Relationship between foliar polycyclic aromatic hydrocarbons (PAHs) concentrations and plant traits: Intracanopy variability for a broadleaf species in an urban environment.

The emission of potentially harmful compounds, including polycyclic aromatic hydrocarbons (PAHs), and the resulting air pollution is a serious problem in modern cities. It is therefore important to develop mitigation strategies, such as "smart" planting of trees that act as sinks for PAHs. However, the intra-individual (within-tree) variability in leaf PAH concentrations remains unknown. In this paper, we studied 15 ornamental apple trees (Malus × moerlandsii 'Profusion') growing on a main street in a medium-sized city in Galicia (NW Spain). We determined the PAH concentrations at 12 canopy positions in each tree (2 orientations and 2 distances from the trunk at 3 heights), measured various ecological traits (specific leaf area [SLA], δ13C, stomatal density, fatty acid contents and leaf hairiness) and analyzed the variability in traits within the canopy in relation to PAH concentrations. We observed high intra-individual variability in the PAH concentrations and the leaf traits. Statistical analyses revealed that leaf height was the main source of variability both in the PAH concentrations and in the traits, mainly due to the leaf morphology, particularly to the SLA. Therefore, the ideal vegetation to remove PAHs would be high leaf biomass trees, not too tall and with a high proportion of shade leaves.

The generally recognized as safe (GRAS) microalgae Haematococcus pluvialis (wet) as a multifunctional additive for coloring and improving the organoleptic and functional properties of foods.

This work proposes the application of astaxanthin-rich H. pluvialis wet paste (HPW) as a partial substitute for wheat flour in the preparation of filloas, a dish that combines the basic ingredients of industrial bakery. The nutritional and color profile of HPW-enriched samples was evaluated by comparative analysis with a mixture of synthetic food dyes. The highest content of carotenoids (798 ± 12 µg g-1) and fatty acids (76 ± 2 mg g-1) was obtained for a filloa fortified with H. pluvialis in contrast to a non-significant dye response. Subsequently, the color stability of the fortified filloa was evaluated over time (3, 6 and 9 days), as well as its physicochemical properties and microbiological profile. As a result, HPW provided filloas with a longer shelf life, brightness (*L), and texture, in comparison with a mixture of synthetic dyes. In addition, an inhibitory effect of HPW towards mesophilic aerobic microorganisms in the food was obtained.

First approach to assess the effects of nanoplastics on the soil species Folsomia candida: A mixture design with bisphenol A and diphenhydramine.

The terrestrial environment is one of the main recipients of plastic waste. However, limited research has been performed on soil contamination by plastics and even less assessing the effects of nanoplastics (NPls). Behind the potential toxicity caused per se, NPls are recognized vectors of other environmental harmful contaminants. Therefore, the main aim of the present study is to understand whether the toxicity of an industrial chemical (bisphenol A - BPA) and a pharmaceutical (diphenhydramine - DPH) changes in the presence of polystyrene NPls to the terrestrial invertebrate Folsomia candida. Assessed endpoints encompassed organismal (reproduction, survival and behavior) and biochemical (neurotransmission and oxidative stress) levels. BPA or DPH, 28 d single exposures (1 to 2000 mg/kg), induce no effect on organisms' survival. In terms of reproduction, the calculated EC50 (concentration that causes 50% of the effect) and determined LOEC (lowest observed effect concentration) were higher than the environmental concentrations, showing that BPA or DPH single exposure may pose no threat to the terrestrial invertebrates. Survival and reproduction effects of BPA or DPH were independent on the presence of NPls. However, for avoidance behavior (48 h exposure), the effects of the tested mixtures (BPA + NPls and DPH + NPls) were dependent on the NPls concentration (at 0.015 mg/kg - interaction: no avoidance; at 600 mg/kg - no interaction: avoidance). Glutathione S-transferase activity increased after 28 d exposure to 100 mg/kg DPH + 0.015 mg/kg NPls (synergism). The increase of lipid peroxidation levels found after the exposure to 0.015 mg/kg NPls (a predicted environmental concentration) was not detected in the mixtures (antagonism). The results showed that the effects of the binary mixtures were dependent on the assessed endpoint and the tested concentrations. The findings of the present study show the ability of NPls to alter the effects of compounds with different natures and mechanisms of toxicity towards soil organisms, showing the importance of environmental risk assessment considering mixtures of contaminants.

