► Theoretical and experimental aspects of ultrasound extraction. ► Recent advances in ultrasound extraction. ► Comparison of advantages and disadvantages of ultrasound extraction with other ...techniques. ► Ultrasound extraction applied to food and environmental analysis in 2010–12.
In recent years, ultrasound-assisted extraction (UAE) has attracted growing interest, as it is an effective method for the rapid extraction of a number of compounds from food and environmental samples, with extraction efficiency comparable to that of classical techniques. In particular, recently, numerous analytical applications of this technique dealt with the extraction of natural compounds and pollutants from food and environmental samples.
This review gives a brief presentation of the theory of UAE, discusses recent advances that influence its efficiency, and summarizes the main results in selected applications published in the period 2010–12. There is discussion of the advantages and the disadvantages of UAE and the possibility of coupling UAE with other analytical techniques.
The analysis, prevention, and removal of microplastics (MPs) pollution in water is identified as one major problem the world is currently facing. MPs can be directly released to water or formed by ...the degradation of bigger plastics. Nowadays, it is estimated that annually between 4 and 12 million tonnes of plastic go into the seas and oceanswith a forecast for them to outweigh the amount of fish in 2050. Based on the existing studies, the characterization of MPs in waters is still one of the remaining challenges because they can be easily confused with organic or other types of matter. Consequently, there is an urgent necessity to establish pathways for the chemical identification of the MP nature. In this perspective, the recent techniques and instrumentation for MP characterization (Raman and Fourier-transform infrared spectroscopies and microscopies, pyrolysis and thermal desorption gas chromatography, imaging techniques, etc.) are discussed including considerations to the multidimensionality of the problem. This perspective also summarizes and provides updated data on the sources and occurrence, transport and fate of MPs in aquatic ecosystems, as well as influencing conditions and factors affecting dispersal. Additionally, how engineering and biotechnological tools, such as advanced water treatments, would help to control, reduce, or even eliminate MP pollution in the near future is outlined.
Pyrolysis gas chromatography-mass spectrometry (Py-GC-MS) has great potential within environmental analysis. This technique is mainly used for the chemical identification of macromolecules that ...cannot be characterized by either liquid or gas chromatography due to their big size. Through pyrolysis (controlled thermal degradation), these macromolecules are broken down into simpler molecules that can be separated by gas chromatography and detected by mass spectrometry. This technique has been traditionally used in environmental samples for the characterization of organic matter and humic substances, contaminants, lignins, etc. It attains the identification of the different types of chemical units that integrate the macromolecules. In addition, recently, this technique has experienced an important boom in the chemical characterization of microplastics present in environmental samples. This has triggered its use in this type of matrix. We describe the fundamentals and modalities of Py-GC-MS and outline some of the recent applications for the environmental analysis with special emphasis on humic substances and/or other types of organic matter components as well as microplastics, but reporting also other interesting application of environmental relevance.
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•Recent innovations in Py-GC-MS for environmental analysis are presented.•Advances in the design of currently used pyrolyzers are discussed.•Recently developed working modes within Py-GC-MS are described.•Py-GC-MS applications to organic matter and microplastics are highlighted.•Progresses and promising trends in Py-GC-MS analysis are pointed out.
This book reviews new technology and challenges in food analysis from multiple perspectives: a review of novel technologies being used in food analysis, an in-depth analysis of several specific ...approaches, and an examination of the most innovative applications and future trends. The book is structured in two parts: the first describes the role of the latest developments in analytical and bio-analytical techniques and the second reviews the most innovative applications and issues in food analysis. Each chapter is written by experts on the subject and is extensively referenced in order to serve as an effective resource for more detailed information. The techniques discussed range from the non-invasive and non-destructive, such as infrared spectroscopy and ultrasound, to emerging areas such as nanotechnology, biosensors and electronic noses and tongues. Important tools for problem-solving in chemical and biological analysis are discussed in detail.
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•First nationwide study in Spain assessing exposure to phthalates by analysing sewage.•17 sewage treatment plants serving 13 cities and ca. 6 million people sampled.•Estimated levels ...in urine close to levels reported in literature for 5 metabolites.•Average exposure levels for parent phthalates ranged from 2 to 1347 μg/(day∙inh).•Safe reference values of butylated phthalates exceeded in some sites.
