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Sample records for lysergic acid diethyl

  1. 21 CFR 862.3580 - Lysergic acid diethylamide (LSD) test system.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Lysergic acid diethylamide (LSD) test system. 862... Test Systems § 862.3580 Lysergic acid diethylamide (LSD) test system. (a) Identification. A lysergic acid diethylamide (LSD) test system is a device intended to measure lysergic acid diethylamide, a...

  2. Lysergic acid diethylamide: a drug of 'use'?

    Science.gov (United States)

    Das, Saibal; Barnwal, Preeti; Ramasamy, Anand; Sen, Sumalya; Mondal, Somnath

    2016-06-01

    Lysergic acid diethylamide (LSD), described as a classical hallucinogen, began its journey from the middle of the last century following an accidental discovery. Since then, it was used as a popular and notorious substance of abuse in various parts of the world. Its beneficial role as an adjunct to psychotherapy was much unknown, until some 'benevolent' experiments were carried out over time to explore some of its potential uses. But, many of its effects were unclear and seemed to be a psychedelic enigma. In this review article, we have described the receptor pharmacology, mechanism of action, effects and adverse effects of LSD on the normal body system. We have also highlighted its addictive potentials and the chances of developing tolerance. We have assimilated some of the interesting therapeutic uses of this drug, such as an antianxiety agent, a creativity enhancer, a suggestibility enhancer, and a performance enhancer. We have also described LSD to be successfully used in drug and alcohol dependence, and as a part of psychedelic peak therapy in terminally ill patients. The relevant chronological history and literature in the light of present knowledge and scenarios have been discussed. Based on available evidence, LSD could be tried therapeutically in certain specific conditions under controlled settings. But as we mention, due to all the safety concerns, the use of this nonaddictive 'entheogen' in actual practice warrants a lot of expertise, caution, cooperation and ethical considerations.

  3. Reversal learning enhanced by lysergic acid diethylamide (LSD)

    Science.gov (United States)

    King, A.R.; Martin, I.L.; Arabella Melville, K.

    1974-01-01

    1 Small doses of lysergic acid diethylamide (LSD) (12.5-50 μg/kg) consistently facilitated learning of a brightness discrimination reversal. 2 2-Bromo-lysergic acid diethylamide (BOL-148), a structural analogue of LSD, with similar peripheral anti-5-hydroxytrypamine activity but no psychotomimetic properties, had no effect in this learning situation at a similar dose (25 μg/kg). 3 LSD, but not BOL-148, caused a small but significant increase in brain 5-hydroxytryptamine levels, but had no effect on the levels of catecholamines in the brain at 25 μg/kg. PMID:4458849

  4. Acute effects of lysergic acid diethylamide in healthy subjects

    OpenAIRE

    2015-01-01

    After no research in humans for >40 years, there is renewed interest in using lysergic acid diethylamide (LSD) in clinical psychiatric research and practice. There are no modern studies on the subjective and autonomic effects of LSD, and its endocrine effects are unknown. In animals, LSD disrupts prepulse inhibition (PPI) of the acoustic startle response, and patients with schizophrenia exhibit similar impairments in PPI. However, no data are available on the effects of LSD on PPI in humans.;...

  5. Lysergic acid diethylamide: a drug of ‘use’?

    Science.gov (United States)

    Das, Saibal; Barnwal, Preeti; Ramasamy, Anand; Sen, Sumalya; Mondal, Somnath

    2016-01-01

    Lysergic acid diethylamide (LSD), described as a classical hallucinogen, began its journey from the middle of the last century following an accidental discovery. Since then, it was used as a popular and notorious substance of abuse in various parts of the world. Its beneficial role as an adjunct to psychotherapy was much unknown, until some ‘benevolent’ experiments were carried out over time to explore some of its potential uses. But, many of its effects were unclear and seemed to be a psychedelic enigma. In this review article, we have described the receptor pharmacology, mechanism of action, effects and adverse effects of LSD on the normal body system. We have also highlighted its addictive potentials and the chances of developing tolerance. We have assimilated some of the interesting therapeutic uses of this drug, such as an antianxiety agent, a creativity enhancer, a suggestibility enhancer, and a performance enhancer. We have also described LSD to be successfully used in drug and alcohol dependence, and as a part of psychedelic peak therapy in terminally ill patients. The relevant chronological history and literature in the light of present knowledge and scenarios have been discussed. Based on available evidence, LSD could be tried therapeutically in certain specific conditions under controlled settings. But as we mention, due to all the safety concerns, the use of this nonaddictive ‘entheogen’ in actual practice warrants a lot of expertise, caution, cooperation and ethical considerations. PMID:27354909

  6. The paradoxical psychological effects of lysergic acid diethylamide (LSD).

    Science.gov (United States)

    Carhart-Harris, R L; Kaelen, M; Bolstridge, M; Williams, T M; Williams, L T; Underwood, R; Feilding, A; Nutt, D J