The chemistry behind the body art: unveiling the elemental profile and heavy metal content of natural tattoos and dyes by ICP-MS.

Temporary tattoos and dyes are increasing popularity as an alternative to permanent ones. However, knowledge on its elementary composition is scarce and, this scientific gap can potentially make them a source of heavy metal exposure on humans. The present research aimed to explore the possibility of using the inorganic chemical signature to characterize natural pigments-based products and to evaluate the heavy metal content in jagua temporary tattoos and henna temporary hair dyes and tattoos. Thirty-four different samples of commercial products were analyzed for the presence and quantity of eleven trace elements (Al, Cr, Mn, Co, Ni, Cu, Zn, As, Cd, Ba, and Pb) by inductively coupled plasma mass spectrometry (ICP-MS). The overall mean concentrations varied between 0.02 and 973 µg g-1 in solid samples or 0.01-1878 µg g-1 for paste ones, wherein potential fake products were uncovered. None of the 34 samples considered comply with the current European Cosmetics Regulation. Samples were differentiated according to their Cr, Zn, Ba, and Pb content. The overall results revealed highly variable levels in the investigated samples, which leads us to suggest detailed quality controls of these materials, due the fact that their continued use can origin potential threat to human health.

Optimization of bioactives extraction from grape marc via a medium scale ambient temperature system and stability study.

A scalable procedure with minimum energy requirements, MSAT (Medium Scale Ambient Temperature), in combination with solvents generally recognized as safe (GRAS), has been optimized to obtain polyphenolic extracts from white grape (Vitis vinifera) marc. The solvents considered were propylene glycol (Pg), ethanol (Et), and ethyl lactate (Lc), as well as their respective hydro-organic mixtures. In a first approach, the operating parameters were optimized through a response surface matrix: extraction solvent volume (range 10-150 mL), marc mass (range 20-200 g) and marc/dispersant mass ratio (range 0.5-2 g⋅g-1), using the total polyphenol content (TPC) and the antioxidant activity (AA) of the extracts as response parameters. The highest TPC (5,918 mgGAE⋅L-1) and AA (44 mmolTE⋅L-1) values were obtained using 200 g marc and 100 mL solvent. Regarding the type of solvent, a better response was reached with Lc > Et > Pg > H2O obtaining a polyphenol concentration of 252 mg⋅L-1 for the hydro-organic isovolumetric ratio of ethyl lactate. In addition, the stability of the extracts was studied for 62 days. The effect of factors such as temperature, light exposure, and oxidative reactivity was evaluated. The bioactivity indices showed no changes with the storage conditions of the extracts in the first month of analysis, after which 75% of the antioxidant activity as the concentration of the polyphenolic profile (204 mg⋅L-1) remains. The absence of reactive oxygen and the cooling of the extract (4°C) were the most determining factors (p < 0.05) in modulating the stability of the total polyphenolic profile.

Understanding the chemical and mineralogical composition of commercial henna and jagua tattoos and dyes-a multi-analytical approach.

Temporary tattoos and dyes constitute a great analytical challenge in relation to the regulatory control of their ingredients. Most of these commercial products are not labeled according to their content and their chemical nature is highly diverse. Therefore, it is necessary to analyze these complex samples to evaluate the potential presence of metallic impurities, to ensure the safety of cosmetic products contributing to health protection. This study proposes a multi-analytical methodology, which includes handheld X-ray fluorescence (h-XRF) and X-ray diffraction (XRD), complemented by variable pressure scanning electron microscopy coupled with energy-dispersive X-ray spectrometry (VP-SEM-EDS) to fully characterize 34 commercial samples of jagua and henna tattoos and dyes. The approach allowed the identification of the main constituents providing complementary compositional data and differences between sample types were established. In addition, information on the degree of natural pigments homogeneity was also obtained. The results' discussion considering the current European cosmetics regulation may be useful to support the drafting of safety requirements and specific regulation.

Gone with the flow - Assessment of personal care products in Portuguese rivers.

