A stability indicating RP-HPLC-UV assay method for the simultaneous determination of hydroquinone, tretinoin, hydrocortisone, butylated hydroxytoluene and parabens in pharmaceutical creams.

Multicomponent drugs are medications that combine two or more active pharmaceutical ingredients in a single dosage form. These dosage forms improve the patient compliance, reduce the risk of drug interactions, and simplify dosing regimens. However, quality control of these multicomponent dosage forms can be challenging, especially if the final product contains four or more ingredients that are active (comprise stabilizers, preservatives, excipients, and other components). This problem can be more pronounced if the excipients can interfere with the analysis. In this work, a stability indicating assay method was developed and validated (according to the ICH International Guidelines) for the simultaneous determination of hydroquinone (HQ), tretinoin (TRT), hydrocortisone (HCA), butylated hydroxytoluene (BHT), methyl paraben (MP) and propyl paraben (PP) in commercially available pharmaceutical creams. The proposed method is based on gradient elution using X-Bridge C18 (150 × 4.6 mm, 5 µm) column with a flow rate of 1 mL/min. The linear ranges (µg/mL) were 240-560 for HQ, 24-56 for MP, 132-308 for HCA, 6-14 for PP, 12-28 for BHT, 6.6-15 for TRT. During the validation process, the intra- and interday precision and trueness (evaluated as recovery) were found to be below 2.0% and between 100-102%, respectively. System suitability tests (SST) allow validating the herein proposed procedure specifically for pharmaceutical and industrial applications. SST test shows that the reported procedure fulfill with the Guidelines, allowing excellent separation of the analytes with very sensitive, accurate (precise and true) and reproducible quantitation of each analytes. The method was successfully applied in forced degradation studies of the six analytes. Specifically, acid degradation slightly affected HCA and BHT (91% recovery), while alkaline degradation drastically reduced HCA recovery (5.5%) and moderately affected BHT (85%). Photodegradation primarily influenced TRT quantity, and oxidative degradation intensified the BHT peak (130%).

A facile fabric phase sorptive extraction method for monitoring chloramphenicol residues in milk samples.

Determination of pharmaceutical active molecules in the biological matrices is crucial in various fields of clinical and pharmaceutical chemistry, e.g., in pharmacokinetic studies, developing new drugs, or therapeutic drug monitoring. Chloramphenicol (CP) is used for treating bacterial infections, and it's one of the first antibiotics synthetically manufactured on a large scale. Fabric phase sorptive extraction (FPSE) was used to determine Chloramphenicol antibiotic residues in milk samples by means of validated HPLC-DAD instrumentation. Cellulose fabric phases modified with polyethylene glycol-block-polypropylene glycol-block-polyethylene glycol triblock copolymer was synthesized using sol-gel synthesis approach (Sol-gel PEG-PPG-PEG) and used for batch-type fabric phase extractions. Experimental variables of the FPSE method for antibiotic molecules were investigated and optimized systematically. The HPLC analysis of chloramphenicol was performed using a C18 column, isocratic elution of trifluoroacetic acid (0.1%), methanol, and acetonitrile (17:53:30) with a flow rate of 1.0 mL/min. The linear range for the proposed method for chloramphenicol (r2 > 0.9982) was obtained in the range of 25.0-1000.0 ng/mL. The limit of detections (LOD) is 8.3 ng/mL, while RSDs% are below 4.1%. Finally, the developed method based on FPSE-HPLC-DAD was applied to milk samples to quantitatively determine antibiotic residues.

Facile extraction of berberine from different plants, separation, and identification by thin-layer chromatography, high-performance liquid chromatography, and biological evaluation against Leishmaniosis.

