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In the last decade, several developments, particularly in the liquid chromatography and hyphenated techniques fields, have allowed researchers to reach analytical limits that are becoming very close to the single molecule level. Sample preparation, however, despite being a key step in the analytical methodology, did not track these developments and very few approaches able to cope with these stringent analytical requirements were developed. One such approach is microextraction by packed sorbent (MEPS), a sophisticated and miniaturized form of solid phase extraction that has reduced to the microliter scale every step of the sample extraction methodology including sample volume and solvent usage. Simultaneously, the amount of extraction phase used was also reduced and, more importantly, the sorbent is reusable dozens of times which significantly lowers the cost of analysis versus other solid-phase extraction approaches. In this review, we will update the state-of-the-art of the MEPS technique, focusing on the trends and applications reported since 2010 and future perspectives and developments that in our view will further improve the high-throughput potential and applications of this sample preparation methodology. KeywordsMicroextraction by packed sorbent (MEPS) • eVol • Sample preparation • Solid phase extraction (SPE) © 2013 J. Pereira et al., licensee Versita Sp. z o. o. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivs license, which means that the text may be used for non-commercial purposes, provided credit is given to the author Unauthenticated Download Date | 12/26/14 1:57 PM Microextraction using packed sorbent as an effective and high-throughput sample extraction technique: Recent applications and future trends. Unauthenticated Download Date | 12/26/14 1:57 PM J. Pereira et al. 40 Unauthenticated Download Date | 12/26/14 1:57 PM Microextraction using packed sorbent as an effective and high-throughput sample extraction technique: Recent applications and future trends. Unauthenticated Download Date | 12/26/14 1:57 PM Microextraction using packed sorbent as an effective and high-throughput sample extraction technique: Recent applications and future trends.

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The word "cannabinoid" refers to every chemical substance, regardless of structure or origin, that joins the cannabinoid receptors of the body and brain and that have similar effects to those produced by the Cannabis plant and based on their source of production, cannabinoids can be classified into endocannabinoids, phytocannabinoids and synthetic cannabinoids. Synthetic cannabinoids represent the largest class of drugs detected through the EU Early Warning System with a total of 190 substances notified from 2008 to 2018 and about 280 have been reported worldwide to the United Nations Office on Drugs and Crime. Sprayed on natural herb mixtures with the aim to mimic the euphoria effect of cannabis and sold as "herbal smoking blends" or "herbal incense" under brand names like "Spice" or "K2", synthetic cannabinoids are available from websites for the combination with herbal materials or more recently, for the use in e-cigarettes. Currently labeled as "not for human consumption" to circumvent legislation, their legal status varies by country with many government institutions currently pushing for their control. However, due to the emergence of new substances, it requires a constant update of the list of controlled drugs. Little is known about how these substances work and their toxic effects in humans and the same product could vary not only in the amount and in the type of substance added. In the last years, synthetic cannabinoids have been associated with deaths and acute intoxications in Europe and, despite a range of new measures introduced in this area, continue to represent a challenge to current drug policy models. These synthetic substances are much more potent than natural cannabis, as well as displayed greater efficacy, acting as full agonists at the cannabinoid receptors. It is possible that, along with being highly potent, some may also have long half-lives, potentially leading to a prolonged psychoactive effect. The present work provides a review on existing literature about the development of synthetic cannabinoids as substances of abuse, current patterns of abuse and their legal status, chemical classification, and some pharmacological and toxicological properties.

The human population continues to grow exponentially in the fast developing and most populated countries, whereas in Western Europe it is getting older and older each year. This inevitably raises the demand for better and more efficient medical services without increasing the economic burden in the same proportion. To meet these requirements, improvement of medical diagnosis is certainly a key aspect to consider. Therefore, we need powerful analytical methodologies able to go deeper and further in the characterization of human metabolism and identification of disease biomarkers and endogenous molecules in body fluids and tissues. The ultimate goal is to have a reliable and early medical diagnosis, mitigating the disease complications as much as possible. Microextraction techniques (METs) represent a key step in these analytical methodologies by providing samples in the suitable volumes and purification levels necessary for the characterization of the target analytes. In this aspect, solid-phase microextraction (SPME) and, more recently, microextraction by packed sorbent (MEPS), are powerful sample preparation techniques, characterized by their reduced time of analysis, low solvent consumption, and broad application. Moreover, as miniaturized techniques, they can be easily automatized to have a high-throughput performance in the clinical environment. In this review, we explore some of the most interesting MEPS and SPME applications, focusing on recent trends and applications to medical diagnostic, particularly the in vivo and near real time applications.

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Fruits and vegetables are considered a good source of antioxidants, which are beneficial in protecting the human body against damage induced by free radicals and other reactive oxygen (ROS) and nitrogen (RNS) species. In this work, we aimed to evaluate the integral antioxidant activity (AOA) and determine individual polyphenols in fruits and vegetables of frequent consumption. For this purpose, an innovative and high throughput analytical approach based on original QuEChERS assisted by ultrasound extraction (USAE), instead of the manual agitation used in the classical procedure, was optimized and implemented for the isolation of polyphenols. The total phenolic content (TPC), flavonoids, anthocyanins, and betalains were evaluated using different spectrophotometric assays. In addition, free radical scavenging by methods 2,2’-azinobis-(3-ethylbenzothiazoline-6-sulfonate) (ABTS) and 2,2′-diphenyl-1-picrylhydrazyl (DPPH) and ferric reducing antioxidant power (FRAP) were used to estimate the AOA of the investigated fruit and vegetable extracts. Red onion, tamarillo, and beetroot were the samples with the highest AOA. The quantification and identification of free low molecular weight polyphenols from QuEChERS-USAE extracts was carried out by ultra-high-pressure liquid chromatography equipped with a photodiode array detection system (UHPLC-PDA). Catechin was the most abundant polyphenol, followed by gentisic and ferulic acids, mainly in the watercress sample. In relation to flavonols, quercetin and kaempferol were found mostly in onion samples, and in small quantities in tomato and watercress. The improved analytical approach, QuEChERS-USAE/UHPLC-PDA, offers an attractive alternative for the analysis of polyphenols from fruit and vegetable samples, providing several advantages over traditional extraction techniques, in terms of reproducibility, simplicity, low cost, analysis speed, and analytical performance.

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