Although there are several works in the literature that study the presence of pharmaceuticals and personal care products (PPCPs) in surface waters, the vast majority focus their attention on pharmaceuticals and little information is found about personal care products (PCPs). Therefore, this study focused, for the first time, on the monitoring of five classes of PCPs - fragrance allergens, synthetic musks, phthalates, antioxidants, and ultraviolet-filters - in the surface water of four small-size typically pollution-impacted Portuguese rivers (Ave, Leça, Antuã and Cértima). A solid-phase microextraction (SPME) followed by gas chromatography - tandem mass spectrometry (GC-MS/MS) protocol was employed to analyse surface water samples collected in two seasonal campaigns - summer and winter (34 samples per season). A total of 22 out of 37 target PCPs were detected concomitantly at least once in one sampling point, being the most frequently detected α-isomethyl ionone, galaxolide, tonalide and cashmeran. The highest concentrations were confirmed for diethylhexyl phthalate (610.6 ng L-1), galaxolide (379.2 ng L-1), geraniol (290.9 ng L-1), linalool (271.2 ng L-1), benzophenone-3 (254.1 ng L-1) and citronellol (200.2 ng L-1). Leça River, traversing the more densely urban and industrialized area, had the highest levels of contaminants, which were also found in the sampling points located downstream of wastewater treatment plants discharge points. In general, higher levels were detected in summer, when the river flows are lower. Hazard quotients were determined and octocrylene, tonalide, and geraniol presented values above 1 in some sampling sites, which may indicate an ecotoxicological risk to the aquatic environment. The results presented suggest that these three PCPs should be included as priority pollutants in environmental monitoring schemes in surface waters, due to their high detection, persistence, and potential adverse effects.

Recent Advances in Sample Preparation for Cosmetics and Personal Care Products Analysis.

The use of cosmetics and personal care products is increasing worldwide. Their high matrix complexity, together with the wide range of products currently marketed under different forms imply a challenge for their analysis, most of them requiring a sample pre-treatment step before analysis. Classical sample preparation methodologies involve large amounts of organic solvents as well as multiple steps resulting in large time consumption. Therefore, in recent years, the trends have been moved towards the development of simple, sustainable, and environmentally friendly methodologies in two ways: (i) the miniaturization of conventional procedures allowing a reduction in the consumption of solvents and reagents; and (ii) the development and application of sorbent- and liquid-based microextraction technologies to obtain a high analyte enrichment, avoiding or significantly reducing the use of organic solvents. This review provides an overview of analytical methodology during the last ten years, placing special emphasis on sample preparation to analyse cosmetics and personal care products. The use of liquid-liquid and solid-liquid extraction (LLE, SLE), ultrasound-assisted extraction (UAE), solid-phase extraction (SPE), pressurized liquid extraction (PLE), matrix solid-phase extraction (MSPD), and liquid- and sorbent-based microextraction techniques will be reviewed. The most recent advances and future trends including the development of new materials and green solvents will be also addressed.

Multi-Target Strategy to Uncover Unexpected Compounds in Rinse-Off and Leave-On Cosmetics.

The wide range and complexity of cosmetic formulations currently available on the market poses a challenge from an analytical point of view. In addition, during cosmetics manufacture, impurities coming from raw materials or formed by reaction of different organic compounds present in the formulation may be present. Their identification is mandatory to assure product quality and consumer health. In this work, micro-matrix solid-phase dispersion (µMSPD) is proposed as a multi-target sample preparation strategy to analyze a wide number of unexpected families of compounds including polycyclic aromatic hydrocarbons (PAHs), pesticides, plasticizers, nitrosamines, alkylphenols (APs), and alkylphenol ethoxylates (APEOs). Analytical determination was performed by gas chromatography-mass spectrometry (GC-MS) for the determination of 51 target compounds in a single run, whereas liquid chromatography tandem mass spectrometry (LC-MS/MS) was employed for the analysis of six APs and APEOs. Both methodologies were successfully validated in terms of linearity, accuracy, and precision in leave-on and rinse-off cosmetics. Limits of detection (LODs) were calculated in the low ng g-1, showing their suitability to determine trace levels of impurities and banned compounds with different chemical natures, providing useful tools to cosmetic control laboratories and companies.

Matrix solid-phase dispersion as a greener alternative to obtain bioactive extracts from Haematococcus pluvialis. Characterization by UHPLC-QToF.

