Pomegranate Wastes Are Rich in Bioactive Compounds with Potential Benefit on Human Health

Pomegranate use is increasing worldwide, as it is considered a tasteful healthy food. It is mainly used as fruit, juice, and jam. The pomegranate peel represents about 40–50% of the total fruit weight and contains numerous and diverse bioactive substances. The aim of this research was to analyze the pomegranate peel chemical composition of Wonderful cultivated in Southern Italy and treated with an innovative physic dry concentration procedure in comparison with the peel composition of freeze-dried Wonderful cultivated in Southern Italy, freeze-dried Wonderful cultivated in South Africa, and freeze-dried pomegranate cultivated in India. The specific aim was to verify how much the growth area, cultivar type, and dry procedure influenced the chemical composition of the peels in terms of valuable bioactive compounds. Spectrophotometric and HPLC identification methods were used to detect antioxidants, antioxidant activities, and phenolic and flavonoid components. Results evidenced that in pomegranate peels of Wonderful cultivated in Calabria and dried with the innovative process, total phenolic substances, total flavonoids, vitamin C, vitamin E, and antioxidant activities were the highest. Great amounts of single phenolic acids and flavonoids were found in Calabrian Wonderful peels dried with the innovative process. Overall, it emerged that a great amount of bioactive and diverse compounds found in Calabrian Wonderful pomegranate peel comes from the niche pedoclimatic conditions, and the physic drying innovative methodology turned out to be an advantageous procedure to concentrate and conserve biocompounds.     

NMR Investigation of the Interaction of Three Non-Steroidal Anti-Inflammatory Drugs with Human Serum Albumin

The understanding of the interaction between non-steroidal anti-inflammatory drugs and human serum albumin plays a fundamental role in the development of new drugs and new therapeutic strategies. Several studies have been performed, nevertheless, the interaction phenomena are still not fully understood. In this work, high-field solution Nuclear Magnetic Resonance (NMR) spectroscopy was applied to compare the strength of the interaction of diclofenac sodium salt, ketorolac tris salt and flurbiprofen sodium salt toward albumin. To this aim, mono- and bi-selective relaxation rate measurements were performed by applying selective π-pulses at the selected frequencies and by following magnetization recovery. On the basis of the dependence of relaxation parameters on albumin concentration, normalized affinity indexes were calculated for several protons of the drugs. Affinity indexes for diclofenac were about five-fold higher in comparison with ketorolac and flurbiprofen. Aromatic moieties of the three drugs and methine protons at the chiral centers of ketorolac and flurbiprofen were more involved in the interaction with albumin. In conclusion, NMR spectroscopy allows not only for the comparison of drug-to-protein affinities but also points out the nature of the drug sites that are more extensively involved in the interaction.     

Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS

In this work, a simple, quick and efficient analytical method for determination of human and veterinary fluoroquinolone antimicrobial residues in lettuce, cucumber and spinach is developed. The procedure entails a 6 min ultrasound-assisted extraction (UAE, 3 × 2 min) in an alkaline (2% v/v NH₃) aqueous solution containing Mg²⁺ ions (3 × 6 mL), with no need for organic solvents. The extract is submitted to cleanup on the HLB™ cartridge and the fluoroquinolones are separated and quantified by HPLC-MS/MS in a 10 min chromatographic run, using a small amount of acetonitrile in the mobile phase. The method, entirely developed in real matrices, is validated according to the updated analytical guidelines and provided suitable recoveries in the range of 67–116% and precision (RSD ≤ 20%, n = 3) at different concentrations (15, 70 and 150 ng g⁻¹), with method quantification limits of 2–10 ng g⁻¹. Fluoroquinolones were detected and quantified at concentrations from few to hundreds of nanograms per gram in vegetables from supermarkets, demonstrating the applicability of the method for monitoring residues of these pharmaceuticals.     

