Effects of γ-irradiation on the lipid composition of inner sprout of garlic

The aim of this work was to evaluate the effects of a dose of 60.0 Gy of ⁶⁰Co γ-rays on the concentration and composition of lipids from the inner sprout of garlic cloves. 210 days after treatment, the levels of phospholipids, triacylglycerols and glycolipids were significantly reduced as a result of radiation. Levels of polyunsaturated fatty acids from these lipid fractions such as linoleic acids showed a similar trend of decrease. Irradiation also brought about an increase in diacylglycerols. Results are correlated with sprouting inhibition induced by γ-irradiation in garlic.     

In vitro evaluation of the amoebicidal activity of rosemary (Rosmarinus officinalis L.) and cloves (Syzygium aromaticum L. Merr. & Perry) essential oils against Acanthamoeba polyphaga trophozoites

Several species of the genus Acanthamoeba cause human diseases. Treatment of infections involves various problems, emphasising the need to develop alternative antiprotozoal agents. We studied the anti-amoebic activity of Essential Oils (EOs), derived from rosemary (Rosmarinus officinalis L.) and cloves (Syzygium aromaticum L. Merr. & Perry), against Acanthamoeba polyphaga strain. The amoebicidal activity of cloves and rosemary EOs was preliminary demonstrated by the morphology change (modifications in the cell shape, the presence of precipitates in the cytoplasm, autophagic vesicles, membrane blends) of the treated trophozoites. The cell-counts, carried out after staining trophozoites with a Trypan blue solution, revealed that both EOs were active in a dose-dependent manner and in relation to the exposure time. This activity was evident after few hours, with encouraging results obtained in particular with cloves EO, able to act at the lower concentrations and after 1 h, probably for its high eugenol content (65.30%).     

Optimizing stirred cell membrane emulsification process for making a food-grade multiple emulsion

The stirred cell membrane emulsification process that was used to produce a food-grade multiple emulsion was optimized. The produced water-in-oil-in-water emulsion contained garlic ethanol extract water solution-in-pumpkin seed and sunflower oil mixture (1:1 w/w)-in-glucose water solution. A sintered glass filter-disk membrane was employed in the stirred cell device. The transmembrane pressure and the impeller rotational speed values were varied in a range from 0.2 to 1 10⁵ Pa, and in a range from 140 to 1400 rpm, respectively. For the investigated ranges of the process parameters, the primary emulsion flux through the membrane was in a range from 26 to 366 Lm^?2 h^?1, and the obtained values of the Sauter mean diameter of oil droplets and the span of droplet size distribution was in a range from 45 to 112 μm, and in a range from 0.46 to 1.62, respectively. Optimization procedure was applied to obtain the smallest oil droplets with the narrowest droplet size distribution at the highest flux of the dispersed phase through the membrane.     

Speciation of Selenium in Enriched Garlic Sprouts by High-Performance Liquid Chromatography Coupled with Inductively Coupled Plasma-Mass Spectrometry

Selenium species in enriched garlic (Allium Sativum L) sprouts were determined by high-performance liquid chromatography coupled with inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). The garlic was grown in a 10 mg/L selenite nutrient solution, and the total selenium accumulated by the sprouts was 250 µg/g. Three mobile phase systems were investigated and a buffer of 20 mmol/L ammonium acetate/5% methanol was chosen for subsequent analysis. Comparative experiments were performed to determine the selenium species in the garlic sprouts with four extraction solutions: 0.1 mol/L HCl, 0.1 mol/L NaOH, 20 mmol/L ammonium acetate/5% methanol and protease XIV. The most suitable results were obtained using 0.1 mol/L HCl as the extracting solution. Validation was performed; all selenium compounds had recoveries of 102.5% to total selenium, with good linearity and precision. The major compound accumulated in the garlic sprouts was methylselenocysteine, which accounted for 65.01% of the selenium.     

