A New and Fast HPLC Method for Determination of Rutin, Troxerutin, Diosmin and Hesperidin in Food Supplements Using Fused-Core Column Technology

A new and fast high-performance liquid chromatography (HPLC) method using fused-core column for separation of rutin, troxerutin, diosmin, and hesperidin has been developed and used for determination of these flavonoids in food supplements. Efficient separation of flavonoids and internal standard methylparaben was achieved on the fused-core column Ascentis Express RP-Amide (100?×?3.0 mm), particle size 2.7 μm, with mobile phase acetonitrile/water solution of acetic acid pH?3 (30:70, v/v) at a flow rate of 1.0 mL?min^?1 and at temperature 50 °C. The detection wavelengths were set at 283 nm for hesperidin and at 255 nm for rutin, troxerutin, diosmin, and internal standard methylparaben. Under the optimal chromatographic conditions, good linearity with correlation coefficients in the range (r?=?0.9991–0.9998; n?=?7) for all flavonoids was achieved. Commercial samples of food supplements were extracted with 100 % dimethyl sulfoxide using ultrasound bath for 10 min and then diluted to methanol. A 5-μL sample volume of the filtered solution was directly injected into the HPLC system. Accuracy of the method defined as a mean recovery of flavonoids from food supplement matrix was in the range 96.2–104.4 % for all flavonoids. The intraday method precision was satisfactory, and relative standard deviations of sample analysis including preparation and determination of different food supplements were in the range 0.5–3.5 % for all flavonoids. The developed method has shown high sample throughput during sample preparation process, modern separation approach, and short time (5 min) of analysis.     

Synthesis of CaCO3–P(MMA–BA) nanocomposite and its application in water based alkyd emulsion coating

As part of broader effort to synthesize a new class of water-based composite, hybrid emulsion polymerization was carried out with acrylic monomers [methyl methacrylate (MMA), n-butyl acrylate (BA)]. Nanocomposite of P(MMA–BA)/nano CaCO₃ was synthesized by in situ emulsion polymerization. Water-based alkyd coating with various proportions nano CaCO₃, P(MMA–BA) and its nanocomposite was formulated. Extent of polymerization with and without nano CaCO₃ was measured using gravimetric method. Thermal properties of neat polymer, nanocomposite and coating films were evaluated by TGA and DSC, DTA analysis. Uniform dispersion of nano CaCO₃ in polymer matrix was ensured from SEM/TEM images. Incorporation of nanoparticles to hybrid polymer and nanocomposite to alkyd emulsion showed significant enhancement in mechanical and thermal properties. Dual role of nanocomposite in coating; as a partial binder and a filler to improve property profile of neat coating has been reported.     

In situ MTBE biodegradation supported by diffusive oxygen release

Microcosm studies with sediments from Vandenberg Air Force Base, CA, suggest that native aerobic methyl tert-butyl ether (MTBE)-degrading microorganisms can be stimulated to degrade MTBE. In a series of field experiments, dissolved oxygen has been released into the anaerobic MTBE plume by diffusion through the walls of oxygen-pressurized polymeric tubing placed in contact with the flowing groundwater. MTBE concentrations were decreased from several hundred to less than 10 microg/L during passage through the induced aerobic zone, due apparently to in situ biodegradation: abiotic MTBE loss mechanisms were insignificant. Lag time for initiation of degradation was less than 2 months, and the apparent pseudo-first-order degradation rate was 5.3 day(-1). Additional MTBE was added in steps to raise the influent concentration to a maximum of 2.1 mg/L. With each step, MTBE was degraded within the preestablished aerobic treatment zone at rates ranging from 4.4 to 8.6 day(-1). Excess dissolved oxygen suggested that even higher MTBE concentrations could have been treated. Continued flow through the treatment zone was repeatedly confirmed through tracer and other tests. These and others' results suggest that it is possible to create permeable in situ treatment zones solely by releasing oxygen to support native microbial degradation of MTBE.     

Solar-plus-storage economics: What works where,and why?

This paper explores the economics of solar-plus-storage projects for commercial-scale, behind-the-meter applications. It provides insight into the near-term and future solar-plus-storage market opportunities across the U.S. We explore the impacts of location, building load profile, technology cost, utility rate structure, and policies on solar-plus-storage economic viability, and identify which factors are most significant to project economics. While savings from storage-only projects are largely derived from demand charge reductions, solar combined with storage also provides significant energy charge savings. A common assumption is that load profiles with peaks are likely candidates for savings from storage, due to the opportunity for demand charge reduction. Our results indicate that potential for savings from combining solar with storage is independent of building load variability, likely due to the energy cost reductions from the solar. Systems are more often economical under time of use and demand charge rates, particularly when demand charges are >$10 per kilowatt. Where systems were found to be economical, expected lifetime savings averaged between 7%–10%, with savings of 30% in numerous cases. Near term markets exist for solar-plus-storage in locations such as California and New York. As technology prices drop, the number of building types that can benefit increase, and additional markets appear in Colorado, New Mexico, and Alaska. All data from the study and interactive modeling results are available at: https://openei.org/wiki/Solar+Storage.     