The extraction of berberine was carried out from Berberis vulgaris, Berberis aquifolium, and Hydrastis canadensis plants using ethanol and water (70:30, v/v). The extracted berberine was characterized by ultraviolet-visible and Fourier-transform infrared spectroscopy. The purity of berberine was ascertained by thin-layer chromatography using n-propanol-formic acid-water (95:1:4) and (90:1:9) solvents. hRf values were in the range of 44-49 with compact spots (diameter 0.2-0.4 cm). HPLC was carried out using ammonium acetate buffer and acetonitrile in gradient mode with Zodiac (4.6 × 150 mm, 3 µm) column. The flow rate was 1.0 mL/min and detection was at 220 nm. The values of separation and resolution factors of the standard and the extracted berberine were in the range of 1.13-1.16 and 1.40-1.71, respectively. A comparison has shown that both thin-layer chromatography and high-performance liquid chromatography (HPLC) methods found applications in different situations and requirements. The extracted berberine samples were used to treat Leishmaniosis and the results showed better activity of berberine in comparison to the standard drug Amphotericin B. Briefly, the reported research is a novel and may be used to extract berberine from plants, separation and identification of berberine by thin layer chromatography and HPLC and to treat Leishmaniosis.

HPLC-DAD validated method for DM4 and its metabolite S-Me-DM4 quantification in biological matrix for clinical and pharmaceutical applications.

The present study focuses on the development and validation of an HPLC-DAD methodology for the detection of a potent chemotherapeutic agent, Maytansinoid Ravtansine (DM4), and its metabolite, S-methyl-DM4 (S-Me-DM4), in plasma samples. Methodologically, after a simple protein precipitation with acetonitrile and after drying 1 mL of supernatant, the sample (suspended with N,N-Dimethylacetamide, DMA) was directly analyzed by HPLC under isocratic elution using a mobile phase comprising milliQ water and methanol (25:75, v:v), both acidified with 0.1 % v:v formic acid. Employing a flow rate of 1.0 mL/min and a reversed-phase GraceSmart RP18 column thermostated at 40 °C, we achieved complete resolution and separation of DM4 and S-Me-DM4 within 13 min. The optimized injection volume of 20 µL and the wavelength set at 254 nm were utilized for quantitative analyses. Rigorous validation has not only ensured its reliability and reproducibility but has also addressed potential limitations associated with methodological inconsistency. The limit of detection and quantification of the method were 0.025 and 0.06 µg/mL for both the analytes, respectively. The calibration curve showed a good linearity in the range 0.06-20 µg/mL. For both analytes, the intraday precision and trueness were 2.3-8.2 % and -1.1 to 3.1 %, respectively, while the interday values were 0.7-10.1 % and -10.4 to 7.5 %, respectively. The developed methodology enables the concurrent determination and quantification of free DM4 and its metabolite, free S-Me-DM4, making it a valuable tool for assessing the pharmacokinetics and pharmacodynamics of DM4-based therapies. In addition, the procedure was successfully applied to analyse the presence of free DM4 or its metabolite, free S-Me-DM4, in human plasma samples spiked with the 1959-sss/DM4 antibody-drug conjugate (ADC). The utilization of the herein validated methodology allowed to confirm the presence of these analytes, thereby providing insights into their potential release from the ADC structure.

Endurance-dependent urinary extracellular vesicle signature: shape, metabolic miRNAs, and purine content distinguish triathletes from inactive people.

Extracellular vesicles (EVs) enriched with bioactive molecules have gained considerable attention in nanotechnology because they are critical to intercellular communication while maintaining low immunological impact. Among biological matrices, urine has emerged as a noninvasive source of extracellular-contained liquid biopsy, currently of interest as a readout for physiological adaptations. Therefore, we aimed to evaluate chronic adaptations of endurance sport practice in terms of urinary EV parameters and evaluated by food consumption assessment. Two balanced groups of 13 inactive controls vs. triathlon athletes were enrolled; their urinary EVs were obtained by differential ultracentrifugation and analyzed by dynamic light scattering and transmission electron and atomic force microscopy. The cargo was analyzed by means of purine and miRNA content through HPLC-UV and qRT-PCR. Specific urinary EV signatures differentiated inactive versus endurance-trained in terms of peculiar shape. Particularly, a spheroid shape, smaller size, and lower roughness characterize EVs from triathletes. Metabolic and regulatory miRNAs often associated with skeletal muscle (i.e., miR378a-5p, miR27a-3p, miR133a, and miR206) also accounted for a differential signature. These miRNAs and guanosine in urinary EVs can be used as a readout for metabolic status along with the shape and roughness of EVs, novel informative parameters that are rarely considered. The network models allow scholars to entangle nutritional and exercise factors related to EVs' miRNA and purine content to depict metabolic signatures. All in all, multiplex biophysical and molecular analyses of urinary EVs may serve as promising prospects for research in exercise physiology.