Study of the Essential Oil Composition of Cumin Seeds by an Amino Ethyl-Functionalized Nanoporous SPME Fiber

An ultrasound assisted SPME method with a new nanoporous SBA-15 fiber functionalized with 3-[bis(2-hydroxyethyl)amino]propyl-triethoxysilane was successfully applied to the study of the essential oil composition of cumin (Cuminum cyminum L.) seeds. The sample was irradiated by ultrasound radiation and its volatile components were collected by the fiber from the sample headspace and directly injected into a GC-MS injection port for analysis. A simplex method was used for optimization of four different parameters affecting the efficiency of the extraction. Under the optimized conditions (i.e. sample weight, 0.6 g; temperature, 70 °C; sonication time, 12 min and extraction time, 28 min), the number of components identified by the proposed method and their amounts were identical to those of a hydrodistillation technique. The extraction efficiency of the SBA-15 fiber was superior to a PDMS commercial fiber. The major components identified were p-menta-1,3-dien-7-al, cuminaldehyde, γ-terpinene and p-cymene, respectively. The proposed method was applied to a comparative study of the essential oil composition of cumin in three different climate conditions of the Lorestan province in Iran. The results indicated that the essential oils in the temperate and tropical locations were 94.0 and 85.6% of the cold region, respectively.     

Comprehensive Metabolite Profiling in Genetic Resources of Garlic (Allium sativum L.) Collected from Different Geographical Regions

Garlic (Allium sativum) is the second most important Allium crop that has been used as a vegetable and condiment from ancient times due to its characteristic flavor and taste. Although garlic is a sterile plant that reproduces vegetatively through cloves, garlic shows high biodiversity, as well as phenotypic plasticity and environmental adaptation capacity. To determine the possible mechanism underlying this phenomenon and to provide new genetic materials for the development of a novel garlic cultivar with useful agronomic traits, the metabolic profiles in the leaf tissue of 30 garlic accessions collected from different geographical regions, with a special focus on the Asian region, were investigated using LC/MS. In addition, the total saponin and fructan contents in the roots and cloves of the investigated garlic accessions were also evaluated. Total saponin and fructan contents did not separate the garlic accessions based on their geographical origin, implying that saponin and fructan contents were clone-specific and agroclimatic changes have affected the quantitative and qualitative levels of saponins in garlic over a long history of cultivation. Principal component analysis (PCA) and dendrogram clustering of the LC/MS-based metabolite profiling showed two major clusters. Specifically, many Japanese and Central Asia accessions were grouped in cluster I and showed high accumulations of flavonol glucosides, alliin, and methiin. On the other hand, garlic accessions grouped in cluster II exhibited a high accumulation of anthocyanin glucosides and amino acids. Although most of the accessions were not separated based on country of origin, the Central Asia accessions were clustered in one group, implying that these accessions exhibited distinct metabolic profiles. The present study provides useful information that can be used for germplasm selection and the development of new garlic varieties with beneficial biotic and abiotic stress-adaptive traits.     

Application of Nanocrystalline Iranian Diatomite in Immobilized Form for Removal of a Textile Dye

The aim of the present investigation was to immobilize nanocrystalline diatomite within calcium alginate matrix for the adsorption of Direct Red23 (DR23) in aqueous media. Scanning electron microscopy (SEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy were used to characterize the samples. As a result, the adsorption process obeyed pseudo-second-order kinetic model (R² = 0.9934) and Langmuir isotherm model (R² = 0.9732) with a maximum adsorption capacity of 24.10 mg/g. The value of mean free energy (15.81 kJ/mol) demonstrated that the process has been taken place chemically. As the adsorbent dosage increased from 0.5 to 3.0 g/L, the decolorization efficiency (%) increased from 26.0 to 75.5%, respectively. Inversely, the decolorization efficiency (%) decreased from 98.0 to 29.0% with increasing initial dye concentration from 5 to 160 mg/L, respectively. The negative values obtained for Gibbs free energy (ΔG°) and positive value of enthalpy change (ΔH°) indicated spontaneous and endothermic nature of the process.     

