Extraction and analysis of cannabinoids: A decade of progress, challenges and future directions.

Cannabis is the most widely consumed illicit drug worldwide and its rapid expansion into medical and recreational markets has highlighted the need for effective analytical techniques. The analysis of major cannabinoids and their metabolites in different matrices has recently gained considerable attention in fields such as forensics, healthcare, environmental monitoring, and the cannabis food industry. However, the complexity of these matrices, ranging from biological samples to cannabis-infused products, raises significant challenges that require selective and effective extraction methods prior to chromatographic analysis.

Phenolic extraction from prickly pear peels using deep eutectic solvents with macrocyclic enhancers.

The study valorizes prickly pear peels, traditionally considered agro-waste, as a source of phenolic antioxidants using an eco-friendly extraction method. Natural deep eutectic solvents (NaDESs) combined with ultrasound-assisted extraction were optimized via response surface methodology to maximize phenolic recovery (80 % v/v choline chloride-citric acid NaDES in water, 30 mL/g solvent-to-solid ratio, 16-min extraction time). HPLC analysis identified catechin, myricetin, rutin, and gallic acid.

Enantiomeric separation of nefopam and cathinone derivatives using a supramolecular deep eutectic solvent as a chiral selector in capillary electrophoresis.

The present study investigates the utilization of a supramolecular deep eutectic solvent (SUPRADES), consisting of sulfated-β-cyclodextrin (S-β-CD) and citric acid (CA), as a chiral selector (CS) in capillary electrophoresis for the enantiomeric separation of nefopam (NEF) and five cathinone derivatives (3-methylmethcathinone [3-MMC], 4-methylmethcathinone [4-MMC], 3,4-dimethylmethcathinone [3,4-DMMC], 4-methylethcathinone [4-MEC], and 3,4-methylendioxycathinone [MDMC]). A significant improvement in enantiomeric separation of the target analytes was observed upon the addition of S-β-CD-CA to the background electrolyte (BGE), leading to a baseline separation of all analytes. In particular, the optimum percentage of S-β-CD-CA, added to the BGE, was determined to be 0.

The Utilization of an Aloe Vera Rind By-Product: Deep Eutectic Solvents as Eco-Friendly and Recyclable Extraction Media of Polyphenolic Compounds.

In this study, an optimized environmentally friendly procedure was employed to enhance the sustainable utilization of phenolic antioxidants derived from aloe vera rind by-products. The procedure involved the application of ultrasound-assisted extraction (UAE) in combination with deep eutectic solvents (DESs). Eleven different DESs and three conventional solvents were employed as extraction media for polyphenolic compounds.

Novel supramolecular deep eutectic solvent (SUPRADES) as a sole chiral selector in capillary electrophoresis for the enantiomeric separation of fluorine-substituted amphetamine analogs.

In this study, a novel supramolecular deep eutectic solvent consisting of sulfated-β-CD and citric acid (S-β-CD-CA) is reported for the first time. This innovative system was evaluated as a sole chiral selector in capillary electrophoresis for the enantioseparation of six fluorine-substituted amphetamine analogs, yielding remarkable outcomes. Baseline separations of all amphetamine analogs under study were achieved in less than 21.

Stereoselective separation of psychoactive substances: Multivariate optimization and validation of a capillary electrophoresis method using carboxymethyl-β-CD/deep eutectic solvent dual system.

A comprehensive study was performed to determine an optimum enantioseparation method for fluorine-substituted amphetamine and cathinone derivatives (fluor-amphetamine and fluor-cathinone derivatives), using a binary system consisting of carboxymethyl-β-CD (CM-β-CD) and a deep eutectic solvent (DES), namely choline chloride-ethylene glycol (ChCl-EG). Under this framework, the optimization and modeling of the separation conditions in a binary system were performed with the objective of maximizing resolution and minimizing analysis time. This was achieved through the application of response surface methodology.

The potential of the use of deep eutectic solvents and amino acid-based ionic liquids to enhance the chiral discrimination ability of different chiral selectors in capillary electrophoresis.

The effect of the combined use of amino acid-based ionic liquids (AAILs) and deep eutectic solvents (DESs) with either cyclodextrin- (CD) or cyclofructan- (CF) based chiral selectors for the chiral separation of amphetamine derivatives was investigated in the present study. A non-significant improvement in enantiomeric separation of target analytes was observed when AAILs were combined with either CF or CD. On the other side, a markedly improved chiral separation of enantiomers was obtained using the dual carboxymethyl-β-cyclodextrin/DES system, highlighting the existence of a synergistic effect.

Phenolic Profile, Antioxidant Activity, and Chemometric Classification of Carob Pulp and Products.

