A simple method for extracting both active oily and water soluble extract (WSE) from Nigella sativa (L.) seeds using a single solvent system

The current study provides a way of extraction for both active NSO and WSE from Nigella sativa seeds using 98% methanol. About 1?kg of ground seeds was macerated by 1:2.5 w/v (g/mL) for 72?hours. After rotary evaporation and 7 days of continuous drying and chilling at 50 and 4?°C, NSO and WSE were obtained at the same instant. Solubility tests of 24 solvents and 11 thin layer chromatographic analyses while 2, 2-diphenyl-1-picrylhydrazyl free radical scavenging assay of NSO (73.66) , WSE (33.32) and NSO?+?WSE (78.22) against ascorbic acid (IC50?=?4.28?mg/mL) was performed. WSE was found to be highly soluble in water and 5% NaOH exhibiting the same Rf value of 0.95 for EtOH:DMSO (9:1) against the honey. WSE has revealed more than twofold higher anti-oxidant activity than others. Formulation of WSE with Tualang honey may provide better targeted hydrophilic drug delivery systems.     

Sharp bounds for the valence of certain harmonic polynomials

In Khavinson and Swiatek (2002) it was proved that harmonic polynomials , where is a holomorphic polynomial of degree , have at most complex zeros. We show that this bound is sharp for all by proving a conjecture of Sarason and Crofoot about the existence of certain extremal polynomials . We also count the number of equivalence classes of these polynomials.

     

Determination of 13C/12C ratios of endogenous urinary steroids: method validation, reference population and application to doping control purposes

The application of a comprehensive gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS)-based method for stable carbon isotopes of endogenous urinary steroids is presented. The key element in sample preparation is the consecutive cleanup with high-performance liquid chromatography (HPLC) of underivatized and acetylated steroids, which allows the isolation of ten analytes (11beta-hydroxyandrosterone, 5alpha-androst-16-en-3beta-ol, pregnanediol, androsterone, etiocholanolone, testosterone, epitestosterone, 5alpha-androstane-3alpha,17beta-diol, 5beta-androstane-3alpha,17beta-diol and dehydroepiandrosterone) from a single urine specimen. These steroids are of particular importance to doping controls as they enable the sensitive and retrospective detection of steroid abuse by athletes.Depending on the biological background, the determination limit for all steroids ranges from 5 to 10 ng/mL for a 10 mL specimen. The method is validated by means of linear mixing models for each steroid, which covers repeatability and reproducibility. Specificity was further demonstrated by gas chromatography/mass spectrometry (GC/MS) for each analyte, and no influence of the sample preparation or the quantity of analyte on carbon isotope ratios was observed. In order to determine naturally occurring (13)C/(12)C ratios of all implemented steroids, a reference population of n = 61 subjects was measured to enable the calculation of reference limits for all relevant steroidal Delta values.     

Determination of therapeutics with growth-hormone secretagogue activity in human urine for doping control purposes

The administration of growth-promoting agents such as human growth hormone as well as compounds with respective secretagogue activity is prohibited in sports according to the regulations of the World Anti-Doping Agency. Acetylcholine esterase inhibitors have been demonstrated to stimulate growth-hormone secretion in elderly humans, and new orally active drugs have been developed to provide alternatives to therapeutic injections of growth-hormone preparations. Preventive anti-doping strategies include method development for emerging drugs and potentially misused compounds. Hence, the mass spectrometric dissociation behavior of three acetylcholine esterase inhibitors (donepezil, galantamine and rivastigmine) and a structural analogue to the growth-hormone secretagogue SM-130686 were studied using high-resolution/high-accuracy orbitrap mass spectrometry. These data provided substantial information for screening procedures, complementing common methods of sports drug testing. Using liquid-liquid extraction and subsequent liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis, the four target analytes were determined at urinary concentrations of 15-20 ng/mL, recoveries ranged from 55-97%, and assay precisions were calculated at 5.2-15.8% (intraday) and 10.2-21.6% (interday) for all compounds. The applicability of the developed assay to authentic urine specimens was tested using two administration study urine samples after application of Reminyl (galantamine) and Aricept (donepezil). In both cases, the administered drug and the respective desmethylated metabolites were detected.     

Sulphur and oxygen isotopic characters of dissolved sulphate in groundwater from the Pleistocene aquifer in the southern Jordan Valley (Jericho area, Palestine)

Sulphate and chloride concentrations in the shallow Pleistocene aquifer systems in the lower Jordan valley area indicate a general trend of increasing salinity eastward and southward. This study was conducted in one of the important sub-basins feeding the Pleo-Pleistocene aquifer in the Jericho area in the southern part of the valley using S and O isotopes of dissolved sulphate. The results show that sulphate has mainly two contributions to the groundwater. One is the surface seepage, which is present as a salty leachate form with the positive delta34Ssulphate values of primary gypsum in Lisan and Samara formations, and the second is the upwelling saline water which was in contact with a deep secondary gypsum, aragonites and salty rocks and rose up under heavy abstraction with depleted 34S in sulphate and relatively high sulphate and chloride content. The latest was clearly shown in the Arab Project wells to the east that is undergoing a continuous heavy abstraction. The isotopic signatures of S and O in these wells to the east show that this depleted 34S and highly concentrated sulphate might also indicate a dissolved sulphate originating from pyrite oxidation that results from the interaction with a pyrite-rich aquifer, which can well up with salty water under heavy abstraction and is oxidised in the upper aerobic shallow aquifer.     

Stereoselective synthesis of highly functionalized thiopeptide thiazole fragments from uronic acid/cysteine condensation products: access to the core dipeptide of the thiazomycins and nocathiacins

We present the stereoselective synthesis of various highly functionalized thiazole dipeptides that are found in thiopeptide antibiotics like thiazomycins and nocathiacins. The condensation of an uronic acid with l-cysteine methyl ester delivers along two different protocols the stereopure thiazolidine lactones or lactams on the multigram scale, respectively. Oxidation of the thiazolidine moiety to the thiazole and tailoring of the sugar chains yield the thiazole dipeptide as present in the core motif of the thiopeptide antibiotics, as well as its epimer and a homolog. The modular assembly of the potent natural products and their analogs relies on the synthetic accessibility of adequately protected building blocks of tailored absolute stereochemistry.     

Measurement of the noise generation at the trailing edge of porous airfoils

Owls are commonly known for their quiet flight, enabled by three adaptions of their wings and plumage: leading edge serrations, trailing edge fringes and a soft and elastic downy upper surface of the feathers. In order to gain a better understanding of the aeroacoustic effects of the third property that is equivalent to an increased permeability of the plumage to air, an experimental survey on a set of airfoils made of different porous materials was carried out. Several airfoils with the same shape and size but made of different porous materials characterized by their flow resistivities and one non-porous reference airfoil were subject to the flow in an aeroacoustic open jet wind tunnel. The flow speed has been varied between approximately 25 and 50 m/s. The geometric angle of attack ranged from −16° to 20° in 4°-steps. The results of the aeroacoustic measurements, made with a 56-microphone array positioned out of flow, and of the measurements of lift and drag are given and discussed.