Search Results (44)

Grape pomace is one of the most abundant byproducts of the wine industry. This by-product contains many valuable bioactive substances, including polysaccharides, amino acids, and polyphenols. To enable its effective reuse, this study developed and optimized a micelle-assisted extraction process using a 2% (w/w) decyl glucoside solution aqueous as an extraction medium. The influence of key process parameters—the pomace-to-medium ratio, extraction temperature, and extraction time—was systematically evaluated to determine their impact on extraction yield and the physicochemical properties of the recovered compounds. Extraction efficiency was assessed by determining total phenolic content (TPC) and antioxidant capacity (DPPH, ABTS) using UV-VIS spectrophotometry and by determining selected phenolic compounds, amino acids, and sugars using Ultraperformance Liquid Chromatography Coupled with Tandem Mass Spectrometry (UPLC-MS/MS) The results demonstrated that all the parameters investigated significantly influenced the recovery of bioactive substances. The developed decyl glucoside-based micellar extraction proved to be an efficient, low-temperature, and environmentally favorable method for valorizing grape pomace, offering strong potential for cosmetic and related applications. Full article

This study reports the synthesis and catalytic evaluation of a series of imidazolium-based polymeric ionic liquids (PILs) for the cycloaddition of CO₂ to epichlorohydrin (ECH). The synthesized catalysts include homopolymers, poly(3-hydroxyethyl-1-vinylimidazole chloride) (p[HVIm][Cl]) and poly(3-carboxymethyl-1-vinylimidazole chloride) (p[CMVIm][Cl]), and their block copolymers with polystyrene, synthesized for the first time, pS-b-p[HVIm][Cl] and pS-b-p[CMVIm][Cl]. Structural characterization by NMR, IR spectroscopy, and gel permeation chromatography confirmed the successful synthesis. The block copolymers exhibited a low polydispersity index (PDI 1.1–1.2), which is indicative of homogeneous chain lengths and the propensity to form ordered nanostructures, whereas the homopolymers showed higher PDI (2.4–2.9). Catalytic testing at 90 °C and 1 MPa CO₂ for 4 h revealed a clear activity trend: p[CMVIm][Cl] < p[HVIm][Cl] < pS-b-p[CMVIm][Cl] < pS-b-p[HVIm][Cl], with conversions exceeding 75% for all catalysts and a maximum of 82.69% for pS-b-p[HVIm][Cl]. These results demonstrate that the catalytic performance of PILs is governed by a synergistic interplay between the local chemical functionality of the ionic moiety and the overall polymer architecture. Based on these results, the synthesized polymeric ionic liquids, particularly pS-b-p[HVIm][Cl], demonstrate strong potential for creating multifunctional materials. Their ability to self-assemble into ordered nanostructures with distinct hydrophobic and hydrophilic domains provides a foundational architecture for combined gas separation and catalysis. The observed “micellar catalytic effect”, which enhances local reagent concentration near active sites, could be leveraged in a membrane reactor to simultaneously capture and convert CO₂ directly within the membrane. This integrated “separation–reaction” approach represents a promising strategy for advancing circular carbon economy technologies. Full article

Many polar compounds of biochemical and pharmaceutical relevance exhibit low retention in reversed-phase liquid chromatography (RPLC), making their separation challenging. While hydrophilic interaction liquid chromatography (HILIC) columns are commonly used for such analyses, they require mobile phases with high organic solvent content. This work explores an alternative approach using RPLC with conventional C18 columns and mobile phases containing low percentages of acetonitrile, along with small amounts of the surfactant sodium dodecyl sulfate (SDS). This combination significantly enhances the retention of highly polar compounds. When the SDS concentration is sufficiently low, below the critical micellar concentration in water (8 mM), the retention increase follows a linear pattern. The retention behavior of polar compounds with different properties (nucleosides, methylxanthines, sulfonamides, and the diuretic hydrochlorothiazide) is examined using mobile phases in the submicellar region, with SDS concentrations ranging from 0 to 0.3 mM, acetonitrile contents between 10 and 20% (v/v), and temperatures varying from 25 to 55 °C. Changes in peak half-widths are also analyzed. Since SDS adsorbs onto the stationary phase, modifying its surface, the equilibration time has been investigated as a critical factor affecting retention reproducibility, influenced by the SDS concentration, acetonitrile content, and temperature. The results emphasize the need for complete equilibration to ensure reliable and consistent results. Full article