So far, research on the microalga Haematococcus pluvialis has been focused mainly on the exploitation of its high astaxanthin content, leaving aside the use of other bioactive compounds present. This study is focused on obtaining and characterizing extracts enriched in bioactive compounds from this microalga red aplanospores. This is performed by means of Matrix Solid-Phase Dispersion (MSPD) extraction process, in an environmentally friendly way with low energy consumption and GRAS solvents. The effects of extraction parameters, particularly the extraction solvents (ethanol, ethyl lactate and water) are studied, in order to obtain maximum recovery of the main antioxidant compounds of interest (carotenoids, fatty acids and derivatives). Characterization of extracts is carried out by HPLC-DAD (High Performance Liquid Chromatography Diode Array Detector) and UHPLC-QToF (Ultra High-Performance Liquid Chromatography Quadrupole Time-of-Flight). The results show that MSPD produced extracts with higher bioactive compound recoveries than conventional cell disruption extractions. At the same time, a novel untargeted characterization for this species is performed, identifying compounds not previously dated in H. pluvialis, which include 10-phenyldecanoic acid and the -oxo and -hydroxy derivatives of palmitic acid. This approach, first applied to a freshwater microalgae, characterized by rigid and resistant aplanospores, provided a synergistic and sustainable extract, giving a broader focus on the use of this microalga.

Determination of multiclass personal care products in continental waters by solid-phase microextraction followed by gas chromatography-tandem mass spectrometry.

A methodology based on solid-phase microextraction (SPME) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous analysis of different families of personal care products (PCPs) including fragrance allergens, synthetic musks, phthalates, antioxidants and UV filters in continental waters. The main parameters affecting SPME procedure were optimized by an ANOVA study. The final selected conditions comprised the use of 10 mL of sample with 20% (w/v) of sodium chloride (NaCl), polydimtehylsiloxane/divinylbenzene (PDMS/DVB) fiber and 20 min of extraction time at 100 °C in the head-space mode. Good linearity (R2>0.9925), quantitative recoveries (>79%), and precision (RSD < 15%) were achieved for all compounds under the optimal conditions. Limits of quantification (LOQs) at the sub and low ng L-1 were obtained. The validated methodology was successfully applied to the analysis of river water samples from the North Portuguese coast allowing the determination of five different families of PCPs, including a total of 43 compounds in a single chromatographic run within 23 min.

Body-decorating products: Ingredients of permanent and temporary tattoos from analytical and european regulatory perspectives.

This review summarizes the current regulatory status of tattoos in all their versions in the European Union framework, as well as the analytical approaches developed so far to control the safety of this type of products. Publications from the last two decades (2000-2019) have been reviewed in which body-decorating products have become more and more popular. Tattoo inks, permanent make-up, sticker tattoos, and henna-based products are covered. The report highlights that there is no unique regulation for body art products, conforming a complex legislative framework even within the European community. The labelling of tattoo related products is generally non-existent or incorrect. It is therefore very difficult to know their chemical composition in detail. Pigments are ingredients common to all types of tattoos, so they are the most covered compounds in this review, along with their impurities and degradation products, including aromatic amines, metals or PAH. Other types of undesirable compounds are also included, such as plasticizers or para-phenylenediamine. Although the development of methods of analysis has increased in recent times, there is still margin for improvement in the analytical coverage of this topic. The challenge is, indeed, a systematic analytical approach to control body-decorating products, but ideally within a clear and common harmonised regulatory framework. Finally, tattoo-based sensors for biomonitoring have also been included in this review, since although its purpose is not decorative; its clinical importance is very relevant.

Footprints in the sand - Assessing the seasonal trends of volatile methylsiloxanes and UV-filters.

This study focused on the determination of seven volatile methylsiloxanes (VMSs) and eleven UV-filters (UVFs) in beach sand from the Oporto's region (Portugal). A QuEChERS methodology ("Quick, Easy, Cheap, Effective, Rugged, and Safe") was used to extract VMSs from the sand, which has never been employed before. To extract the UVFs, a solid-phase microextraction (SPME) was used. The analyses were performed by gas chromatography-mass spectrometry (GC-MS). Twenty-three beach sand samples were analysed, from two campaigns - summer/winter. VMSs were found in all the samples with concentrations ranging from 0.007 ±â€¯0.001 to 17.8 ±â€¯0.9 ng g-1dw, while UVFs in summer samples from 0.030 ±â€¯0.001 to 373 ±â€¯17 ng g-1dw. Cyclic VMSs and octocrylene (OC) were detected in higher concentrations. In general, higher levels were detected in summer than winter. Hazard quotients were determined and 3-(4'-methylbenzylidene) camphor (4-MBC), 2-ethylhexyl 4-methoxycinnamate (EMC) and benzophenone-3 (BP3) presented values >1, which may indicate that they may pose an ecotoxicological risk.

