencapsulated material used as feed additive is presented.

Synthesis, Photochemical, and Redox Properties of Gold(I) and Gold(III) Pincer Complexes Incorporating a 2,2':6',2"-Terpyridine Ligand Framework.

Reaction of [Au(C6F5)(tht)] (tht = tetrahydrothiophene) with 2,2':6',2"-terpyridine (terpy) leads to complex [Au(C6F5)(η(1)-terpy)] (1). The chemical oxidation of complex (1) with 2 equiv of [N(C6H4Br-4)3](PF6) or using electrosynthetic techniques affords the Au(III) complex [Au(C6F5)(η(3)-terpy)](PF6)2 (2). The X-ray diffraction study of complex 2 reveals that the terpyridine acts as tridentate chelate ligand, which leads to a slightly distorted square-planar geometry.

Determination of plastic additives in packaging by liquid chromatography coupled to high resolution mass spectrometry.

A simple and sensitive analytical method for the determination of several plastic additives in multilayer packaging based on solid-liquid extraction (SLE) and ultra-high performance liquid chromatography (UHPLC) coupled to variable wavelength (VWD) and time of flight mass spectrometry (TOF-MS) detectors is presented. The proposed method allows the simultaneous determination of fourteen additives belonging to different families such as antioxidants, slip agents and light stabilizers, as well as two oxidation products in only 9min. The developed method was validated in terms of linearity, matrix effect error, detection and quantification limits, repeatability and intermediate precision.

Analytical method for the determination and a survey of parabens and their derivatives in pharmaceuticals.

Exposure of humans to parabens is a concern due to the estrogenic activity of these compounds. Parabens are widely used as preservatives in some personal care products, foodstuffs and pharmaceuticals owing to their low cost, high water solubility and broad spectrum antimicrobial properties. Despite this, little is known on the occurrence of parabens in pharmaceutical products.

Use of microextraction by packed sorbents following selective pressurised liquid extraction for the determination of brominated diphenyl ethers in sewage sludge by gas chromatography-mass spectrometry.

In this work, a method based on selective pressurised liquid extraction followed by microextraction by packed sorbents (MEPS) for the determination of brominated diphenyl ethers (BDEs) in sewage sludge is presented. The factors affecting the MEPS procedure were optimised. Acetone:water (25:75) sPLE extracts were drawn-ejected 10 times through C18 cartridges at 5 μL s(-1).

Determination of perfluorinated alkyl acids in corn, popcorn and popcorn bags before and after cooking by focused ultrasound solid-liquid extraction, liquid chromatography and quadrupole-time of flight mass spectrometry.

An analytical method is proposed to determine ten perfluorinated alkyl acids (PFAAs) [nine perfluorocarboxylic acids (PFCAs) and perfluorooctane sulfonate (PFOS)] in corn, popcorn and microwave popcorn packaging by focused ultrasound solid-liquid extraction (FUSLE) and ultra high performance liquid chromatography (UHPLC) coupled to quadrupole-time of flight mass spectrometry (QTOF-MS/MS). Selected PFAAs were extracted efficiently in only one 10-s cycle by FUSLE, a simple, safe and inexpensive technique. The developed method was validated for microwave popcorn bags matrix as well as corn and popcorn matrices in terms of linearity, matrix effect error, detection and quantification limits, repeatability and recovery values.

Fast determination of perfluorocompounds in packaging by focused ultrasound solid-liquid extraction and liquid chromatography coupled to quadrupole-time of flight mass spectrometry.

A focused ultrasound solid-liquid extraction (FUSLE) and liquid chromatography (HPLC) coupled to quadrupole-time of flight mass spectrometry (QTOF-MS/MS) based method is proposed to determine six perfluorocarboxylic acids (PFCA) and perfluorooctane sulfonate (PFOS) in food-contact packaging. FUSLE, a simple, inexpensive and fast extraction technique, has been carried out with just 8mL of ethanol in one cycle of only 10s. The whole method presented good repeatability and intermediate precision, with RSDs below 11% and 15%, respectively; limits of detection, with values between 0.

Focused ultrasound solid-liquid extraction of perfluorinated compounds from sewage sludge.

A method for the determination of perfluorocarboxylic acids (PFCAs) and perfluorooctanesulfonic acid (PFOS) in sewage sludge based on focused ultrasound solid-liquid extraction (FUSLE) and reverse-phase ultra-performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry (QTOFMS) has been developed. FUSLE is a fast, low-cost and efficient extraction technique based on the application of high power focused ultrasonic waves using a micro-tip immersed directly in the extraction mixture. For the method development, the extraction solvent was studied and afterwards the factors affecting the extraction efficiency were optimised by means of a central composite design.

Determination of perfluorocompounds in popcorn packaging by pressurised liquid extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

The development and characterisation of a method based on reverse-phase ultra-performance liquid chromatography (UPLC) coupled to a quadrupole-time of flight mass spectrometer (Q-TOF-MS) with negative electrospray ionisation (ESI) to determine perfluorinated compounds (PFCs) in packaging is presented in this paper. Analytes were quantitatively recovered from packaging with methanol in only one PLE cycle of 6 min at 100 °C. The UPLC allowed the successful separation of the studied PFCs in less than 4 min.

Determination of bisphenol-type endocrine disrupting compounds in food-contact recycled-paper materials by focused ultrasonic solid-liquid extraction and ultra performance liquid chromatography-high resolution mass spectrometry.