The unregulated consumption of corticosteroids causes significant adverse effects on human health. Therefore, it is important to develop methodologies that allow their analysis in pharmaceutical matrices with competitive analysis times and costs. The determination of corticosteroids by micellar electrokinetic chromatography (MEKC) using a background electrolyte (BGE) composed of phosphate buffer and a micellar pseudo-stationary phase constituted by a mixture of surfactants is proposed as an alternative quantification technique. The variables involved in the BGE: phosphate concentration, surfactant (sodium dodecyl sulfate (SDS) or sodium lauryl ether sulfate (SLES)), sodium taurocholate (STC) and the pH value were optimized using a Taguchi L₉ (3⁴) experimental design. Employing the optimal BGE, the separation of the three corticosteroids is possible in a linear range of 1.05–10.0 mg L⁻¹, with limits of detection (LOD) of 0.28–0.35 mg L⁻¹. The relative standard deviation (RSD) values obtained for the repeatability (n = 3) and intermediate precision (n = 9) were less than 5.0%. Pharmaceutical formulations (ointments, injectable solution and ophthalmic solution) were analyzed using the proposed methodology (MEKC) and the official methodology (high-performance liquid chromatography, HPLC), and no significant differences were found between the corticosteroid contents obtained from both methods. Full article

Rosa damascena Mill., widely recognized for its remarkable skincare benefits, is extensively used in the cosmeceutical industry. This study introduces a novel green approach to extract bioactive compounds from R. damascena for cosmeceutical applications while also evaluating its stability in terms of physical, chemical, and biological properties. R. damascena petals were extracted using deionized water instead of organic solvents, using various green extraction methods, including infusion, microwave, ultrasound, pulsed electric field, and micellar extraction. Their chemical composition was analyzed using high-performance liquid chromatography. The extract with the highest concentration of bioactive compounds was further evaluated for its cosmeceutical properties and stability and compared with its individual chemical components. Various factors influencing stability were evaluated, including pH level (5, 7, and 9), temperature (4 °C, 30 °C, and 45 °C), and light exposure. The findings indicate that the extract obtained through microwave-assisted extraction (MAE) contained the highest concentration of bioactive constituents, with corilagin being the most abundant, followed by cyanidin-3,5-O-diglucoside, gallic acid, ellagic acid, L-ascorbic acid, and rutin, respectively. Additionally, MAE exhibited excellent antioxidant, whitening, and anti-skin-aging effects, demonstrating significantly higher activities than both the positive control (L-ascorbic acid for antioxidant effects, kojic acid for anti-tyrosinase effects, and epigallocatechin gallate and oleanolic acid for anti-skin-aging effects) and the individual chemical constituents. However, the physico-chemical and biological stability of MAE was influenced by pH, temperature, and light exposure, and as such, light-protected and controlled temperature (not exceeding 30 °C) is essential to maintain the extract’s efficacy in skincare products, and optimal formulation strategies are strongly recommended to ensure long-term stability. Full article

A hybrid method—combining liquid biomimetic chromatography techniques (immobilized artificial membrane chromatography and biopartitioning micellar chromatography) and Quantitative Structure–Activity Relationships—was used to derive helpful models for predicting selected biological properties such as penetration through the plant cuticle, the skin and the blood–brain barrier, and binding to human serum albumin of phenoxyacetic acid-derived congeners regarded as potential herbicides. Reliable, high-concept models were developed indicating the lipophilicity, polarizability, and sum of hydrogen bond donors and acceptors as properties that determine the biological efficacy of the title compounds. These models were validated by leave-one-out cross-validation. Modeling the toxicity of phenoxyacetic acid-derived congeners to red blood cells allowed the identification of the most toxic substances as well as those molecular descriptors that determine their hemolytic properties. Full article