Extreme cosmetics and borderline products: an analytical-based survey of European regulation compliance.

The cosmetic industry currently focuses on products with magnified or exaggerated effects or extremely long-lasting characteristics. There are also a number of related commercial products for which the regulatory framework is far from clear; they are called 'borderline', and the European authorities only recommend which regulations they need to comply with. In any case, all these products must be safe under reasonable conditions of use in accordance with the applicable laws in force in the European Union (EU) framework. In this context, adequate analytical methodology is needed to evaluate the degree of compliance. Ultrasound Assisted Extraction (UAE) procedures for the analysis of 70 cosmetic ingredients have therefore been developed in this work. Moreover, for cosmetics with plastic applicators, a Supported-UAE (Sup-UAE) method was also opportunely optimized to check if a partial transfer of plasticizers to the cosmetics-and thereby to the consumers-could happen. In a survey of 50 commercial products (30 'extreme' and 20 'borderline'), the methods afforded mean recoveries of about 100% and RSD values lower than 5% for UAE and 10% for Sup-UAE, and with detection limits far below the legal requirements, for all the target compounds, thereby demonstrating their analytical suitability. Results are discussed in detail for phthalates, fragrances (musks and allergens) and some frequent preservatives. Additionally, a labelling study was performed to check if the consumer is correctly and fully informed. Graphical abstract ᅟ.

Simultaneous determination of preservatives and synthetic dyes in cosmetics by single-step vortex extraction and clean-up followed by liquid chromatography coupled to tandem mass spectrometry.

A simple methodology based on vortex extraction (VE) followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) has been developed for the simultaneous analysis of 22 regulated preservatives and synthetic dyes in cosmetics. The extraction procedure was performed in an Eppendorf tube allowing both extraction and clean-up in a single step, reducing sample and reagents consumption, and resulting in an effective and quick extraction. The method exhibited good linearity (R2 ≥ 0.9918) and intra and inter-day precision (%RSD ≤ 13) with LOQs lower than 0.587 µg g-1 for preservatives and 3.437 µg g-1 for synthetic dyes. Quantitative recoveries were obtained at four concentration levels in the range 2-100 µg g-1 in the cosmetic matrices. The method was successfully applied to a broad range of cosmetics, including both leave-on and rinse-off products in which 13 of the target compounds could be quantified at concentrations ranging from 0.39 to 442 µg g-1 in the case of dyes, and from 1.89 to 1335 µg g-1 for the preservatives. It can be highlighted the presence of parabens in 24 out of the 35 analyzed samples at concentrations higher than 1000 µg g-1 in a toothpaste.

Different miniaturized extraction methodologies followed by GC-MS/MS analysis for the determination of UV filters in beach sand.

Four different miniaturized methodologies were developed and applied to the analysis of 11 UV filters in sand samples. These approaches were based on ultrasound and vortex extractions, on-column lixiviation, and ultrasound extraction followed by solid-phase microextraction. Gas chromatography with tandem mass spectrometry was used for quantitative analysis. The analytical performance provided by the four methods was evaluated in terms of linearity, accuracy, precision, and limits of quantification. Lixiviation was discarded since it provided the lowest recoveries and the highest limits of quantification. In contrast, ultrasound and vortex extractions, and ultrasound extraction followed by solid-phase microextraction were suitable, with recoveries in general >85% and limits of quantification at the low ng/g level. Moreover, ultrasound extraction followed by solid-phase microextraction allowed using external calibration with aqueous standards and it provided higher sensitivity, with limits of quantification in general one order of magnitude lower than those achieved with the other techniques. The methodologies were applied for the analysis of four marine sand samples, and the results were statistically compared performing an analysis of variance. Eight out of the eleven target UV filters were detected. Octocrylene was found at very high concentrations (up to 1000 ng/g) followed by ethylhexyl salicylate, 4-methylbenzylidene camphor, homosalate, and 2-ethylhexyl methoxycinnamate.