In recent years, carob and its derived products have gained wide attention due to their health-promoting effects, which are mainly attributed to their phenolic compounds. Carob samples (carob pulps, powders, and syrups) were analyzed to investigate their phenolic profile using high-performance liquid chromatography (HPLC), with gallic acid and rutin being the most abundant compounds. Moreover, the antioxidant capacity and total phenolic content of the samples were estimated through DPPH (IC 98.

Evaluation of cyclodextrin- and cyclofructan-based chiral selectors for the enantioseparation of psychoactive substances in capillary electrophoresis.

During this study, a simple and easy-to-prepare electrophoretic method was developed for the enantioseparation of amphetamine and cathinone derivatives. Different types of β-cyclodextrin and cyclofructan-based chiral selectors (CSs), both native and derivatized, were utilized, and the most effective ones, in terms of resolution and analysis time, were identified. In addition, several electrophoretic parameters, such as background electrolyte concentration and pH, and CS concentration, were examined to optimize the separation conditions.

Comparison of cyclofructan-, cyclodextrin-, and polysaccharide-based chiral stationary phases for the separation of pharmaceuticals.

In this study, cyclofructan (CF)-, cyclodextrin (CD)-, and polysaccharide-based chiral stationary phases (CSPs) were exploited in high-performance liquid chromatography (HPLC) for the chiral separations of different clinically and pharmaceutically important compounds. In particular, R-naphthylethyl carbamate CF6 (RN-CF6), 3,5-dimethylphenyl carbamate CF7 (DMP-CF7), neutral beta cyclodextrin (β-CD), 3,5-dimethylphenyl carbamate β-CD (DMP-β-CD), and cellulose tris-(3,5-dimethylphenylcarbamate) (Cellulose-Tris DMP) columns were utilized under isocratic elution. The performance of these CSPs as chiral separation media was evaluated by use of nine analytes: acidic, basic, and amphiprotic.

Anti-Cancer Activity and Phenolic Content of Extracts Derived from Cypriot Carob ( L.) Pods Using Different Solvents.

Extracts derived from the L. (carob) tree have been widely studied for their ability to prevent many diseases mainly due to the presence of polyphenolic compounds. In this study, we explored, for the first time, the anti-cancer properties of Cypriot carobs.

Combined use of β-cyclodextrin and ionic liquid as electrolyte additives in EKC for separation and determination of carob's phenolics-A study of the synergistic effect.

In this work, a simple, reliable, and fast capillary electrophoretic method was developed and validated for the simultaneous determination of 12 polyphenolic compounds, the most frequently found in carob's pulp and seeds. The present work deals with the development of a novel dual electrophoretic system based on the combined use of β-CD and ionic liquid (IL) as buffer additives. A baseline separation of the target analytes was achieved in less than 10 min by using a BGE consisting of 35 mM borate along with 15 mM β-CD and 3 mM l-alanine tert butyl ester lactate (l-AlaC Lac) IL as buffer additives at pH 9.

Continuous and pulsed ultrasound-assisted extraction of carob's antioxidants: Processing parameters optimization and identification of polyphenolic composition.

Polyphenols in carobs have recently attracted great attention due to their wide range of biological and health promoting effects. A comprehensive study was conducted to find an optimum method for the extraction, purification and characterization of these valuable bioactive substances. Under this framework, the ultrasound-assisted extraction (UAE) of polyphenols from carob pulp was optimized by the maximization of the yield in total phenolics using response surface methodology.

Analysis of cannabinoids in conventional and alternative biological matrices by liquid chromatography: Applications and challenges.

Cannabis is by far the most widely abused illicit drug globe wide. The analysis of its main psychoactive components in conventional and non-conventional biological matrices has recently gained a great attention in forensic toxicology. Literature states that its abuse causes neurocognitive impairment in the domains of attention and memory, possible macrostructural brain alterations and abnormalities of neural functioning.

Application of an ultra-performance liquid chromatography-tandem mass spectrometric method for the detection and quantification of cannabis in cerumen samples.

In this study, cerumen, a non-conventional biological secretion, was examined as an alternative matrix for forensic analyzis. A fully validated analytical UPLC-MS/MS method was developed for the detection and quantification of the most prevalent psychoactive illicit drug globe wide, Δ-tethrahydrocannabinol, commonly known as THC, and four major cannabinoids found in cannabis Sativa. The method was validated, and standard external calibration curves were established with correlation coefficients > 0.

An extensive case study on the dispersion parameters of HI-assisted reduced graphene oxide and its graphene oxide precursor.

The formation of highly concentrated and stable graphene derivatives dispersions remains a challenge towards their exploitation in various applications, including flexible optoelectronics, photovoltaics, 3D-printing, and biomedicine. Here, we demonstrate our extensive investigation on the dispersibility of graphene oxide (GO) and reduced graphene oxide (RGO) in 25 different solvents, without the use of any surfactant or stabilizer. Although there is a significant amount of work covering the general field, this is the first report on the dispersibility of: a) RGO prepared by a HI/AcOH assisted reduction process, the method which yields RGO of higher graphitization degree than the other well-known reductants met in the literature, b) both GO and RGO, explored in such a great range of solvents, with some of them not previously reported.