Advances in Polymeric Colloids for Cancer Treatment.

Polymer colloids have remarkable features and are gaining importance in many areas of research including medicinal science. Presently, the innovation of cancer drugs is at the top in the world. Polymer colloids have been used as drug delivery and diagnosis agents in cancer treatment. The polymer colloids may be of different types such as micelles, liposomes, emulsions, cationic carriers, and hydrogels. The current article describes the state-of-the-art polymer colloids for the treatment of cancer. The contents of this article are about the role of polymeric nanomaterials with special emphasis on the different types of colloidal materials and their applications in targeted cancer therapy including cancer diagnoses. In addition, attempts are made to discuss future perspectives. This article will be useful for academics, researchers, and regulatory authorities.

A comprehensive phytochemical, biological, and toxicological studies of roots and aerial parts of Crotalaria burhia Buch.-Ham: An important medicinal plant.

This study was designed to seek the phytochemical analysis, antioxidant, enzyme inhibition, and toxicity potentials of methanol and dichloromethane (DCM) extracts of aerial and root parts of Crotalaria burhia. Total bioactive content, high-performance liquid chromatography-photodiode array detector (HPLC-PDA) polyphenolic quantification, and ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) analysis were utilized to evaluate the phytochemical composition. Antioxidant [including 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH)], 2,2'-azino-bis[3-ethylbenzothiazoline-6-sulfonic acid (ABTS), ferric reducing antioxidant power assay (FRAP), cupric reducing antioxidant capacity CUPRAC, phosphomolybdenum, and metal chelation assays] and enzyme inhibition [against acetylcholinesterase (AChE), butyrylcholinesterase (BChE), α-glucosidase, α-amylase, and tyrosinase] assays were carried out for biological evaluation. The cytotoxicity was tested against MCF-7 and MDA-MB-231 breast cell lines. The root-methanol extract contained the highest levels of phenolics (37.69 mg gallic acid equivalent/g extract) and flavonoids (83.0 mg quercetin equivalent/g extract) contents, and was also the most active for DPPH (50.04 mg Trolox equivalent/g extract) and CUPRAC (139.96 mg Trolox equivalent /g extract) antioxidant assays. Likewise, the aerial-methanol extract exhibited maximum activity for ABTS (94.05 mg Trolox equivalent/g extract) and FRAP (64.23 mg Trolox equivalent/g extract) assays. The aerial-DCM extract was noted to be a convincing cholinesterase (AChE; 4.01 and BChE; 4.28 mg galantamine equivalent/g extract), and α-glucosidase inhibitor (1.92 mmol acarbose equivalent/g extract). All of the extracts exhibited weak to modest toxicity against the tested cell lines. A considerable quantities of gallic acid, catechin, 4-OH benzoic acid, syringic acid, vanillic acid, 3-OH-4-MeO benzaldehyde, epicatechin, p-coumaric acid, rutin, naringenin, and carvacrol were quantified via HPLC-PDA analysis. UHPLC-MS analysis of methanolic extracts from roots and aerial parts revealed the tentative identification of important phytoconstituents such as polyphenols, saponins, flavonoids, and glycoside derivatives. To conclude, this plant could be considered a promising source of origin for bioactive compounds with several therapeutic uses.

Multifaced Assessment of Antioxidant Power, Phytochemical Metabolomics, In-Vitro Biological Potential and In-Silico Studies of Neurada procumbens L.: An Important Medicinal Plant.