Allixin accumulation with long-term storage of garlic

Extremely high accumulation of allxiin, a phytoalexin derived from garlic, was observed in necrotic tissue areas after long-term storage. The allixin produced recrystallized on the surface of the garlic clove. The amount of allixin produced in raw garlic with necrotic tissue areas was 1400 ng/mg wet garlic, which exceeds the minimum exhibitory concentration of allixin. After approximately 2 years of storage, amount of allixin accumulated reached slightly less than 1% of the dry weight of garlic cloves.     

Determination of Herbicide Residues in Garlic by GC–MS

A rapid multi-residue method has been developed for the determination of 16 herbicides in garlic. The analytical procedure is based on prior microwave heating prevention of the generation of sulfur-containing compounds. The garlic samples which had been pretreated were extracted with acetonitrile and cleaned up by solid-phase extraction. The herbicide residues were detected by gas chromatography–mass spectrometry with selected ion monitoring. The recoveries of 16 herbicides ranged from 69.0 to 105.4% with the relative standard deviations (RSD) below 10.1%. The limit of quantification (LOQ) ranged from 0.003 to 0.015 mg kg⁻¹.

     

Allixin induction and accumulation by light irradiation.

Allixin, a phytoalexin isolated from garlic, was induced by irradiating fresh garlic cloves with sunlight or UV light. Induced allixin was analyzed by HPLC, and the accumulated amounts of allixin were 3.1-6.3 microg/g under experimental conditions.     

Determination of Herbicide Residues in Garlic by GC–MS

A rapid multi-residue method has been developed for the determination of 16 herbicides in garlic. The analytical procedure is based on prior microwave heating prevention of the generation of sulfur-containing compounds. The garlic samples which had been pretreated were extracted with acetonitrile and cleaned up by solid-phase extraction. The herbicide residues were detected by gas chromatography–mass spectrometry with selected ion monitoring. The recoveries of 16 herbicides ranged from 69.0 to 105.4% with the relative standard deviations (RSD) below 10.1%. The limit of quantification (LOQ) ranged from 0.003 to 0.015 mg kg^?1.     

Kinetic study of oxalic acid pretreatment of moso bamboo for textile fiber

In this study, samples of moso bamboo were hydrolyzed for textile fiber with oxalic acid under various process conditions. Saeman hydrolysis models were applied to predict the percentage of xylan remained in the substrate after pretreatment and the net xylose yield in the liquid stream. Kinetic constants for Saeman hydrolysis models were analyzed by an Arrhenius-type expansion which include activation energy and catalyst concentration factors. The result showed that the degradation activation energies of xylan and xylose were 97.27 and 136.38 kJ/mol, respectively. Then the kinetic of mathematical models were obtained. Furthermore, the reaction parameters of oxalic acid concentration (1–4 % w/w), reaction temperature (150–180 °C), and reaction time (5–60 min) were handled as a single parameter, combined severity, which ranged in the present study from 0.86 to 1.62. Using combined severity parameters, an optimal condition was achieved which was as the followings: oxalic acid 2.0 % w/w, 170 °C, and 20 min. Under these conditions, 2.3 g glucose/L and 13.65 g xylose/L were produced in the hydrolysate fraction, 54.1 % glucan and 10.8 % xylan were produced in the residue fraction.     

The role of counter-anions in photocatalytic reduction of Ni(II) with a trace amount of titania nanoparticles

The reduction of Ni(II) ion, originated from nitrate or sulfate salts, was investigated based on photo-generated electrons in UV-irradiated TiO₂ aqueous suspensions. Design of experiments, modeling, and process optimization were performed using central composite design of response surface methodology. Influence of pH, temperature, and nickel concentration was investigated based on percentage of reduction efficiency (RE). Under operating conditions of pH = 9.3, T = 40 °C, [Ni(II)]_o = 5 mg L^?1, [TiO₂] = 100 mg L^?1 and after 90 min treatments, 64.8 and 76.1 % RE were achieved for nitrate and sulfate counter-anions, respectively. The higher efficiency obtained with sulfate anion was attributed to the more ionic strength and its interaction with titania nanoparticles. Rate of Ni(II) ions reduction, originated from both of the nickel salts, obeys pseudo-first-order kinetic model. As a relevant criterion, the electrical energy consumption and other criteria were evaluated and were compared with other previously reported processes.     