Synergistic enantioseparation systems with either cyclodextrins or cyclofructans and L-alanine Tert butyl ester lactate.

The combined use of chiral ionic liquids (CILs) and conventional chiral selectors (CSs) in CE, to establish a synergistic system, has proven to be an effective approach for the separation of enantiomeric pairs. In this study, a new CE method was developed, employing a binary system of a CS, either a cyclodextrin (CD) or a cyclofructan (CF), and a chiral amino acid ester-based ionic liquid (AAIL), for the chiral separation of four basic, acidic and zwitterionic drug compounds. In particular, the enantioseparation of two anticoagulants, warfarin (WAR) and coumachlor (COU), a non-opioid analgesic, nefopam (NEF) and a third-generation antihistamine, fexofenadine (FXD), was examined, by supporting the BGE with a CS and the chiral AAIL L-alanine tert butyl ester lactate (L-AlaC Lac).

Polyphenols in carobs: A review on their composition, antioxidant capacity and cytotoxic effects, and health impact.

Carob (Ceratonia Siliqua L., tree of the pea family Fabaceae) and its products have recently attracted great interest due to their polyphenolic composition. This review summarizes the polyphenolic compounds that are contained in different carob parts (leaves, pod, seeds, barks) and products (syrup, flour, fiber).

Chiral selectors in CE: Recent development and applications (mid-2014 to mid-2016).

This report, which is a sequence of a series of reviews, records the most important chiral selectors (CSs) applied in CE. It highlights the CSs that were used during the period 2014 to mid-2016. In this review, method developments, validations, and pharmaceutical along with biomedical applications are presented.

Enantioseparations in open-tubular capillary electrochromatography: Recent advances and applications.

This review highlights recent advances and applications in open-tubular capillary electrochromatography (OT-CEC) for enantioseparations during the last decade. Although extensive research has been conducted in the area of separations by use of CEC, and a big number of reviews have been published, there is not a review on exclusively the use of chiral stationary phases (CSPs) in OT-CEC for enantioseparations. Therefore, in this review, the design and synthesis of different CSPs are presented, and their potential applications in OT-CEC for enantioseparations are discussed.

Combined use of cyclofructans and an amino acid ester-based ionic liquid for the enantioseparation of huperzine A and coumarin derivatives in CE.

Cyclofructans (CFs) and their derivatives have recently been proven to be efficient chiral selectors (CSs) for the enantioseparation of several analytes in CE, HPLC, and GC. In this study, the chiral separation ability of a number of native and derivatized CFs was examined in CE. Particularly, six different CFs, with different derivatization groups and cavity sizes [native CF-6 and CF-7, isopropyl cyclofructan-6 (IPCF-6), IPCF-7, sulfated cyclofructan-6 (SCF-6), and SCF-7] were used as CSs for the enantioseparation of huperzine A, warfarin, and coumachlor.

Chiral selectors in CE: recent developments and applications (2012-mid 2014).

There is a large number of chiral selectors (CSs) that have, over the years, been synthesized and used in electrophoretic enantioseparations. This report highlights the most important CSs applied in CE during the period 2012 to mid-2014. It is mainly focused on method developments and validations, along with pharmaceutical and biomedical applications.

Chiral ionic liquids in chromatographic and electrophoretic separations.

This report provides an overview of the application of chiral ionic liquids (CILs) in separation technology, and particularly in capillary electrophoresis and both gas and liquid chromatography. There is a large number of CILs that have been synthesized and designed as chiral agents. However, only a few have successfully been applied in separation technology.

Chiral separation of the clinically important compounds fucose and pipecolic acid using CE: determination of the most effective chiral selector.

In this study, simple electrophoretic methods were developed for the chiral separation of the clinically important compounds fucose and pipecolic acid. In recent years, these analytes, and particularly their individual enantiomers, have attracted considerable attention due to their role in biological functions and disorders. The detectability and sensitivity of pipecolic acid and fucose were improved by reacting them with fluorenylmethyloxycarbonyl chloride (FMOC-Cl) and 5-amino-2-naphthalene-sulfonic acid (ANSA), respectively.

Facile preparation of polysaccharide-coated capillaries using a room temperature ionic liquid for chiral separations.

In this study, the dissolution of polysaccharides into an ionic liquid was investigated and applied as a coating onto the capillary walls of a fused-silica capillary in open-tubular CEC. The coating was evaluated by examining the chiral separation of two analytes (thiopental, sotalol) with three cellulose derivatives (cellulose acetate, cellulose acetate phthalate, and cellulose acetate butyrate). Baseline separation of thiopental enantiomers was achieved by use of each polysaccharide coating (Rs: 7.