This work was undertaken to explore the phytochemical composition, antioxidant, and enzyme-inhibiting properties of Neurada procumbens L. extracts/fractions of varying polarity (methanol extract and its fractions including n-hexane, chloroform, n-butanol, and aqueous fractions). A preliminary phytochemical study of all extracts/fractions, HPLC-PDA polyphenolic quantification, and GC-MS analysis of the n-hexane fraction were used to identify the phytochemical makeup. Antioxidant (DPPH), enzyme inhibition (against xanthine oxidase, carbonic anhydrase, and urease enzymes), and antibacterial activities against seven bacterial strains were performed for biological investigation. The GC-MS analysis revealed the tentative identification of 22 distinct phytochemicals in the n-hexane fraction, the majority of which belonged to the phenol, flavonoid, sesquiterpenoid, terpene, fatty acid, sterol, and triterpenoid classes of secondary metabolites. HPLC-PDA analysis quantified syringic acid, 3-OH benzoic acid, t-ferullic acid, naringin, and epicatechin in a significant amount. All of the studied extracts/fractions displayed significant antioxidant capability, with methanol extract exhibiting the highest radical-scavenging activity, as measured by an inhibitory percentage of 81.4 ± 0.7 and an IC50 value of 1.3 ± 0.3. For enzyme inhibition experiments, the n-hexane fraction was shown to be highly potent against xanthine oxidase and urease enzymes, with respective IC50 values of 2.3 ± 0.5 and 1.1 ± 0.4 mg/mL. Similarly, the methanol extract demonstrated the strongest activity against the carbonic anhydrase enzyme, with an IC50 value of 2.2 ± 0.4 mg/mL. Moreover, all the studied extracts/fractions presented moderate antibacterial potential against seven bacterial strains. Molecular docking of the five molecules ß-amyrin, campesterol, ergosta-4,6,22-trien-3ß-ol, stigmasterol, and caryophyllene revealed the interaction of these ligands with the investigated enzyme (xanthine oxidase). The results of the present study suggested that the N. procumbens plant may be evaluated as a possible source of bioactive compounds with multifunctional therapeutic applications.

Investigation of phytochemical composition and enzyme inhibitory potential of Anagallis arvensis L.

Anagallis arvensis L. commonly known as 'Scarlet Pimpernel' has been used in folklore as natural remedy for treating common ailments. The present research is aimed to explore the phytochemical composition and enzyme inhibition potential of methanol and dichloromethane (DCM) extracts of A. arvensis aerial and root parts. The phytochemical composition was established via HPLC-PDA polyphenolic quantification and UHPLC-MS analysis, while the inhibition potential against amylase and tyrosinase enzymes were assessed using standard in vitro protocols. The HPLC-PDA polyphenolic quantification revealed the presence of important compounds including catechin, gallic acid, chlorogenic acid, and ferulic acid, whereas 34 different secondary metabolites were tentatively identified by UHPLC-MS of both the DCM extracts. All the extracts showed moderate tyrosinase and a weak amylase inhibition activity. The aerial-DCM extract showed comparatively higher tyrosinase and amylase enzyme inhibition potential, which may be due to the presence of secondary metabolites as tentatively identified by its UHPLC-MS profiling.

Phytopharmacological Evaluation of Different Solvent Extract/Fractions From Sphaeranthus indicus L. Flowers: From Traditional Therapies to Bioactive Compounds.

Sphaeranthus indicus L. is a medicinal herb having widespread traditional uses for treating common ailments. The present research work aims to explore the in-depth phytochemical composition and in vitro reactivity of six different polarity solvents (methanol, n-hexane, benzene, chloroform, ethyl acetate, and n-butanol) extracts/fractions of S. indicus flowers. The phytochemical composition was accomplished by determining total bioactive contents, HPLC-PDA polyphenolic quantification, and UHPLC-MS secondary metabolomics. The reactivity of the phenolic compounds was tested through the following biochemical assays: antioxidant (DPPH, ABTS, FRAP, CUPRAC, phosphomolybdenum, and metal chelation) and enzyme inhibition (AChE, BChE, α-glucosidase, α-amylase, urease, and tyrosinase) assays were performed. The methanol extract showed the highest values for phenolic (94.07 mg GAE/g extract) and flavonoid (78.7 mg QE/g extract) contents and was also the most active for α-glucosidase inhibition as well as radical scavenging and reducing power potential. HPLC-PDA analysis quantified rutin, naringenin, chlorogenic acid, 3-hydroxybenzoic acid, gallic acid, and epicatechin in a significant amount. UHPLC-MS analysis of methanol and ethyl acetate extracts revealed the presence of well-known phytocompounds; most of these were phenolic, flavonoid, and glycoside derivatives. The ethyl acetate fraction exhibited the highest inhibition against tyrosinase and urease, while the n-hexane fraction was most active for α-amylase. Moreover, principal component analysis highlighted the positive correlation between bioactive compounds and the tested extracts. Overall, S. indicus flower extracts were found to contain important phytochemicals, hence could be further explored to discover novel bioactive compounds that could be a valid starting point for future pharmaceutical and nutraceuticals applications.