The cosmetics industry is one of the fastest-growing sectors worldwide. The dynamic evolution of this industry results in an increasingly diverse range of products containing various active ingredients. Ensuring the quality of these products is crucial for consumer safety, necessitating the use of advanced analytical methods and adherence to legal regulations. Electrophoretic techniques, particularly capillary electrophoresis and micellar electrokinetic chromatography, facilitate the rapid and precise separation and identification of cosmetic ingredients. A well-chosen technique and optimized analytical conditions ensure high sensitivity, repeatability, and resolution, achieving detection limits that meet legal requirements. Although electromigration techniques are less common in routine laboratory analyses compared to liquid chromatography, they show potential for broader application in analyzing various substances found in cosmetics. This study reviews the possibilities of applying different electrophoretic techniques to analyze selected cosmetic ingredients serving various functions, including preservatives, dyes, exfoliating agents, UV filters, and also contaminants, while considering sample preparation methods, equipment used, and analysis conditions. The compiled data indicate that capillary electrophoresis, when compared to high-performance liquid chromatography and ion chromatography, shows comparable or superior sensitivity and repeatability, with detection limits adequate to meet regulatory standards. Full article

The measurement of selected norepinephrine metabolites, such as 3,4-dihydroxyphenylglycol (DHPG), 3-methoxy-4-hydroxyphenylethylenglycol (MHPG), and vanillylmandelic acid (VMA), in biological matrices—including urine—is of great clinical importance for the diagnosis and monitoring of diseases. This fact has forced researchers to evaluate new analytical methodologies for their isolation and preconcentration from biological samples. In this study, the three most popular extraction techniques—liquid-liquid extraction (LLE), solid-phase extraction (SPE), and a new 3D-printed system for dispersive solid-phase extraction (3D-DSPE)—were investigated. Micellar electrokinetic chromatography (MEKC) with a diode array detector (DAD) at 200 nm wavelength was applied to the separation of analytes, allowing for the assessment of the extraction efficiency (R) and enrichment factor (EF) for the tested extraction types. The separation buffer (BGE) consisted of 5 mM sodium tetraborate decahydrate, 50 mM SDS, 15% (v/v) MeOH, 150 mM boric acid, and 1 mM of 1-hexyl-3-methylimidazolium chloride (the apparent pH of the BGE equaled 7.3). The EF for each extraction procedure was calculated with respect to standard mixtures of the analytes at the same concentration levels. The 3D-DSPE procedure, using DVB sorbent and acetone as the desorption solvent, proved to be the most effective approach for the simultaneous extraction and determination of the chosen compounds, achieving over 3-fold signal amplification for DHPG and MHPG and over 2-fold for VMA. Moreover, all extraction protocols used for the selected norepinephrine metabolites were estimated and discussed. It was also confirmed that the 3D-DSPE-MEKC approach could be considered an effective tool for sample pretreatment and separation of chosen endogenous analytes in urine samples. Full article

Skin aging is an inevitable and intricate process instigated, among others, by oxidative stress. The search for natural sources that inhibit this mechanism is a promising approach to preventing skin aging. The purpose of our study was to evaluate the composition of phenolic compounds in the micellar extract of Phaseolus vulgaris sprouts. The results of a liquid chromatography–mass spectrometry (LC-MS) analysis revealed the presence of thirty-two constituents, including phenolic acids, flavanols, flavan-3-ols, flavanones, isoflavones, and other compounds. Subsequently, the extract was assessed for its antioxidant, anti-inflammatory, anti-collagenase, anti-elastase, anti-tyrosinase, and cytotoxic properties, as well as for the evaluation of collagen synthesis. It was demonstrated that micellar extract from common bean sprouts has strong anti-aging properties. The performed WST-8 (a water-soluble tetrazolium salt) assay revealed that selected concentrations of extract significantly increased proliferation of human dermal fibroblasts compared to the control cells in a dose-dependent manner. A similar tendency was observed with respect to collagen synthesis. Our results suggest that micellar extract from Phaseolus vulgaris sprouts can be considered a promising anti-aging compound for applications in cosmetic formulations. Full article