    2016-05-01

    Lysergic acid diethylamide (LSD) is a potent serotonergic hallucinogen or psychedelic that modulates consciousness in a marked and novel way. This study sought to examine the acute and mid-term psychological effects of LSD in a controlled study. A total of 20 healthy volunteers participated in this within-subjects study. Participants received LSD (75 µg, intravenously) on one occasion and placebo (saline, intravenously) on another, in a balanced order, with at least 2 weeks separating sessions. Acute subjective effects were measured using the Altered States of Consciousness questionnaire and the Psychotomimetic States Inventory (PSI). A measure of optimism (the Revised Life Orientation Test), the Revised NEO Personality Inventory, and the Peter's Delusions Inventory were issued at baseline and 2 weeks after each session. LSD produced robust psychological effects; including heightened mood but also high scores on the PSI, an index of psychosis-like symptoms. Increased optimism and trait openness were observed 2 weeks after LSD (and not placebo) and there were no changes in delusional thinking. The present findings reinforce the view that psychedelics elicit psychosis-like symptoms acutely yet improve psychological wellbeing in the mid to long term. It is proposed that acute alterations in mood are secondary to a more fundamental modulation in the quality of cognition, and that increased cognitive flexibility subsequent to serotonin 2A receptor (5-HT2AR) stimulation promotes emotional lability during intoxication and leaves a residue of 'loosened cognition' in the mid to long term that is conducive to improved psychological wellbeing.

  7. The pharmacology of lysergic acid diethylamide: a review.

    Science.gov (United States)

    Passie, Torsten; Halpern, John H; Stichtenoth, Dirk O; Emrich, Hinderk M; Hintzen, Annelie

    2008-01-01

    Lysergic acid diethylamide (LSD) was synthesized in 1938 and its psychoactive effects discovered in 1943. It was used during the 1950s and 1960s as an experimental drug in psychiatric research for producing so-called "experimental psychosis" by altering neurotransmitter system and in psychotherapeutic procedures ("psycholytic" and "psychedelic" therapy). From the mid 1960s, it became an illegal drug of abuse with widespread use that continues today. With the entry of new methods of research and better study oversight, scientific interest in LSD has resumed for brain research and experimental treatments. Due to the lack of any comprehensive review since the 1950s and the widely dispersed experimental literature, the present review focuses on all aspects of the pharmacology and psychopharmacology of LSD. A thorough search of the experimental literature regarding the pharmacology of LSD was performed and the extracted results are given in this review. (Psycho-) pharmacological research on LSD was extensive and produced nearly 10,000 scientific papers. The pharmacology of LSD is complex and its mechanisms of action are still not completely understood. LSD is physiologically well tolerated and psychological reactions can be controlled in a medically supervised setting, but complications may easily result from uncontrolled use by layman. Actually there is new interest in LSD as an experimental tool for elucidating neural mechanisms of (states of) consciousness and there are recently discovered treatment options with LSD in cluster headache and with the terminally ill.

  8. Pharmacokinetics and Pharmacodynamics of Lysergic Acid Diethylamide in Healthy Subjects.

    Science.gov (United States)

    Dolder, Patrick C; Schmid, Yasmin; Steuer, Andrea E; Kraemer, Thomas; Rentsch, Katharina M; Hammann, Felix; Liechti, Matthias E

    2017-02-14

    Lysergic acid diethylamide (LSD) is used recreationally and in clinical research. The aim of the present study was to characterize the pharmacokinetics and exposure-response relationship of oral LSD. We analyzed pharmacokinetic data from two published placebo-controlled, double-blind, cross-over studies using oral administration of LSD 100 and 200 µg in 24 and 16 subjects, respectively. The pharmacokinetics of the 100-µg dose is shown for the first time and data for the 200-µg dose were reanalyzed and included. Plasma concentrations of LSD, subjective effects, and vital signs were repeatedly assessed. Pharmacokinetic parameters were determined using compartmental modeling. Concentration-effect relationships were described using pharmacokinetic-pharmacodynamic modeling. Geometric mean (95% confidence interval) maximum plasma concentration values of 1.3 (1.2-1.9) and 3.1 (2.6-4.0) ng/mL were reached 1.4 and 1.5 h after administration of 100 and 200 µg LSD, respectively. The plasma half-life was 2.6 h (2.2-3.4 h). The subjective effects lasted (mean ± standard deviation) 8.2 ± 2.1 and 11.6 ± 1.7 h for the 100- and 200-µg LSD doses, respectively. Subjective peak effects were reached 2.8 and 2.5 h after administration of LSD 100 and 200 µg, respectively. A close relationship was observed between the LSD concentration and subjective response within subjects, with moderate counterclockwise hysteresis. Half-maximal effective concentration values were in the range of 1 ng/mL. No correlations were found between plasma LSD concentrations and the effects of LSD across subjects at or near maximum plasma concentration and within dose groups. The present pharmacokinetic data are important for the evaluation of clinical study findings (e.g., functional magnetic resonance imaging studies) and the interpretation of LSD intoxication. Oral LSD presented dose-proportional pharmacokinetics and first-order elimination up to 12 h. The effects of LSD were related

  9. Genetic toxicology of lysergic acid diethylamide (LSD-25).

    Science.gov (United States)