In vitro and in silico interaction of faba bean (Vicia faba L.) seed extract with xanthine oxidase and evaluation of antioxidant activity as a therapeutic potential

Acetone extract of faba bean (Vicia faba L.) was found to be highest total phenol and flavonoid content among all extracts. Antioxidant activity for inhibition percentage (free radical scavenging activity) had 86.47% for acetone extract, and 97.36% for ascorbic acid respectively. IC₅₀ value of ascorbic acid and acetone extact were found to be 9 μg/mL ± 0.20 and 30 μg/mL ± 0.21. Faba bean seeds had catechin, epicatechin, gallic acid and ellagic acid which on molecular docking study revealed that it binds effectively with xanthine oxidase by binding energy of –7.78, –6.11, –6.39, –5.78 kcal/mol respectively compared to allopurinol drug having binding energy of –4.94 kcal/mol. Gallic acid, ellagic acid, catechin, epicatechin (polyphenols) and allopurinol bind other than catalytic residues (Glu-1261) of xanthine oxidase. In vitro and in silico analysis recommended that mode of enzyme inhibition was mixed type.     

Fractionation of Sugarcane Bagasse Using a Combined Process of Dilute Acid and Ionic Liquid Treatments

Biorefineries processing lignocellulose will produce chemicals and fuels from chemical constituents, cellulose, hemicelluloses, and lignin to replace fossil-derived products. Fractionation of sugarcane bagasse into three pure streams of chemical constituents was addressed through dissolution of constituents with the ionic liquids, 1-ethyl-3-methylimidazolium acetate ([EMiM]CH₃COO) or 1-butyl-3-methylimidazolium methyl sulfate ([BMiM]MeSO₄). Constituents were isolated from the reaction mixture with the anti-solvents acetone (ā), acetone–water (AW), and sodium hydroxide (NaOH). Delignification was enhanced by NaOH, although resulting in impure product streams. Xylose pre-extraction (75 % w/w) by dilute acid pretreatment, prior to ionic liquid treatment, improved lignin purity after anti-solvent separation. Fractionation efficiency of the combined process was maximized (84 %) by ionic liquid treatment at 125 °C for 120 min, resulting in 80.2 % (w/w) lignin removal and 76.5 % (w/w) lignin recovery. Ionic liquids achieved similar degrees of delignification, although fully digestible cellulose-rich solids were produced only by [EMiM]CH₃COO treatment.     

Investigation of adsorption behavior and energy transfer of cationic porphyrins on clay surface at low loading levels by picosecond time-resolved fluorescence measurement

Time-resolved fluorescence and steady-state spectroscopic measurements were performed with +4-charged cationic porphyrins adsorbed on an anionic-type clay (Sumecton SA; SSA) surface at a low molecular loading level (10 % vs. cation-exchange capacity of clay) corresponding to an occupied area of ca 50 nm² per molecule. Absorption spectra indicated no interaction between transition moments of the porphyrins on the clay surface. An efficient energy-transfer process from donor to acceptor porphyrin was observed on the clay surface even under low porphyrin loading conditions. The efficiency of energy transfer obtained from the steady-state measurement was 65 %. Real-time behavior of the porphyrins was successfully captured during energy transfer. The rate constant of the energy transfer obtained from time-resolved fluorescence measurements was found to be 5.3 × 10⁸ s^?1. According to the efficiency and the rate constant, it is proposed that the adsorbed porphyrins did not have a uniform and fixed distribution.     