We investigated the pharmacokinetic pathway of berberine and its metabolites in vitro, in Caco-2 cells, and in human participants following the administration of dihydroberberine (DHB) and micellar berberine (LipoMicel^®, LMB) formulations. A pilot trial involving nine healthy volunteers was conducted over a 24 h period; blood samples were collected and subjected to Ultra High-Performance Liquid Chromatography–High Resolution Mass Spectrometry (UHPLC-HRMS) analyses to quantify the concentrations of berberine and its metabolites. Pharmacokinetic correlations indicated that berberrubine and thalifendine follow distinct metabolic pathways. Additionally, jatrorrhizine sulfate appeared to undergo metabolism differently compared to the other sulfated metabolites. Moreover, berberrubine glucuronide likely has a unique metabolic pathway distinct from other glucuronides. The human trial revealed significantly higher blood concentrations of berberine metabolites in participants of the DHB treatment group compared to the LMB treatment group—except for berberrubine glucuronide, which was only detected in the LMB treatment group. Similarly, results from in vitro investigations showed significant differences in berberine metabolite profiles between DHB and LMB. Dihydroberberine, dihydroxy-berberrubine/thalifendine and jatrorrhizine sulfate were detected in LMB-treated cells, but not in DHB-treated cells; thalifendine and jatrorrhizine-glucuronide were detected in DHB-treated cells only. While DHB treatment provided higher blood concentrations of berberine and most berberine metabolites, both in vitro (Caco-2 cells) and in vivo human studies showed that treatment with LMB resulted in a higher proportion of unmetabolized berberine compared to DHB. These findings suggest potential clinical implications that merit further investigation in future large-scale trials. Full article

Each year, a substantial amount of food is discarded around the globe. A significant portion of this waste consists of by-products derived from Citrus fruits such as lemons. The purpose of this research is to examine the polyphenol extraction and the antioxidant ability of lemon peel using cloud point extraction (CPE), a sustainable approach. CPE was conducted using three steps with a 20% w/v concentration of Span 20 as the surfactant, which has a critical micellar concentration of 6.13 × 10⁻⁵ mol/L. The pH was set at 7 and a salt concentration of 20% was maintained at 45 °C for 20 min. The subsequent outcomes of the analysis were obtained: total polyphenol content (TPC): 526.32 mg gallic acid equivalents per liter; total flavonoid content (TFC): 90.22 mg rutin equivalents per liter; FRAP, DPPH, and hydrogen peroxide assays: 2.40, 2.68 and 1.03 mmol ascorbic acid equivalents per liter, respectively, and 168.63 mg/L ascorbic acid content. The quantification of the polyphenolic compounds through High-Performance Liquid Chromatography showed that the most abundant compounds in the lemon peels are eriocitrin (159.43 mg/L) and hesperidin (135.21 mg/L). The results indicate that the proposed CPE technique is successful in extracting antioxidant compounds from lemon peels. The generated extracts have the potential to be exploited as dietary additives to enhance human health and can also be utilized for nutraceuticals or pharmaceutical purposes. Full article

The regular consumption of citrus fruits by humans has been associated with lower incidence of chronic-degenerative diseases, especially those mediated by free radicals. Most of the health-promoting properties of citrus fruits derive from their antioxidant content of carotenoids and ascorbic acid (ASC). In the current work we have investigated the scavenging (against hydroxyl radical) and quenching capacities (against singlet oxygen) of four different carotenoid extracts of citrus fruits in the presence or absence of ASC (μM range) in organic solvent, aqueous solution, micelles and in an innovative biomimicking liposomal system of animal cell membrane (AML). The fruits of four varieties of citrus were selected for their distinctive carotenoid composition (liquid chromatography characterization): ‘Nadorcott’ mandarin and the sweet oranges ‘Valencia late’, ‘Ruby Valencia’ and ‘Pinalate’ mutant. The quenching activity of citrus carotenoids strongly depended on the biological assemblage: freely diffusible in organic solvent, ‘Ruby Valencia’ carotenoids (containing lycopene) showed the highest quenching activity, whereas ‘Nadorcott’ mandarin extracts, rich in β-cryptoxanthin, prevailed in micellar systems. Interestingly, the addition of 10 μM ASC significantly increased the quenching activity of all citrus extracts in micelles: ‘Valencia’ orange (+53%), ‘Pinalate’ (+87%), ‘Ruby’ (4-fold higher) and ‘Nadorcott’ mandarins (+20%). Accurate C₁₁-BODIPY^581/591 fluorescence assays showed solid scavenging activities of all citrus extracts against AML oxidation: ‘Valencia’ (−61%), ‘Pinalate’ (−58%) and ‘Ruby’ oranges (−29%), and ‘Nadorcott’ mandarins (−70%). Indeed, all four citrus extracts tested here have balanced antioxidant properties; extracts from the ‘Nadorcott’ mandarin slightly prevailed overall, due, at least in part, to its high content of β-cryptoxanthin. This study depicts some of the antioxidant interactions between citrus fruit carotenoids and ascorbic acid in models of animal cell membranes and reinforces the contribution of them in promoting health benefits for humans. Full article