    Cohen, M M; Shiloh, Y

    The acute and the chronic psychotomimetic potentials of the hallucinogen lysergic acid diethylamide (LSD-25) have been recognized for almost 40 years. That additional types of the biological effects should have come under scrutiny was directly attributable to widespread use and abuse of this drug on a world-wide basis. Although "genetic toxicology" encompasses a broad spectrum of disciplines, including many areas of highly specialized research, perhaps the most germane, and those on which this review has concentrated, are Clastogenicity, Mutagenicity, Teratogenicity and Oncogenicity. Based on our current understanding and interpretation of the available data, the genetic toxicology of LSD provides an excellent example of Newton's "third law of motion", e.g., to every force there is an equal and opposite reaction force. From the published material it is impossible to draw clear cut conclusions regarding any of the above "problem areas" in spite of the considerable scientific effort invested. Most of the in vitro studies performed on the clastogenicity of LSD indicate either suppression of mitosis or enhanced chromosome damage. However, extrapolation of such results to the in vivo situation is very difficult. With regard to in vivo human use of the drug, no concensus is attainable as to chromosome breakage and the inconsistencies within and between studies remain inexplicable. However, several of the "controlled" investigations assessing the in vivo effect of chemically pure LSD suggest a transient increase in lymphocyte chromosome breakage. On the other hand, the results of cytogenetic studies on experimental animals are contradictory. Although human studies are nonexistent, in those experimental organisms tested, using accepted techniques, LSD proved to be, at best, a weak mutagen, if mutagenic at all. Teratogenicity studies in animals are confusing due to the multitude of organisms and plethora of discriminant parameters studied. However, with regard to man there

  10. Optimization and immunological characterization of a photochemically coupled lysergic acid diethylamide (LSD) immunogen.

    Science.gov (United States)

    Kerrigan, S; Brooks, D E

    1998-01-01

    A photoreactive heterobifunctional linker was used to prepare an immunogen in which lysergic acid diethylamide was indirectly coupled to keyhole limpet hemocyanin at multiple sites on the drug. It was possible to attach approximately 35 drug molecules to each protein using approximately equal amounts of both species during the reaction. The presence of buffer components or water severely compromised reaction efficiency, as estimated from the molar substitution ratio. Factors such as excess linker, pH, irradiation of dry matrix in the absence of buffer, and the drug/protein ratio used during photolysis were shown to have pronounced effects on reaction efficiency. Structural insights regarding immunogen coupling were obtained by determining the specificities of antibodies which were raised against the immunogen. Cross-reactivity data indicated that haptenation of protein likely occurred at positions N1 and N6 of lysergic acid diethylamide, which is plausible given the electrophilicity of the photogenerated aryl nitrene.

  11. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    Science.gov (United States)

    Musshoff, F; Daldrup, T

    1997-08-04

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

  12. Possible role of biochemiluminescent photons for lysergic acid diethylamide (LSD)-induced phosphenes and visual hallucinations.

    Science.gov (United States)

    Kapócs, Gábor; Scholkmann, Felix; Salari, Vahid; Császár, Noémi; Szőke, Henrik; Bókkon, István

    2017-01-01

    Today, there is an increased interest in research on lysergic acid diethylamide (LSD) because it may offer new opportunities in psychotherapy under controlled settings. The more we know about how a drug works in the brain, the more opportunities there will be to exploit it in medicine. Here, based on our previously published papers and investigations, we suggest that LSD-induced visual hallucinations/phosphenes may be due to the transient enhancement of bioluminescent photons in the early retinotopic visual system in blind as well as healthy people.

  13. Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

    Science.gov (United States)

    Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

    2014-12-01

    Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Lysergic acid diethylamide (LSD) for alcoholism: meta-analysis of randomized controlled trials.

    Science.gov (United States)

    Krebs, Teri S; Johansen, Pål-Ørjan

    2012-07-01

    Assessments of lysergic acid diethylamide (LSD) in the treatment of alcoholism have not been based on quantitative meta-analysis. Hence, we performed a meta-analysis of randomized controlled trials in order to evaluate the clinical efficacy of LSD in the treatment of alcoholism. Two reviewers independently extracted the data, pooling the effects using odds ratios (ORs) by a generic inverse variance, random effects model. We identified six eligible trials, including 536 participants. There was evidence for a beneficial effect of LSD on alcohol misuse (OR, 1.96; 95% CI, 1.36-2.84; p = 0.0003). Between-trial heterogeneity for the treatment effects was negligible (I² = 0%). Secondary outcomes, risk of bias and limitations are discussed. A single dose of LSD, in the context of various alcoholism treatment programs, is associated with a decrease in alcohol misuse.

  15. d-Lysergic Acid Diethylamide (LSD) as a Model of Psychosis: Mechanism of Action and Pharmacology

    Science.gov (United States)

    De Gregorio, Danilo; Comai, Stefano; Posa, Luca; Gobbi, Gabriella

    2016-01-01

    d-Lysergic Acid Diethylamide (LSD) is known for its hallucinogenic properties and psychotic-like symptoms, especially at high doses. It is indeed used as a pharmacological model of psychosis in preclinical research. The goal of this review was to understand the mechanism of action of psychotic-like effects of LSD. We searched Pubmed, Web of Science, Scopus, Google Scholar and articles’ reference lists for preclinical studies regarding the mechanism of action involved in the psychotic-like effects induced by LSD. LSD’s mechanism of action is pleiotropic, primarily mediated by the serotonergic system in the Dorsal Raphe, binding the 5-HT2A receptor as a partial agonist and 5-HT1A as an agonist. LSD also modulates the Ventral Tegmental Area, at higher doses, by stimulating dopamine D2, Trace Amine Associate receptor 1 (TAAR1) and 5-HT2A. More studies clarifying the mechanism of action of the psychotic-like symptoms or psychosis induced by LSD in humans are needed. LSD’s effects are mediated by a pleiotropic mechanism involving serotonergic, dopaminergic, and glutamatergic neurotransmission. Thus, the LSD-induced psychosis is a useful model to test the therapeutic efficacy of potential novel antipsychotic drugs, particularly drugs with dual serotonergic and dopaminergic (DA) mechanism or acting on TAAR1 receptors. PMID:27886063

  16. d-Lysergic Acid Diethylamide (LSD) as a Model of Psychosis: Mechanism of Action and Pharmacology.