Phthalates are widely used plasticizers that produce endocrine-disrupting disorders. Quantifying exposure is crucial to perform risk assessments and to develop proper health measures. Herein, a wastewater-based epidemiology approach has been applied to estimate human exposure to six of the mostly used phthalates within the Spanish population. Wastewater samples were collected over four weekdays from seventeen wastewater treatment plants serving thirteen cities and ca. 6 million people (12.8 % of the Spanish population). Phthalate metabolite loads in wastewater were transformed into metabolite concentrations in urine and into daily exposure levels to the parent phthalates. Considering all the sampled sites, population-weighted overall means of the estimated concentrations in urine varied between 0.7 ng/mL and 520 ng/mL. Very high levels, compared to human biomonitoring data, were estimated for monomethyl phthalate, metabolite of dimethyl phthalate. This, together with literature data pointing to other sources of this metabolite in sewage led to its exclusion for exposure assessments. For the remaining metabolites, estimated concentrations were closer to those found in urine. Their 4-days average exposure levels ranged from 2 to 1347 μg/(day∙inh), exceeding in some sites the daily exposure thresholds set for di-i-butyl phthalate and di-n-buthyl phthalate by the European Food Safety Authority.
•Developments in the determination of ENMs in food are detailed.•Problems and limitations of sample preparation protocols are discussed.•A critical review of analytical methods for determination of ...ENMs in food is presented•Challenges are outlined and future prospects envisaged.
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Detection, characterization, and quantification of engineering nanomaterials (ENMs) in foods is still a pending issue that needs to be tackle to protect consumers and to fix some related aspects (e.g. labelling or control). The global challenge for the analytical sciences is that ENMs are a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). In this critical review, we evaluate and compare the procedures involved in the analytical methods and studies developed thus far for the identification and quantification of ENMs in food. We discuss advantages and limitation as well as prospects. We pointed out the main specific challenges that remain within this topic. Finally, we also envisaged future perspectives on the determination of ENMs.
Data obtained from wastewater analysis can provide rapid and complementary insights in illicit drug consumption at community level. Within Europe, Spain is an important country of transit of both ...cocaine and cannabis. The quantity of seized drugs and prevalence of their use rank Spain at the top of Europe. Hence, the implementation of a wastewater monitoring program at national level would help to get better understanding of spatial differences and trends in use of illicit drugs. In this study, a national wastewater campaign was performed for the first time to get more insight on the consumption of illicit drugs within Spain. The 13 Spanish cities monitored cover approximately 6 million inhabitants (12.8% of the Spanish population). Untreated wastewater samples were analyzed for urinary biomarkers of amphetamine, methamphetamine, MDMA, cocaine, and cannabis. In addition, weekend samples were monitored for 17 new psychoactive substances. Cannabis and cocaine are the most consumed drugs in Spain, but geographical variations showed, for instance, comparatively higher levels of methamphetamine in Barcelona and amphetamine in Bilbao, with about 1-fold higher consumption of these two substances in such metropolitan areas. For amphetamine, an enantiomeric profiling was performed in order to assure the results were due to consumption and not to illegal dumping of production residues. Furthermore, different correction factors for the excretion of cannabis were used to compare consumption estimations. All wastewater results were compared with previously reported data, national seizure data and general population survey data, were a reasonable agreement was found. Daily and yearly drug consumption were extrapolated to the entire Spanish population with due precautions because of the uncertainty associated. These data was further used to estimate the retail drug market, where for instance cocaine illicit consumption alone was calculated to contribute to 0.2–0.5% of the Spanish gross domestic product (ca. 3000–6000 million Euro/year).