A key factor in the prevention of hair loss is the provision of optimal conditions on the scalp. In this regard, reduction of oxidative stress on the scalp is one critical requirement to support the hair follicles to function optimally. Recently, a novel shampoo formulation technology containing anti-oxidants such as piroctone olamine has been demonstrated to improve hair retention based on micellar degradation and coacervation effects. Caffeine has also been shown to exhibit anti-oxidant activity including the ability to inhibit lipid peroxidation. As with piroctone olamine, it is expected that follicular delivery of caffeine will enhance its anti-oxidant activity in a region that will be beneficial for hair retention. In this study, two shampoo formulations as well as a control formulation were applied to the calf area of n = 9 male participants. The technique of differential tape stripping was applied to obtain the caffeine penetrated to the stratum corneum and to the hair follicles. Isotope-dilution liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was performed to demonstrate caffeine follicular delivery from the shampoo formulas. The results showed that the percentage of caffeine recovered in the hair follicles was 8–9% of the caffeine absorbed into the skin and matched an existing caffeine-based shampoo. In conclusion, a novel shampoo formulation technology has been developed that effectively delivers beneficial anti-oxidants to improve hair retention. This new shampoo is expected to be especially useful in the goal of retaining hair during aging. Full article

Ionic liquids (ILs), such as imidazoles, can be used to prevent the sorption of analytes onto the walls of the capillary. Prior works have confirmed that coating the capillary wall with a cationic layer can increase its surface stability, thereby improving the repeatability of the separation process. In this study, micellar electrokinetic chromatography (MEKC) is employed to evaluate how two ILs with different anions—namely, 1-hexyl-3-methylimidazolium chloride [HMIM⁺Cl⁻] and 1-hexyl-3-methylimidazolium tetrafluoroborate [HMIM⁺BF₄⁻]—affect the separation efficiency for biogenic amines (BAs) such as metanephrine (M), normetanephrine (NM), vanilmandelic acid (VMA), and homovanillic acid (HVA) in urine samples. To this end, solid-phase extraction (SPE) is employed using different sample pH values, with the results demonstrating that HVA and VMA is easily extracted at a sample pH of 5.5, while a sample pH of 9.0 facilitated the extraction of M and NM. In the applied SPE protocol, selected analytes were isolated from urine samples using hydrophilic–lipophilic-balanced (HLB) columns and eluted with methanol (MeOH). The validation data confirmed the method’s linearity (R² > 0.996) for all analytes within the range of 0.25–10 µg/mL. The applicability of the optimized SPE-MEKC-UV method was confirmed by employing it to quantify clinically relevant BAs in real urine samples from pediatric neuroblastoma (NBL) patients. Full article

Micellar microemulsions are thermodynamically stable self-emulsifying systems that have been used to successfully improve the low oral bioavailability of several bioactive phytochemicals, such as antioxidant polyphenols. However, most studies have reported the micellization of single-compounds or purified chemical fractions; thus, the stability, phytochemical-loading efficiency, and bioactivity of complex crude extracts remain largely unexplored. In this study, we evaluated the effects of micellar emulsification of tropical apple (Malus domestica cv. Anna), plum (Prunus domestica cv. Satsuma), and guava (Psidium guajava L.) extracts regarding particle size and stability, polyphenol-loading efficiency, antioxidant capacity, and cytotoxic activity in human and murine cells. Simple food-grade extraction protocols were implemented to obtain apple, plum, and guava extracts. Total polyphenols, flavonoids, and antioxidant activity (DPPH) were determined in the fruit extracts, and their polyphenol profile was further characterized by liquid chromatography (HPLC-DAD). The dried extracts were mixed into a food-grade, self-emulsifying system, and their cytotoxicity in human and murine cell lines was compared. Our research showed that complex fruit matrixes were successfully emulsified into thermodynamically stable polysorbate-based nanometric micelles with uniform size distribution and consistent pH stability, with potential applications in food and biomedical industries. Full article