Comparison of HPLC and MEEKC for Miconazole Nitrate Determination in Pharmaceutical Formulation

A simple solid phase extraction (SPE) method coupled with high performance liquid chromatography (HPLC) using UV detector and microemulsion electrokinetic chromatography (MEEKC) has been developed and compared for the quantitative determination of miconazole nitrate in pharmaceutical formulation. For HPLC method, two parameters were optimized, namely, the wavelength and the mobile phases. The optimized condition was at the 225 nm wavelength and the mobile phase of ACN:MeOH (90:10 v/v). There are seven MEEKC parameters that were optimized, in this research, which were applied to voltage, temperature, wavelength, sodium dodecyl sulfate (SDS) concentration, buffer pH, buffer concentration and butan-1-ol concentration. The optimum MEEKC condition was obtained using 86.35 % (w/w) 2.5 mM borate buffer pH 9, 0.25 % (w/w) SDS, 0.8 % (w/w) ethyl acetate, 6.6 % w/w butan-1-ol and 6.0 % (w/w) acetonitrile. The combination of SPE using a diol column with HPLC–UV and the MEEKC methods were successfully applied for the determination of miconazole nitrate in a pharmaceutical formulation with the recovery percentage of 98.35 and 92.50 %, respectively.

     

Separation and purification of six compounds from the flowers of Cerasus yedoensis (Matsum.) by high-speed countercurrent chromatography in stepwise elution mode

Six compounds from the flower of Cerasus yedoensis (Matsum.) were successfully isolated by high-speed countercurrent chromatography (HSCCC) and preparative high performance liquid chromatography using stepwise elution with a pair of two-phase solvent systems composed of ethyl acetate–n-butanol–formic acid–water at volume ratio of 4:1.5:0.15:5 and ethyl acetate–ethanol–formic acid–water at volume ratio of 4:1:0.15:5 for the first time. This separation process produced (a) 141 mg of 1-O-caffeoyl-β-D-glucopyranoside, (b) 28 mg of p-coumaric acid glucoside, (c) 13 mg of chlorogenic acid, (d) 21 mg of quercetin-3-O-β-D-glucopyranoside, (e) 19 mg of kaempferol 3-O-β-D-glucopyranoside, and (f) 25 mg of caffeic acid from 400 mg of crude sample with the purities of 96.51, 98.82, 94.96, 99.01, 82.51, and 82.45%, respectively. MS, ¹H NMR, and ¹³C NMR analyses were used for the chemical structure identification.     

Comparative metabolic profiling of Costus speciosus leaves and rhizomes using NMR,GC-MS and UPLC/ESI-MS/MS

Costus speciosus had been used in oriental systems of medicines, to treat diverse ailments. The present study was focused on NMR, GC-MS and UPLC/ESI-MS/MS-based metabolic profiling of C. speciosus. This metabolic study resulted in the identification of 91 and quantification of 69 metabolites. Caffeic acid derivatives previously unreported in C. speciosus were also identified. High quantity of steroidal saponins namely methyl protogracillin (297.97 ± 0.07 mg/g dried wt.) and dioscin (158.72 ± 0.27 mg/g dried wt.) were observed in butanol fraction of rhizomes. Health care metabolites including caffeic acid (37.88 ± 0.04 mg/g dried wt.) and trehalose (75.12 ± 0.08 mg/g dried wt.) were also detected in ethyl acetate and aqueous fractions of rhizomes, respectively. Metabolites of nutraceutical and biological significance including eremanthine (5.14 ± 0.68%, peak area), tocopherols (~22%), sterols (~25%) were also identified from hexane fractions of rhizomes and leaves using GC-MS. The analytical techniques used had successfully differentiated metabolites composition among leaves and rhizomes.     

Surface-Mediated Hydrohalogenation of Isoprene: A Facile Preparation of Prenyl Halides

Abstract

The reaction of isoprene with SOCl₂ (0.5 mol equiv.) or PBr₃ (0.4 mol equiv.) or PI₃ (0.4 mol equiv.) in the presence of SiO₂ at ?10°C produced prenyl chloride (82%), or bromide (70%) or iodide (65%), respectively, in less than 30 min reaction time.