    Science.gov (United States)

    De Gregorio, Danilo; Comai, Stefano; Posa, Luca; Gobbi, Gabriella

    2016-11-23

    d-Lysergic Acid Diethylamide (LSD) is known for its hallucinogenic properties and psychotic-like symptoms, especially at high doses. It is indeed used as a pharmacological model of psychosis in preclinical research. The goal of this review was to understand the mechanism of action of psychotic-like effects of LSD. We searched Pubmed, Web of Science, Scopus, Google Scholar and articles' reference lists for preclinical studies regarding the mechanism of action involved in the psychotic-like effects induced by LSD. LSD's mechanism of action is pleiotropic, primarily mediated by the serotonergic system in the Dorsal Raphe, binding the 5-HT2A receptor as a partial agonist and 5-HT1A as an agonist. LSD also modulates the Ventral Tegmental Area, at higher doses, by stimulating dopamine D₂, Trace Amine Associate receptor 1 (TAAR₁) and 5-HT2A. More studies clarifying the mechanism of action of the psychotic-like symptoms or psychosis induced by LSD in humans are needed. LSD's effects are mediated by a pleiotropic mechanism involving serotonergic, dopaminergic, and glutamatergic neurotransmission. Thus, the LSD-induced psychosis is a useful model to test the therapeutic efficacy of potential novel antipsychotic drugs, particularly drugs with dual serotonergic and dopaminergic (DA) mechanism or acting on TAAR₁ receptors.

  17. From Psychiatry to Flower Power and Back Again: The Amazing Story of Lysergic Acid Diethylamide.

    Science.gov (United States)

    Mucke, Hermann A M

    2016-07-08

    Among the psychedelic drugs that enjoyed a period of popularity in psychiatric research during the 1950s and 1960s, lysergic acid diethylamide (LSD) is the most prominent one. Psychiatrists of that time had seen LSD not only as a tool for psychotherapy but also as a potential therapeutic for anxiety, depression, alcohol abuse, autism, and even schizophrenia. When it became a quasi-religious epitome of the Hippie counterculture in the mid 1960s, and cases of what we now call hallucinogen persisting perception disorder and acute psychotic "flashbacks" mounted, authorities moved to make LSD illegal. Although research was never actually forbidden, the field almost completely dried out until the early 2010s. Using today's tools of molecular pharmacology, functional imaging, and neuronal network theory, neuropsychiatry is now resurrecting LSD research-with implications that leave us with many medical and ethical questions. Few people are aware that this is a repurposed compound, originally developed in an effort to synthesize a new analeptic. On top of all potential LSD might have in psychiatry, it also serves as a reminder of the unexpected potential that discarded early-stage compounds can have.

  18. Acute Effects of Lysergic Acid Diethylamide on Circulating Steroid Levels in Healthy Subjects.

    Science.gov (United States)

    Strajhar, P; Schmid, Y; Liakoni, E; Dolder, P C; Rentsch, K M; Kratschmar, D V; Odermatt, A; Liechti, M E

    2016-03-01

    Lysergic acid diethylamide (LSD) is a serotonin 5-hydroxytryptamine-2A (5-HT2A ) receptor agonist that is used recreationally worldwide. Interest in LSD research in humans waned after the 1970s, although the use of LSD in psychiatric research and practice has recently gained increasing attention. LSD produces pronounced acute psychedelic effects, although its influence on plasma steroid levels over time has not yet been characterised in humans. The effects of LSD (200 μg) or placebo on plasma steroid levels were investigated in 16 healthy subjects using a randomised, double-blind, placebo-controlled, cross-over study design. Plasma concentration-time profiles were determined for 15 steroids using liquid-chromatography tandem mass-spectrometry. LSD increased plasma concentrations of the glucocorticoids cortisol, cortisone, corticosterone and 11-dehydrocorticosterone compared to placebo. The mean maximum concentration of LSD was reached at 1.7 h. Mean peak psychedelic effects were reached at 2.4 h, with significant alterations in mental state from 0.5 h to > 10 h. Mean maximal concentrations of cortisol and corticosterone were reached at 2.5 h and 1.9 h, and significant elevations were observed 1.5-6 h and 1-3 h after drug administration, respectively. LSD also significantly increased plasma concentrations of the androgen dehydroepiandrosterone but not other androgens, progestogens or mineralocorticoids compared to placebo. A close relationship was found between plasma LSD concentrations and changes in plasma cortisol and corticosterone and the psychotropic response to LSD, and no clockwise hysteresis was observed. In conclusion, LSD produces significant acute effects on circulating steroids, especially glucocorticoids. LSD-induced changes in circulating glucocorticoids were associated with plasma LSD concentrations over time and showed no acute pharmacological tolerance.