Investigation into the biological properties, secondary metabolites composition, and toxicity of aerial and root parts of Capparis spinosa L.: An important medicinal food plant.

Capparis spinose L. also known as Caper is of great significance as a traditional medicinal food plant. The present work was targeted on the determination of chemical composition, pharmacological properties, and in-vitro toxicity of methanol and dichloromethane (DCM) extracts of different parts of C. spinosa. Chemical composition was established by determining total bioactive contents and via UHPLC-MS secondary metabolites profiling. For determination of biological activities, antioxidant capacity was determined through DPPH, ABTS, CUPRAC, FRAP, phosphomolybdenum, and metal chelating assays while enzyme inhibition against cholinesterase, tyrosinase, α-amylase and α-glucosidase were also tested. All the extracts were also tested for toxicity against two breast cell lines. The methanolic extracts were found to contain highest total phenolic and flavonoids which is correlated with their significant radical scavenging, cholinesterase, tyrosinase and glucosidase inhibition potential. Whereas DCM extracts showed significant activity for reducing power, phosphomolybdenum, metal chelation, tyrosinase, and α-amylase inhibition activities. The secondary metabolites profiling of both methanolic extracts exposed the presence of 21 different secondary metabolites belonging to glucosinolate, alkaloid, flavonoid, phenol, triterpene, and alkaloid derivatives. The present results tend to validate folklore uses of C. spinose and indicate this plant to be used as a potent source of designing novel bioactive compounds.

Development of sol-gel phenyl/methyl/poly (dimethylsiloxane) sorbent coating for fabric phase sorptive extraction and its application in monitoring human exposure to selected polycyclic aromatic hydrocarbons using high performance liquid chromatography-fluorescence detection.

Following the convenient, yet very powerful pathway to create designer extraction sorbent using sol-gel chemistry, a novel sol-gel phenyl/methyl/poly(dimethylsiloxane) sorbent coating was created on polyester fabric substrate for fabric phase sorptive extraction (FPSE) and was subsequently applied to monitor human exposure to selected polycyclic aromatic hydrocarbons (PAHs) including pyrene, chrysene, and benzo[a]pyrene in plasma samples obtained from tobacco smoker volunteers using high performance liquid chromatography-fluorescence detector (HPLC-FLD). A rapid FPSE-HPLC-FLD method was developed that adequately resolved the PAHs chromatographically, after their successful extraction from human plasma using fabric phase absorption extraction (FPSE) and subsequently analysed in the liquid chromatographic system by means of an analytical column (InterSustain C-18 column 150 × 4.6 mm, 5 µm) using acetonitrile (ACN) and water as mobile phases in gradient elution mode. With the optimized conditions, the retention times were found to be 6.168, 7.214, and 10.404 min for pyrene, chrysene, and benzo[a]pyrene, respectively. The total chromatographic runtime was limited to 12.5 min. The method, validated through the calculation of all the analytical parameters according to the International Guidelines, was applied to the analysis of real samples collected from informed volunteers. The proposed approach which included the use of sol-gel phenyl/methyl/poly(dimethylsiloxane) immobilized on hydrophobic polyester substrate and C18 stationary phase used in HPLC, has shown a high potential as a rapid tool for future clinical, forensic and toxicological applications, also in the light of the LOD and LOQ values comparable to those normally obtainable with more sophisticated, and expensive instruments that often require highly trained personnel. The results reported here further consolidate the application of FPSE in the analysis of biological samples for both diagnostic and analytical-clinical purposes.

Synthesis and Biological Evaluation of Halogenated E-Stilbenols as Promising Antiaging Agents.