Development and optimization of a solid-phase microextraction gas chromatography-tandem mass spectrometry methodology to analyse ultraviolet filters in beach sand.

A methodology based on solid-phase microextraction (SPME) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for the simultaneous analysis of eleven multiclass ultraviolet (UV) filters in beach sand. To the best of our knowledge, this is the first time that this extraction technique is applied to the analysis of UV filters in sand samples, and in other kind of environmental solid samples. Main extraction parameters such as the fibre coating, the amount of sample, the addition of salt, the volume of water added to the sand, and the temperature were optimized. An experimental design approach was implemented in order to find out the most favourable conditions. The final conditions consisted of adding 1 mL of water to 1 g of sample followed by the headspace SPME for 20 min at 100 °C, using PDMS/DVB as fibre coating. The SPME-GC-MS/MS method was validated in terms of linearity, accuracy, limits of detection and quantification, and precision. Recovery studies were also performed at three concentration levels in real Atlantic and Mediterranean sand samples. The recoveries were generally above 85% and relative standard deviations below 11%. The limits of detection were in the pg g-1 level. The validated methodology was successfully applied to the analysis of real sand samples collected from Atlantic Ocean beaches in the Northwest coast of Spain and Portugal, Canary Islands (Spain), and from Mediterranean Sea beaches in Mallorca Island (Spain). The most frequently found UV filters were ethylhexyl salicylate (EHS), homosalate (HMS), 4-methylbenzylidene camphor (4MBC), 2-ethylhexyl methoxycinnamate (2EHMC) and octocrylene (OCR), with concentrations up to 670 ng g-1.

Miniaturized matrix solid-phase dispersion followed by liquid chromatography-tandem mass spectrometry for the quantification of synthetic dyes in cosmetics and foodstuffs used or consumed by children.

Miniaturized matrix solid-phase dispersion (MSPD) followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) has been proposed for the simultaneous analysis of different classes of synthetic dyes in confectionery and cosmetics intended for or mostly consumed by children. Selected compounds include most of the permitted dyes as food additives as well as some of the most frequently used to color cosmetic products in accordance with the respective European directives. MSPD procedure was optimized by means of experimental design, allowing an effective, rapid and simple extraction of dyes with low sample and reagents consumption (0.1g of sample and 2mL of elution solvent). LC-MS/MS was optimized for good resolution, selectivity and sensitivity using a low ionic strength mobile phase (3mM NH4Ac-methanol). Method performance was demonstrated in real samples showing good linearity (R≥0.9928) and intra- and inter-day precision (%RSD≤15%). Method LODs were ≤0.952µgg-1 and ≤0.476µgg-1 for confectionery and cosmetic samples, respectively. Recoveries of compounds from nine different matrices were quantitative. The validated method was successfully applied to 24 commercial samples (14 cosmetics and 10 foods) in which 9 of the selected dyes were found at concentrations up to 989µgg-1, exceeding in some cases the regulated maximum permitted limits. A non-permitted dye, Acid Orange 7, was found in one candy.

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction.

Camellia (genus of flowering plants of fam. Theaceae) is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain) and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD), and analyzed by gas chromatography (GC) with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition.

Simultaneous in-vial acetylation solid-phase microextraction followed by gas chromatography tandem mass spectrometry for the analysis of multiclass organic UV filters in water.

UV filters are a class of emerging contaminants that are widely used in personal care products (PCPs) and that can be detected at low concentrations in the aquatic environment (ngL-1). Sensitive modern analytical methods are then mandatory to accurately analyze them. A methodology based on solid-phase-microextraction (SPME), considered as a 'Green Chemistry' technique, followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for the simultaneous analysis of 14 UV filters of different chemical nature in environmental and recreational waters. In-vial low-cost derivatization was carried out to improve chromatographic performance of phenolic compounds. The extraction parameters (fiber coating, extraction mode, and salt addition) were optimized by means of experimental designs in order to achieve reliable conditions. Finally, the SPME-GC-MS/MS method was validated in terms of linearity, accuracy and precision with LODs in the low ngL-1 level. Its application to the analysis of 28 different samples including sea, river, spa, swimming pool, and aquapark waters, enabled the detection of 11 target UV filters at concentration levels up to 540µgL-1, highlighting the presence of OCR in all analyzed samples and of 2EHMC (proposed to be considered as priority pollutant) in 79% of them.