Focused ultrasonic solid-liquid extraction (FUSLE) and reverse-phase ultra performance liquid chromatography (UPLC) coupled to a quadrupole-time of flight mass spectrometer (Q-TOF-MS) was applied to the determination of bisphenol-type endocrine disrupting compounds (EDCs) in food-contact recycled-paper materials. Recycled paper is a potential source of EDCs. Bisphenol A (BPA), bisphenol F (BPF) and their derivatives bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) are used for the production of epoxy resins employed in the formulation of printing inks.

Focused ultrasound solid-liquid extraction and gas chromatography tandem mass spectrometry determination of brominated flame retardants in indoor dust.

This study presents a focused ultrasound solid-liquid extraction (FUSLE) and gas chromatography tandem mass spectrometry method for the determination of brominated diphenyl ethers (BDEs), from mono- to hexa-congeners, in indoor dust. This approach provided a simple, fast, and economical method. After the solvent extraction selection, the FUSLE conditions were studied using a central composite design.

Determination of UV filters in packaging by focused ultrasonic solid-liquid extraction and liquid chromatography.

A focused ultrasonic solid-liquid extraction (FUSLE) and high performance liquid chromatography (HPLC) with a diode array detector (DAD) is proposed for the determination of ten fat-soluble UV filters in packaging. FUSLE technique is relatively new and has been used for the extraction of a few analytes; such as polycyclic aromatic hydrocarbons and other organic pollutants. In this work, it has been demonstrated that FUSLE is a useful, fast and simple extraction methodology for UV filters because the complete extraction was carried out with just 6ml of tetrahydrofuran and in only one cycle of 30s.

Determination of brominated diphenyl ethers (from mono- to hexa- congeners) in indoor dust by pressurised liquid extraction with in-cell clean-up and gas chromatography-mass spectrometry.

This study presents a selective pressurised liquid extraction (PLE) and gas chromatography-mass spectrometry/mass spectrometry method for the determination of brominated diphenyl ethers (BDEs) in indoor dust. Selective PLE consisted of the addition of Florisil mixed with the sample in order to perform an in-cell clean-up. This approach provided a cleaner and almost colourless extract, ready to be injected in the gas chromatograph.

Microwave-assisted oxidation of phosphite-type antioxidant additives in polyethylene film extracts.

Two oxidation methods for reducing the analysis time required to determine Irgafos 126 and Irgafos 168 by pressurised liquid extraction (PLE) and high-performance liquid chromatography (HPLC) were optimised and compared. Analyte oxidation was performed using sodium peroxodisulphate (SPD) as oxidation agent and two different heating methods: with a hotplate and a reflux apparatus; and with a microwave oven. The influence of variables, such as oxidation time, temperature and sodium peroxodisulphate concentration was studied using a central composite design in order to optimise experimental conditions.

Analysis of French and American oak chips with different toasting degrees by headspace solid-phase microextraction-gas chromatography-mass spectrometry.

This paper describes the optimisation of headspace solid-phase microextraction (HS-SPME) conditions for the analysis of volatile compounds in oak chips used to accelerate wine aging as an alternative to traditional aging in oak barrels. The direct extraction of ground wood samples and the extraction of sample aqueous slurries using a divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) fibre were studied and compared. Optimal conditions for direct extraction were 110 degrees C and 60 min, whereas for aqueous slurries they were obtained by adding 2mL of a 7.

Determination of ethylphenols in wine by in situ derivatisation and headspace solid-phase microextraction-gas chromatography-mass spectrometry.

Contamination by Brettanomyces is a frequent problem in many wineries that has a dramatic effect on wine aroma and hence its quality. The yeast Brettanomyces/Dekkera is involved in the formation of three important volatile ethylphenols-4-ethylphenol, 4-ethylguaiacol and 4-ethylcatechol-that transmit an unpleasant aroma to wine that has often been described as 'medicinal', 'stable' or 'leather'. This study proposes an in situ derivatisation and headspace solid-phase microextraction- gas chromatography coupled to mass spectrometry method to determine the three ethylphenols in red Brettanomyces-tainted wines.

Comparison of three gas chromatography methods for the determination of slip agents in polyethylene films.

Polymers require the use of some slip agents, such as oleamide and erucamide, in order to reduce their friction coefficient and to make films easier to handle. In this communication, three analytical methods consisting in pressurized liquid extraction (PLE) and gas chromatography (GC) are used to determine oleamide and erucamide in polyethylene films. The sample was extracted with pure isopropanol (two times) at 105 degrees C for 16 min.

Fibre selection based on an overall analytical feature comparison for the solid-phase microextraction of trihalomethanes from drinking water.

This paper describes the optimization of solid-phase microextraction (SPME) conditions for three different fibres (Carboxen-polydimethylsiloxane (CAR-PDMS), divinylbenzene-Carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB)) used to determine trihalomethanes (THMs) in water by headspace solid-phase microextraction and gas chromatography (HS-SPME-GC). The influence of temperature and salting-out effect was examined using a central composite design for each fibre. Extraction time was studied separately at the optimum values found for temperature and sodium chloride concentration (40 degrees C and 0.

Determination of volatile oak compounds in aged wines by multiple headspace solid-phase microextraction and gas chromatography-mass spectrometry (MHS-SPME-GC-MS).

Multiple headspace solid-phase microextraction (MHS-SPME) with gas chromatography-mass spectrometry is proposed for quantification of nine volatile oak compounds in aged wines. These compounds are formed and extracted by wine when it is matured in oak barrels and are responsible for particular organoleptic properties and the high quality of these wines. Some important variables of the extraction process, for example volume of sample and extraction time, were studied.