The increased risk of illness and disability is related to the age inevitable biological changes. Oxidative stress is a proposed mechanism for many age-related diseases. The crucial importance of polyphenol pharmacophore for aging process is largely described thanks to its effects on concentrations of reactive oxygen species. Resveratrol (3,5,4'-trihydroxy-trans-stilbene, RSV) plays a critical role in slowing the aging process but has a poor bioavailabity after oral intake. In this present work, a series of RSV derivatives was designed, synthesized, and evaluated as potential antioxidant agents. These derivatives contain substituents with different electronic and steric properties in different positions of aromatic rings. This kind of substituents affects the activity and the bioavailability of these compounds compared with RSV used as reference compound. Studies of Log P values demonstrated that the introduction of halogens gives the optimum lipophilicity to be considered promising active agents. Among them, compound 6 showed the higher antioxidant activity than RSV. The presence of trifluoromethyl group together with a chlorine atom increased the antioxidant activity compared to RSV.

Metabolic fingerprinting, antioxidant characterization, and enzyme-inhibitory response of Monotheca buxifolia (Falc.) A. DC. extracts.

BACKGROUND: Ethnobotanical and plant-based products allow for the isolation of active constituents against a number of maladies. Monotheca buxifolia is used by local communities due to its digestive and laxative properties, as well as its ability to cure liver, kidney, and urinary diseases. There is a need to explore the biological activities and chemical constituents of this medicinal plant. METHODS: In this work, the biochemical potential of M. buxifolia (Falc.) A. DC was explored and linked with its biological activities. Methanol and chloroform extracts from leaves and stems were investigated for total phenolic and flavonoid contents. Ultrahigh-performance liquid chromatography coupled with mass spectrometry (UHPLC-MS) was used to determine secondary-metabolite composition, while high-performance liquid chromatography coupled with photodiode array detection (HPLC-PDA) was used for polyphenolic quantification. In addition, we carried out in vitro assays to determine antioxidant potential and the enzyme-inhibitory response of M. buxifolia extracts. RESULTS: Phenolics (91 mg gallic-acid equivalent (GAE)/g) and flavonoids (48.86 mg quercetin equivalent (QE)/g) exhibited their highest concentration in the methanol extract of stems and the chloroform extract of leaves, respectively. UHPLC-MS analysis identified a number of important phytochemicals, belonging to the flavonoid, phenolic, alkaloid, and terpenoid classes of secondary metabolites. The methanol extract of leaves contained a diosgenin derivative and polygalacin D, while kaempferol and robinin were most abundant in the chloroform extract. The methanol extract of stems contained a greater peak area for diosgenin and kaempferol, whereas this was true for lucidumol A and 3-O-cis-coumaroyl maslinic acid in the chloroform extract. Rutin, epicatechin, and catechin were the main phenolics identified by HPLC-PDA analysis. The methanol extract of stems exhibited significant 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS) radical-scavenging activities (145.18 and 279.04 mmol Trolox equivalent (TE)/g, respectively). The maximum cupric reducing antioxidant capacity (CUPRAC) (361.4 mg TE/g), ferric-reducing antioxidant power (FRAP) (247.19 mg TE/g), and total antioxidant potential (2.75 mmol TE/g) were depicted by the methanol extract of stems. The methanol extract of leaves exhibited stronger inhibition against acetylcholinesterase (AChE) and glucosidase, while the chloroform extract of stems was most active against butyrylcholinesterase (BChE) (4.27 mg galantamine equivalent (GALAE)/g). Similarly, the highest tyrosinase (140 mg kojic-acid equivalent (KAE)/g) and amylase (0.67 mmol acarbose equivalent (ACAE)/g) inhibition was observed for the methanol extract of stems. CONCLUSIONS: UHPLC-MS analysis and HPLC-PDA quantification identified a number of bioactive secondary metabolites of M. buxifolia, which may be responsible for its antioxidant potential and enzyme-inhibitory response. M. buxifolia can be further explored for the isolation of its active components to be used as a drug.

Liposome-Embedding Silicon Microparticle for Oxaliplatin Delivery in Tumor Chemotherapy.