  19. Complex discriminative stimulus properties of (+)lysergic acid diethylamide (LSD) in C57Bl/6J mice.

    Science.gov (United States)

    Benneyworth, Michael A; Smith, Randy L; Barrett, Robert J; Sanders-Bush, Elaine

    2005-06-01

    The drug discrimination procedure is the most frequently used in vivo model of hallucinogen activity. Historically, most drug discrimination studies have been conducted in the rat. With the development of genetically modified mice, a powerful new tool has become available for investigating the mechanisms of drug-induced behavior. The current paper is part of an ongoing effort to determine the utility of the drug discrimination technique for evaluating hallucinogenic drugs in mice. To establish the training procedures and characterize the stimulus properties of (+)lysergic acid diethylamide (LSD) in mice. Using a two-lever drug discrimination procedure, C57Bl/6J mice were trained to discriminate 0.45 mg/kg LSD vs saline on a VI30 sec schedule of reinforcement, with vanilla-flavored Ensure serving as the reinforcer. As in rats, acquisition was orderly, but the training dose was nearly five-fold higher for mice than rats. LSD lever selection was dose-dependent. Time-course studies revealed a rapid loss of the LSD stimulus effects. The 5-HT(2A/2C) receptor agonist, 2,5-dimethoxy-4-bromoamphetamine [(-)DOB] (1.0 mg/kg), substituted fully for LSD and the 5-HT(1A) receptor agonist, 8-hydroxy-2-(di-n-propylamino)-tetralin (8-OH-DPAT) (1.6 mg/kg), substituted partially for LSD. Pretreatment with the 5-HT(2A) receptor-selective antagonist, MDL 100907, or the 5-HT(1A)-selective antagonist WAY 100635, showed that each antagonist only partially blocked LSD discrimination. Substitution of 1.0 mg/kg (-)DOB for LSD was fully blocked by pretreatment with MDL 100907 but unaltered by WAY 100635 pretreatment. These data suggest that in mice the stimulus effects of LSD have both a 5-HT(2A) receptor and a 5-HT(1A) receptor component.

  20. Agonist-directed signaling of serotonin 5-HT2C receptors: differences between serotonin and lysergic acid diethylamide (LSD).

    Science.gov (United States)

    Backstrom, J R; Chang, M S; Chu, H; Niswender, C M; Sanders-Bush, E

    1999-08-01

    For more than 40 years the hallucinogen lysergic acid diethylamide (LSD) has been known to modify serotonin neurotransmission. With the advent of molecular and cellular techniques, we are beginning to understand the complexity of LSD's actions at the serotonin 5-HT2 family of receptors. Here, we discuss evidence that signaling of LSD at 5-HT2C receptors differs from the endogenous agonist serotonin. In addition, RNA editing of the 5-HT2C receptor dramatically alters the ability of LSD to stimulate phosphatidylinositol signaling. These findings provide a unique opportunity to understand the mechanism(s) of partial agonism.

  1. Research on the Stability of Diethyl Hydroxylamine in Nitric Acid Medium

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    By the means of the comparison of the extraction of PU(Ⅲ,Ⅳ) and plutonium in the aqueous Phasecontaining salting-free agent, the stability of diethyl hydroxylamine in nitric acid medium is investigated.

  2. A review of lysergic acid diethylamide (LSD) in the treatment of addictions: historical perspectives and future prospects.

    Science.gov (United States)

    Liester, Mitchell B

    2014-01-01

    Lysergic acid diethylamide (LSD) is a semisynthetic compound with strong psychoactive properties. Chemically related to serotonin, LSD was initially hypothesized to produce a psychosislike state. Later, LSD was reported to have benefits in the treatment of addictions. However, widespread indiscriminate use and reports of adverse affects resulted in the classification of LSD as an illicit drug with no accepted medical use. This article reviews LSD's storied history from its discovery, to its use as a research tool, followed by its widespread association with the counterculture movement of the 1960s, and finally to its rebirth as a medicine with potential benefits in the treatment of addictions. LSD's pharmacology, phenomenology, effects at neurotransmitter receptors, and effects on patterns of gene expression are reviewed. Based upon a review of the literature, it is concluded that further research into LSD's potential as a treatment for addictions is warranted.

  3. Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Sklerov, J H; Kalasinsky, K S; Ehorn, C A

    1999-10-01

    A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

  4. From Hofmann to the Haight Ashbury, and into the future: the past and potential of lysergic acid diethlyamide.

    Science.gov (United States)

    Smith, David E; Raswyck, Glenn E; Davidson, Leigh Dickerson

    2014-01-01

    Since the discovery of its psychedelic properties in 1943, lysergic acid diethylamide (LSD) has been explored by psychiatric/therapeutic researchers, military/intelligence agencies, and a significant portion of the general population. Promising early research was halted by LSD's placement as a Schedule I drug in the early 1970s. The U.S. Army and CIA dropped their research after finding it unreliable for their purposes. NSDUH estimates that more than 22 million (9.1% of the population) have used LSD at least once in their lives. Recently, researchers have been investigating the therapeutic use of LSD and other psychedelics for end-of-life anxiety, post-traumatic stress disorder (PTSD), cancer, and addiction treatment. Adverse psychedelic reactions can be managed using talkdown techniques developed and in use since the 1960s.