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•First national wastewater campaign to estimate illicit drug consumption in Spain•Methamphetamine and MDMA positively correlated to population size•NPS were only detected sporadically at low concentrations in wastewater•Agreement between WBE consumption estimates and other indicators for several drugs•Size of the retail drug market and contribution to gross domestic product estimated
The occurrence of 21 acidic pharmaceuticals, including illicit drugs, and personal care products (PPCPs) in waste, surface and drinking water and in sediments of the Turia River Basin (Valencia, ...Spain) was studied. A liquid chromatography tandem mass spectrometry (LC–MS/MS) method was developed for the determination of these PPCPs with electrospray (ESI) in negative ionization (NI) mode. Ammonium fluoride in the mobile phase improved ionization efficiency by an average increase in peak area of 5 compared to ammonium formate or formic acid. All studied compounds were detected and their concentration was waste water>surface water>drinking water. PPCPs were in waste water treatment plants (WWTPs) influents up to 7.26μgL−1, dominated by ibuprofen, naproxen and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCOOH). WWTPs were highly effective in removing most of them, with an average removal rate of >90%. PPCPs were still detected in effluents in the 6.72–940ngL−1 range, with the THCOOH, triclocarban, gemfibrozil and diclofenac as most prevalent. Similarly, diclofenac, gemfibrozil, ibuprofen, naproxen and propylparaben were detected quite frequently from the low ngL−1 range to 7μgL−1 in the surface waters of Turia River. Ibuprofen, methylparaben, salicylic acid and tetrahydrocannabinol (THC) were at concentrations up to 0.85ngg−1 d.w. in sediments. The discharge of WWTP as well as of non-treated waters to this river is a likely explanation for the significant amount of PPCPs detected in surface waters and sediments. Mineral and tap waters also presented significant amounts (approx. 100ngL−1) of ibuprofen, naproxen, propylparaben and butylparaben. The occurrence at trace levels of several PPCPs in drinking water raises concerns about possible implications for human health.
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•The occurrence of 21 PPCPs was assessed in waste, surface and drinking water and in sediments.•NH4F as mobile phase modifier in LC–ESI(−)–MS/MS ensures sensitive and precise monitoring data.•Diclofenac, naproxen and propylparaben were the most frequent in waters.•Ibuprofen, methylparaben, salicylic acid and THC were at the highest concentration in sediments.
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•First nationwide study in Spain to assess alcohol consumption from a wastewater biomarker.•Circa 6 million people (12.8% of the Spanish population) covered in the ...sampling.•Wastewater-derived alcohol consumption figures ranged from 4.5 to 46 mL/day/inhabitant.•Significant differences in consumption among regions and between weekdays and weekends.•Wastewater-derived estimates comparable with National Health Survey data.
In this study, an alternative and complementary method to those approaches currently used to estimate alcohol consumption by the population is described. This method, known as wastewater-based epidemiology (WBE), allows back-calculating the alcohol consumption rate in a given population from the concentrations of a selected biomarker measured in wastewater.
Composite (24-h) wastewater samples were collected at the inlet of 17 wastewater treatment plants located in 13 Spanish cities for seven consecutive days in 2018. The sampled area covered 12.8% of the Spanish population. Wastewater samples were analyzed to determine the concentration of ethyl sulfate, the biomarker used to back-calculate alcohol consumption.
Alcohol consumption ranged from 4.5 to 46 mL/day/inhabitant. Differences in consumption were statistically significant among the investigated cities and between weekdays and weekends. WBE-derived estimates of alcohol consumption were comparable to those reported by its corresponding region in the Spanish National Health Survey in most cases. At the national level, comparable results were obtained between the WBE-derived annual consumption rate (5.7 ± 1.2 L ethanol per capita (aged 15+)) and that reported by the National Health Survey (4.7 L ethanol per capita (aged 15+)).
This is the largest WBE study carried out to date in Spain to estimate alcohol consumption rates. It confirms that this approach is useful for establishing spatial and temporal patterns of alcohol consumption, which could contribute to the development of health care management plans and policies. Contrary to established methods, it allows obtaining information in a fast and relatively economical way.
Pressurized liquid extraction (PLE) is a tool able to provide green extraction methods to further determine contaminants in food and the environment. The aim of this review is to offer a critical ...overview of the recent developments within this field and can be considered as an update of the previous that we published in 2015. Trends regarding sample treatment, solvents, in-cell clean-up approaches used in the extraction of organic contaminants are addressed. Special attention deserve those methods that include on-line clean up in the extraction cell. Comparison with other green techniques is also presented. The final objective of this review is to clearly define the role that this technique plays in the analysis of organic pollutants, their strengths and weaknesses, as well as the updated spectrum of applications for which PLE is an essential tool.
•Update review of the PLE to extract contaminants in food and the environment.•Establishment of the applications for which PLE is advantageous.•Main analytical parameters of the different PLE procedures are discussed.•Advantages and limitations in the analysis are considered and evaluated.•Future trends and prospects are envisaged.
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