Mesoporous silicon microparticles (MSMPs) can incorporate drug-carrying nanoparticles (NPs) into their pores. An NP-loaded MSMP is a multistage vector (MSV) that forms a Matryoshka-like structure that protects the therapeutic cargo from degradation and prevents its dilution in the circulation during delivery to tumor cells. We developed an MSV constituted by 1 µm discoidal MSMPs embedded with PEGylated liposomes containing oxaliplatin (oxa) which is a therapeutic agent for colorectal cancer (CRC). To obtain extra-small liposomes able to fit the 60 nm pores of MSMP, we tested several liposomal formulations, and identified two optimal compositions, with a prevalence of the rigid lipid 1,2-distearoyl-sn-glycero-3-phosphocholine and of 1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-[methoxy(polyethylene glycol)-2000]. To improve the MSV assembly, we optimized the liposome-loading inside the MSMP and achieved a five-fold increase of the payload using an innovative lyophilization approach. This procedure also increased the load and limited dimensional changes of the liposomes released from the MSV in vitro. Lastly, we found that the cytotoxic efficacy of oxa-loaded liposomes and-oxa-liposome-MSV in CRC cell culture was similar to that of free oxa. This study increases knowledge about extra-small liposomes and their loading into porous materials and provides useful hints about alternative strategies for designing drug-encapsulating NPs.

Metabolic profiling of different wild and cultivated Allium species based on high-resolution mass spectrometry, high-performance liquid chromatography-photodiode array detector, and color analysis.

Many plants of the genus Allium are widely cultivated and consumed for their nutraceutical and health-enhancing bioactive components effective in many metabolic and infectious diseases. In particular, Allium sativum L. (garlic), the most economically important Allium species, is known to present volatile, comparatively polar sulfur-containing compounds responsible for both the typical garlic aroma and antimicrobial property. More recently, the (moderately) polar portion of garlic metabolome, rich of polyphenols and amino acids, is gaining increasing interest as a source of antioxidants and primary nutrients. In this study, we have explored the chemical diversity of eight different hydroalcoholic extracts obtained by microwave-assisted extraction of white and red crop A. sativum and wild Allium triquetrum, Allium roseum, and Allium ampeloprasum, all originating from the Mediterranean Basin. The aim is to appraise their potential dietetic and healing value through an in-depth chemical characterization and contribute to preserve and exploit natural resources. The multimethodological method applied here is based on an untargeted metabolic profiling by means of high-resolution electrospray ionization Fourier-transform ion cyclotron resonance (ESI FT-ICR) mass spectrometry. More than 850 by ESI(+) and 450 by ESI(-) putative metabolites have been annotated covering all main classes of primary and secondary metabolites, including amino acids, alkaloids, organic and fatty acids, nucleotides, vitamins, organosulfur compounds, and flavonoids. The pigment and polyphenol components have been separated and quantified by a targeted chromatographic high-performance liquid chromatography-photodiode array detector (HPLC-PDA) and CIEL*a*b* colorimetric assay, showing characteristic yellow and red components in each extract, related to a different milieu of anthocyanins and flavonoids as assigned by high-resolution mass spectrometry (MS).

HPLC-PDA Polyphenolic Quantification, UHPLC-MS Secondary Metabolite Composition, and In Vitro Enzyme Inhibition Potential of Bougainvillea glabra.

The plants of the Bougainvillea genus are widely explored regarding nutritive and medicinal purposes. In this study, dichloromethane (DCM) and methanol (MeOH) extracts of Bougainvillea glabra (Choisy.) aerial and flower parts were analyzed for high-performance liquid chromatography with photodiode array detection (HPLC-PDA), ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS) phytochemical composition, and enzyme inhibition potential against key enzymes involved in diabetes (α-amylase), skin problems (tyrosinase), and inflammatory disorders (lipoxygenase (LOX)). HPLC-PDA quantification revealed the identification of nine different polyphenolics, amongst which both flower extracts were richest. The flower MeOH extract contained the highest amount of catechin (6.31 µg/g), gallic acid (2.39 µg/g), and rutin (1.26 µg/g). However, none of the quantified compounds were detected in the aerial DCM extract. UHPLC-MS analysis of DCM extracts revealed the tentative identification of 27 secondary metabolites, where the most common belonged to terpenoid, alkaloid, and phenolic derivatives. Similarly, for enzyme inhibition, all the extracts presented moderate activity against tyrosinase and α-amylases, whereas, for LOX, both methanolic extracts showed higher percentage inhibition compared with DCM extracts. Based on our findings, B. glabra could be regarded as a perspective starting material for designing novel pharmaceuticals.