  5. New Diethyl Ammonium Salt of Thiobarbituric Acid Derivative: Synthesis, Molecular Structure Investigations and Docking Studies

    OpenAIRE

    Assem Barakat; Abdullah Mohammed Al-Majid; Saied M. Soliman; Gehad Lotfy; Ghabbour, Hazem A; Hoong-Kun Fun; Abdul Wadood; Ismail Warad; Joseph C. Sloop

    2015-01-01

    The synthesis of the new diethyl ammonium salt of diethylammonium(E)-5-(1,5-bis(4-fluorophenyl)-3-oxopent-4-en-1-yl)-1,3-diethyl-4,6-dioxo-2-thioxohexaydropyrimidin-5-ide 3 via a regioselective Michael addition of N,N-diethylthiobarbituric acid 1 to dienone 2 is described. In 3, the carboanion of the thiobarbituric moiety is stabilized by the strong intramolecular electron delocalization with the adjacent carbonyl groups and so the reaction proceeds without any cyclization. The molecular stru...

  6. Safety and efficacy of lysergic acid diethylamide-assisted psychotherapy for anxiety associated with life-threatening diseases.

    Science.gov (United States)

    Gasser, Peter; Holstein, Dominique; Michel, Yvonne; Doblin, Rick; Yazar-Klosinski, Berra; Passie, Torsten; Brenneisen, Rudolf

    2014-07-01

    A double-blind, randomized, active placebo-controlled pilot study was conducted to examine safety and efficacy of lysergic acid diethylamide (LSD)-assisted psychotherapy in 12 patients with anxiety associated with life-threatening diseases. Treatment included drug-free psychotherapy sessions supplemented by two LSD-assisted psychotherapy sessions 2 to 3 weeks apart. The participants received either 200 μg of LSD (n = 8) or 20 μg of LSD with an open-label crossover to 200 μg of LSD after the initial blinded treatment was unmasked (n = 4). At the 2-month follow-up, positive trends were found via the State-Trait Anxiety Inventory (STAI) in reductions in trait anxiety (p = 0.033) with an effect size of 1.1, and state anxiety was significantly reduced (p = 0.021) with an effect size of 1.2, with no acute or chronic adverse effects persisting beyond 1 day after treatment or treatment-related serious adverse events. STAI reductions were sustained for 12 months. These results indicate that when administered safely in a methodologically rigorous medically supervised psychotherapeutic setting, LSD can reduce anxiety, suggesting that larger controlled studies are warranted.

  7. (+)Lysergic acid diethylamide, but not its nonhallucinogenic congeners, is a potent serotonin 5HT1C receptor agonist

    Energy Technology Data Exchange (ETDEWEB)

    Burris, K.D.; Breeding, M.; Sanders-Bush, E. (Department of Pharmacology, Vanderbilt University School of Medicine, Nashville, TN (United States))

    1991-09-01

    Activation of central serotonin 5HT2 receptors is believed to be the primary mechanism whereby lysergic acid diethylamide (LSD) and other hallucinogens induce psychoactive effects. This hypothesis is based on extensive radioligand binding and electrophysiological and behavioral studies in laboratory animals. However, the pharmacological profiles of 5HT2 and 5HT1C receptors are similar, making it difficult to distinguish between effects due to activation of one or the other receptor. For this reason, it was of interest to investigate the interaction of LSD with 5HT1C receptors. Agonist-stimulated phosphoinositide hydrolysis in rat choroid plexus was used as a direct measure of 5HT1C receptor activation. (+)LSD potently stimulated phosphoinositide hydrolysis in intact choroid plexus and in cultures of choroid plexus epithelial cells, with EC50 values of 9 and 26 nM, respectively. The effect of (+)LSD in both systems was blocked by 5HT receptor antagonists with an order of activity consistent with interaction at 5HT1C receptors. Neither (+)-2-bromo-LSD nor lisuride, two nonhallucinogenic congeners of LSD, were able to stimulate 5HT1C receptors in cultured cells or intact choroid plexus. In contrast, lisuride, like (+)LSD, is a partial agonist at 5HT2 receptors in cerebral cortex slices and in NIH 3T3 cells transfected with 5HT2 receptor cDNA. The present finding that (+)LSD, but not its nonhallucinogenic congeners, is a 5HT1C receptor agonist suggests a possible role for these receptors in mediating the psychoactive effects of LSD.

  8. Enzymatic synthesis of fatty acid ethyl esters by utilizing camellia oil soapstocks and diethyl carbonate.

    Science.gov (United States)

    Wang, Yingying; Cao, Xuejun

    2011-11-01

    This study was reported on a novel process for fatty acid ethyl esters preparation by transesterification and esterification from renewable low-cost feedstock camellia oil soapstocks and friendly acyl acceptor diethyl carbonate. The main components of product were 83.9% ethyl oleate, 8.9% ethyl palmitate, 4.7% ethyl linoleate and 2.1% ethyl stearate, which could be used as eco-friendly renewable resources or additives of industrial solvent and fossil fuel. The effects of molar ratio of diethyl carbonate to soapstocks oil, lipases, organic solvent, reaction temperature and time were investigated, and process conditions were optimized. The yield was up to 98.4% in solvent-free system with molar ratio of diethyl carbonate to soapstocks oil 3:1 and 5% Novozym 435 (based on the weight of soapstocks oil) at 50 °C and 180 rpm for 24 h. Moreover, there was no obvious loss in the yield after lipases were reused for 10 batches without treatment under optimized conditions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  9. Metabolism of lysergic acid diethylamide (LSD) to 2-oxo-3-hydroxy LSD (O-H-LSD) in human liver microsomes and cryopreserved human hepatocytes.