Spinal amino acid release and precipitated withdrawal in rats chronically infused with spinal morphine

Glutamate receptors are implicated in the genesis of opioid tolerance and dependence. Factors governing release of amino acids in systems chronically exposed to opiates, however, remain undefined. Using rats, each prepared with a spinal loop dialysis catheter and with a chronic lumbar intrathecal infusion catheter connected to a subcutaneous minipump, the release of amino acids before and during antagonist-precipitated withdrawal in unanesthetized rats was examined. Spinal infusion of morphine (20 nmol/micro l/hr) for 4 d had little effect on resting release of amino acids. In morphine-infused, but not saline-infused, rats naloxone (2 mg/kg, i.p.) evoked an immediate increase in the release of L-glutamate (299 +/- 143%) and taurine (306 +/- 113%) but not other amino acids. The magnitude and time course of the release of these amino acids significantly correlated with behavioral indices of withdrawal intensity. Acute intrathecal pretreatment immediately before naloxone with clonidine (20 microg; alpha2 agonist), MK-801 (3 microg; noncompetitive NMDA antagonist), or aminophosphonopentanoic acid (AP-5; 3 microg; competitive NMDA antagonist) suppressed naloxone-induced increases in spinal L-glutamate and taurine release and behavioral signs of withdrawal in spinal morphine-infused rats. Results point to a correlated increase in spinal L-glutamate release, which contributes to genesis of the opioid withdrawal syndrome. Agents such as clonidine that suppress opioid withdrawal may owe their action to an inhibition of excitatory amino acid release. The effects of MK-801 and AP-5 suggest a glutamate-evoked glutamate release.     

High-dose thiotepa and etoposide-based regimens with autologous hematopoietic support for high-risk or recurrent CNS tumors in children and adults

The prognosis in patients with primary brain tumors treated with surgery, radiotherapy and conventional chemotherapy remains poor. To improve outcome, combination high-dose chemotherapy (HDC) has been explored in children, but rarely in adults. This study was performed to determine the tolerability of three-drug combination high-dose thiotepa (T) and etoposide (E)-based regimens in pediatric and adult patients with high-risk or recurrent primary brain tumors. Thirty-one patients (13 children and 18 adults) with brain tumors were treated with high-dose chemotherapy: 19 with BCNU (B) and TE (BTE regimen), and 12 with carboplatin (C) and TE (CTE regimen). Patients received growth factors and hematopoietic support with marrow (n = 15), peripheral blood progenitor cells (PBPC) (n = 11) or both (n = 5). The 100 day toxic mortality rate was 3% (1/31). Grade III/IV toxicities included mucositis (58%), hepatitis (39%) and diarrhea (42%). Five patients had seizures and two had transient encephalopathy (23%). All patients had neutropenic fever and all pediatric patients required hyperalimentation. Median time to engraftment with absolute neutrophil count (ANC) >0.5 x 10(9)/l was 11 days (range 8-37 days). Time to ANC engraftment was significantly longer (P = 0.0001) in patients receiving marrow (median 14 days, range 10-37) than for PBPC (median 9.5 days, range 8-10). Platelet engraftment >50 x 10(9)/l was 24 days (range 14-53 days) in children. In adults, platelet engraftment >20 x 10(9)/l was 12 days (range 9-65 days). In 11 patients supported with PBPC, there was a significant inverse correlation between CD34+ dose and days to ANC (rho = -0.87, P = 0.009) and platelet engraftment (rho = -0.85, P = 0.005), with CD34+ dose predicting time to engraftment following HDC. Overall, 30% of evaluable patients (7/24) had a complete response (CR) (n = 3) or partial response (PR) (n = 4). Median time to tumor progression (TTP) was 7 months, with an overall median survival of 12 months. These TE-based BCNU or carboplatin three-drug combination HDC regimens are safe and tolerable with promising response rates in both children and older adults.     

Three-dimensional structure of lipoamide dehydrogenase from Pseudomonas fluorescens at 2.8 A resolution. Analysis of redox and thermostability properties

The structure of Pseudomonas fluorescens lipoamide dehydrogenase, a dimeric flavoenzyme with a molecular mass of 106,000 daltons, was solved by the molecular replacement method and refined to an R-factor of 19.4% at 2.8 A resolution. The root-mean-square difference from ideal values for bonds and angles is 0.019 A and 3.8 degrees, respectively. The structure is closely related to that of the same flavoprotein from Azotobacter vinelandii. The root-mean-square difference for 932 C alpha atoms is 0.64 A, with 84% sequence identity. The residues in the active site are identical, while 89% of the interface residues are the same in the two enzymes. A few structural variations provide the basis for the differences in thermostability and redox properties between the two homologous proteins. Particularly, in the A. vinelandii molecule a threonine to alanine (T452A) mutation leaves a buried carbonyl oxygen, located at the subunit interface and in proximity of the flavin ring, unpaired to any H-bond donor, probably providing an explanation for the lower stability of the A. vinelandii enzyme with respect to the P. fluorescens enzyme. Six surface loops, which previously could not be accurately positioned in the A. vinelandii structure, are well defined in P. fluorescens lipoamide dehydrogenase. On the basis of the P. fluorescens structure, the six loops could be correctly defined also in the A. vinelandii enzyme. This is an unusual case where similar refinement methodologies applied to two crystal forms of closely related proteins led to electron density maps of substantially different quality. The correct definition of these surface residues is likely to be an essential step for revealing the structural basis of the interactions between lipoamide dehydrogenase and the other members of the pyruvate dehydrogenase multienzyme complex.     

Benign solitary fibrous tumour of the pre-sacral space: MRI findings

Benign solitary fibrous tumour, a rare mesenchymal tumour of adults, usually arises from the pleura. Only a few cases have been reported in the retroperitoneum and, to our knowledge, there has been no report of its imaging features. We describe the MRI features of benign solitary fibrous tumour arising from the pre-sacral space.