Phytochemical analysis and reappraisal of diuretic activity of Delphinium brunonianum Royle and its mode of action in experimental rats.

The aim of this study was the evaluation of diuretic potential of Delphinium brunonianum. Acute diuretic effect in rats was evaluated 8 h after administration of various doses of crude extract, fractions and hydrochlorthiazide. While, prolonged effect of butanolic fraction was assessed after 7days of oral administration in rats. Thereafter, involvement of different pathways in diuretic activity was also appraised. Furthermore, polyphenolic contents in butanolic fraction were assessed using HPLC/UV-VIS technique. All doses of extract and fractions induced a prominent increase in urine and Na+ excretion with no effect on excretion of K+. Prior administration of indomethacin and atropine considerably avoided the diuretic effect of butanolic fraction. Regarding the quantitative chemical analysis the polyphenolic contents were recorded as 28.78 µg/mg. Thus results of present investigation suggested that Delphinium brunonianum possess remarkable diuretic potential.

Polyphenols from Lycium barbarum (Goji) Fruit European Cultivars at Different Maturation Steps: Extraction, HPLC-DAD Analyses, and Biological Evaluation.

Goji berries are undoubtedly a source of potentially bioactive compounds but their phytochemical profile can vary depending on their geographical origin, cultivar, and/or industrial processing. A rapid and cheap extraction of the polyphenolic fraction from Lycium barbarum cultivars, applied after homogenization treatments, was combined with high-performance liquid chromatography (HPLC) analyses based on two different methods. The obtained hydroalcoholic extracts, containing interesting secondary metabolites (gallic acid, chlorogenic acid, catechin, sinapinic acid, rutin, and carvacrol), were also submitted to a wide biological screening. The total phenolic and flavonoid contents, the antioxidant capacity using three antioxidant assays, tyrosinase inhibition, and anti-Candida activity were evaluated in order to correlate the impact of the homogenization treatment, geographical origin, and cultivar type on the polyphenolic and flavonoid amount, and consequently the bioactivity. The rutin amount, considered as a quality marker for goji berries according to European Pharmacopeia, varied from ≈200 to ≈400 µg/g among the tested samples, showing important differences observed in relation to the influence of the evaluated parameters.

Hypoglycemic, Antiglycation, and Cytoprotective Properties of a Phenol-Rich Extract From Waste Peel of Punica granatum L. var. Dente di Cavallo DC2.

Pomegranate peel is a natural source of phenolics, claimed to possess healing properties, among which are antioxidant and antidiabetic. In the present study, an ethyl acetate extract, obtained by Soxhlet from the peel of Dente di Cavallo DC2 pomegranate (PGE) and characterized to contain 4% w/w of ellagic acid, has been evaluated for its hypoglycemic, antiglycation, and antioxidative cytoprotective properties, in order to provide possible evidence for future nutraceutical applications. The α-amylase and α-glucosidase enzyme inhibition, interference with advanced glycation end-products (AGE) formation, and metal chelating abilities were studied. Moreover, the possible antioxidant cytoprotective properties of PGE under hyperglycemic conditions were assayed. Phenolic profile of the extract was characterized by integrated chromatographic and spectrophotometric methods. PGE resulted able to strongly inhibit the tested enzymes, especially α-glucosidase, and exerted chelating and antiglycation properties. Also, it counteracted the intracellular oxidative stress under hyperglycemic conditions, by reducing the levels of reactive oxygen species and total glutathione. Among the identified phenolics, rutin was the most abundant flavonoid (about 4 % w/w). Present results suggest PGE to be a possible remedy for hyperglycemia management and encourage further studies to exploit its promising properties.