    Science.gov (United States)

    Klette, K L; Anderson, C J; Poch, G K; Nimrod, A C; ElSohly, M A

    2000-10-01

    The metabolism of lysergic acid diethylamide (LSD) to 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) was investigated in liver microsomes and cyropreserved hepatocytes from humans. Previous studies have demonstrated that O-H-LSD is present in human urine at concentrations 16-43 times greater than LSD, the parent compound. Additionally, these studies have determined that O-H-LSD is not generated during the specimen extraction and analytical processes or due to parent compound degradation in aqueous urine samples. However, these studies have not been conclusive in demonstrating that O-H-LSD is uniquely produced during in vivo metabolism. Phase I drug metabolism was investigated by incubating human liver microsomes and cryopreserved human hepatocytes with LSD. The reaction was quenched at various time points, and the aliquots were extracted using liquid partitioning and analyzed by liquid chromatography-mass spectrometry. O-H-LSD was positively identified in all human liver microsomal and human hepatocyte fractions incubated with LSD. In addition, O-H-LSD was not detected in any microsomal or hepatocyte fraction not treated with LSD nor in LSD specimens devoid of microsomes or hepatocytes. This study provides definitive evidence that O-H-LSD is produced as a metabolic product following incubation of human liver microsomes and hepatocytes with LSD.

  10. Advantages of analyzing postmortem brain samples in routine forensic drug screening—case series of three non-natural deaths tested positive for lysergic acid diethylamide (LSD)

    DEFF Research Database (Denmark)

    Mardal, Marie; Johansen, Sys Stybe; Thomsen, Ragnar

    2017-01-01

    Three case reports are presented, including autopsy findings and toxicological screening results, which were tested positive for the potent hallucinogenic drug lysergic acid diethylamide (LSD). LSD and its main metabolites were quantified in brain tissue and femoral blood, and furthermore hematoma...... and urine when available. LSD, its main metabolite 2-oxo-3-hydroxy-LSD (oxo-HO-LSD), and iso-LSD were quantified in biological samples according to a previously published procedure involving liquid-liquid extraction and ultra-high performance liquid chromatography − tandem mass spectrometry (UHPLC......-MS/MS). LSD was measured in the brain tissue of all presented cases at a concentration level from 0.34 −10.8 μg/kg. The concentration level in the target organ was higher than in peripheral blood. Additional psychoactive compounds were quantified in blood and brain tissue, though all below toxic concentration...

  11. Determination of lysergic acid diethylamide (LSD) in mouse blood by capillary electrophoresis/ fluorescence spectroscopy with sweeping techniques in micellar electrokinetic chromatography.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Chou, Shiu-Huey; Lin, Cheng-Huang

    2003-03-01

    The separation and on-line concentration of lysergic acid diethylamide (LSD) in mouse blood was achieved by means of capillary electrophoresis/fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as the surfactant. Techniques involving on-line sample concentration, including sweeping micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were applied; the optimum on-line concentration and separation conditions were determined. In the analysis of an actual sample, LSD was found in a blood sample from a test mouse (0.1 mg LSD fed to a 20 g mouse; approximately 1/10 to the value of LD(50)). As a result, 120 and 30 ng/mL of LSD was detected at 20 and 60 min, respectively, after ingestion of the doses.

  12. The hallucinogen d-lysergic acid diethylamide (d-LSD) induces the immediate-early gene c-Fos in rat forebrain.

    Science.gov (United States)

    Frankel, Paul S; Cunningham, Kathryn A

    2002-12-27

    The hallucinogen d-lysergic acid diethylamide (d-LSD) evokes dramatic somatic and psychological effects. In order to analyze the neural activation induced by this unique psychoactive drug, we tested the hypothesis that expression of the immediate-early gene product c-Fos is induced in specific regions of the rat forebrain by a relatively low, behaviorally active, dose of d-LSD (0.16 mg/kg, i.p.); c-Fos protein expression was assessed at 30 min, and 1, 2 and 4 h following d-LSD injection. A time- and region-dependent expression of c-Fos was observed with a significant increase (PLSD administration. These data demonstrate a unique pattern of c-Fos expression in the rat forebrain following a relatively low dose of d-LSD and suggest that activation of these forebrain regions contributes to the unique behavioral effects of d-LSD. Copyright 2002 Elsevier Science B.V.

  13. On-line identification of lysergic acid diethylamide (LSD) in tablets using a combination of a sweeping technique and micellar electrokinetic chromatography/77 K fluorescence spectroscopy.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2003-03-01

    This work describes a novel method for the accurate determination of lysergic acid diethylamide (LSD) in tablets. A technique involving sweeping-micellar electrokinetic chromatography (MEKC) was used for the initial on-line concentration and separation, after which a cryogenic molecular fluorescence experiment was performed at 77 K. Using this approach, not only the separation of LSD from the tablet extract was achieved, but on-line spectra were readily distinguishable and could be unambiguously assigned. The results are in agreement with analyses by gas chromatography-mass spectrometry (GC-MS). Thus, this method, which was found to be accurate, sensitive and rapid, has the potential for use as a reliable complementary method to GC-MS in such analyses.