Fast and Sensitive Analysis of Short- and Long-Chain Perfluoroalkyl Substances in Foods of Animal Origin

The availability of sensitive analytical methods to detect per- and polyfluoroalkyl substances (PFASs) in food of animal origin is fundamental for monitoring programs to collect data useful for improving risk assessment strategies. The present study aimed to develop and validate a fast and sensitive method for determining short and long-chain PFASs in meat (bovine, fish, and swine muscle), bovine liver, hen eggs, and cow’s milk to be easily applicable in routine analysis of food. A QuEChERS extraction and clean-up method in combination with liquid chromatography coupled to mass spectrometry (LC-MSMS) were used. The method resulted in good linearity (Pearson’s R > 0.99), low limits of detection (7.78–16.35 ng/kg, 8.26–34.01 ng/kg, 6.70–33.65 ng/kg, and 5.92–19.07 ng/kg for milk, liver, egg, and muscle, respectively), and appropriate limits of quantification (50 ng/kg for all compounds except for GenX and C6O4, where the limits of quantification were 100 ng/kg). Trueness and precision for all the tested levels met the acceptability criteria of 80–120% and ≤20%, respectively, regardless of the analyzed matrix. As to measurement uncertainty, it was <50% for all compound/matrix combinations. These results demonstrate the selectivity and sensitivity of the method for simultaneous trace detection and quantification of 14 PFASs in foods of animal origin, verified through the analysis of 63 food samples.     

An Efficient Solid-Phase Microextraction–Gas Chromatography–Mass Spectrometry Method for the Analysis of Methyl Farnesoate Released in Growth Medium by Daphnia pulex

Methyl farnesoate (MF), a juvenile hormone, can influence phenotypic traits and stimulates male production in daphnids. MF is produced endogenously in response to stressful conditions, but it is not known whether this hormone can also be released into the environment to mediate stress signaling. In the present study, for the first time, a reliable solid-phase microextraction–gas chromatography–mass spectrometry (SPME-GC-MS) method was developed and validated for the ultra-trace analysis of MF released in growth medium by Daphnia pulex maintained in presence of crowding w/o MK801, a putative upstream inhibitor of MF endogenous production. Two different clonal lineages, I and S clones, which differ in the sensitivity to the stimuli leading to male production, were also compared. A detection limit of 1.3 ng/L was achieved, along with good precision and trueness, thus enabling the quantitation of MF at ultra-trace level. The achieved results demonstrated the release of MF by both clones at the 20 ng/L level in control conditions, whereas a significant decrease in the presence of crowding was assessed. As expected, a further reduction was obtained in the presence of MK801. These findings strengthen the link between environmental stimuli and the MF signaling pathway. Daphnia pulex, by releasing the juvenile hormone MF in the medium, could regulate population dynamics by means of an autoregulatory feedback loop that controls the intra- and extra-individual-level release of MF produced by endogenous biosynthesis.     

Synthesis of a Series of Hydroxycarboxylic Acids as Standards for Oxidation of Nonanoic Acid

The synthesis of a series of nonanoic acids hydroxylated in terminal,ω-1,ω-2,ω-3 positions is described. These compounds will be employed as useful standards for the study of enzymatic and microbiological oxidation of nonanoic acid.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.]     

On the self-condensation of aminoguanidine leading to 1,1,4,10,10-pentaamino-2,3,5,6,8,9-hexaazadeca-1,3,5,7,9-pentaene (structure elucidation through X-ray powder diffraction)

Chemical and spectroscopic (UV; ¹H, ¹³C, ¹⁵N NMR; HRMS) studies determined the structure of 1,1,4,10,10-pentaamino-2,3,5,6,8,9-hexaazadeca-1,3,5,7,9-pentaene for the red-violet compound, which was obtained by treating aminoguanidine hydrochloride with KOH. X-ray powder diffraction and lattice-constrained PBC-DFT optimization confirmed this structure and defined a linear all-trans configuration.