  14. Kinetics and Mechanism of Oxidation of Diethyl Ether by Chloramine-T in Acidic Medium

    Directory of Open Access Journals (Sweden)

    Y. I. Hassan

    2012-01-01

    Full Text Available The kinetics of oxidation of diethyl ether (DE with sodium N-chloro-p-toluenesulphonamide (CAT in hydrochloric acid solution has been studied at (313°K.The reaction rate show a first order dependence on [CAT] and fractional order dependence on each [DE] and [H+] .The variation of ionic strength of the medium has no significant effect on the reaction rate , addition of p-toluenesulphonamide (p-TSA affects the reaction rate marginally the rate increased with decreasing dielectric constant of the medium , the stochiometry of the reaction was found to be 1:2 and oxidation products were identified , A Michaelis – Menten type mechanism has been suggested to explain the results.The equilibrium and the decomposition constants of CAT – diethyl ether complex have been evaluated. Thermodynamic parameters were computed by studying reaction at temperatures range ( 308 – 323°K for the rate limiting step and for the observed first order constants by the linear Arrhenius plot. The mechanism proposed and the derived rate law are consistent with observed kinetics.

  15. New Diethyl Ammonium Salt of Thiobarbituric Acid Derivative: Synthesis, Molecular Structure Investigations and Docking Studies

    Directory of Open Access Journals (Sweden)

    Assem Barakat

    2015-11-01

    Full Text Available The synthesis of the new diethyl ammonium salt of diethylammonium(E-5-(1,5-bis(4-fluorophenyl-3-oxopent-4-en-1-yl-1,3-diethyl-4,6-dioxo-2-thioxohexaydropyrimidin-5-ide 3 via a regioselective Michael addition of N,N-diethylthiobarbituric acid 1 to dienone 2 is described. In 3, the carboanion of the thiobarbituric moiety is stabilized by the strong intramolecular electron delocalization with the adjacent carbonyl groups and so the reaction proceeds without any cyclization. The molecular structure investigations of 3 were determined by single-crystal X-ray diffraction as well as DFT computations. The theoretically calculated (DFT/B3LYP geometry agrees well with the crystallographic data. The effect of fluorine replacement by chlorine atoms on the molecular structure aspects were investigated using DFT methods. Calculated electronic spectra showed a bathochromic shift of the π-π* transition when fluorine is replaced by chlorine. Charge decomposition analyses were performed to study possible interaction between the different fragments in the studied systems. Molecular docking simulations examining the inhibitory nature of the compound show an anti-diabetic activity with Pa (probability of activity value of 0.229.

  16. Return of the lysergamides. Part I: Analytical and behavioral characterization of 1-propionyl-d-lysergic acid diethylamide (1P-LSD)

    Science.gov (United States)

    Brandt, Simon D.; Kavanagh, Pierce V.; Westphal, Folker; Stratford, Alexander; Elliott, Simon P.; Hoang, Khoa; Wallach, Jason; Halberstadt, Adam L.

    2015-01-01

    1-Propionyl-d-lysergic acid diethylamide hemitartrate (1P-LSD) has become available as a ‘research chemical’ in form of blotters and powdered material. This non-controlled derivative of d-lysergic acid diethylamide (LSD) has previously not been described in the published literature despite being closely related to 1-acetyl-LSD (ALD-52), which was developed in the 1950s. This study describes the characterization of 1P-LSD in comparison with LSD using various chromatographic, mass spectrometric methods and nuclear magnetic resonance spectroscopy. An important feature common to LSD and other serotonergic hallucinogens is that they produce 5-HT2A-receptor activation and induce the head-twitch response (HTR) in rats and mice. In order to assess whether 1P-LSD displays LSD-like properties and activates the 5-HT2A receptor, male C57BL/6J mice were injected with vehicle (saline) or 1P-LSD (0.025–0.8 mg/kg, IP) and HTR assessed for 30 min using magnetometer coil recordings. It was found that 1P-LSD produced a dose-dependent increase in HTR counts, and that it had ~38% (ED50 = 349.6 nmol/kg) of the potency of LSD (ED50 = 132.8 nmol/kg). Furthermore, the HTR was abolished when 1P-LSD administration followed pre-treatment with the selective 5-HT2A receptor antagonist M100907 (0.1 mg/kg, SC), which confirms that the behavioral response is mediated by activation of the 5-HT2A receptor. These results indicate that 1P-LSD produces LSD-like effects in mice, consistent with its classification as a serotonergic hallucinogen. Nevertheless, the extent to which 1P-LSD might show psychoactive effects in humans similar to LSD remains to be investigated. PMID:26456305

  17. Return of the lysergamides. Part I: Analytical and behavioural characterization of 1-propionyl-d-lysergic acid diethylamide (1P-LSD).

    Science.gov (United States)

    Brandt, Simon D; Kavanagh, Pierce V; Westphal, Folker; Stratford, Alexander; Elliott, Simon P; Hoang, Khoa; Wallach, Jason; Halberstadt, Adam L

    2016-09-01

    1-Propionyl-d-lysergic acid diethylamide hemitartrate (1P-LSD) has become available as a 'research chemical' in the form of blotters and powdered material. This non-controlled derivative of d-lysergic acid diethylamide (LSD) has previously not been described in the published literature despite being closely related to 1-acetyl-LSD (ALD-52), which was developed in the 1950s. This study describes the characterization of 1P-LSD in comparison with LSD using various chromatographic and mass spectrometric methods, infrared and nuclear magnetic resonance spectroscopy. An important feature common to LSD and other serotonergic hallucinogens is that they produce 5-HT2A -receptor activation and induce the head-twitch response (HTR) in rats and mice. In order to assess whether 1P-LSD displays LSD-like properties and activates the 5-HT2A receptor, male C57BL/6 J mice were injected with vehicle (saline) or 1P-LSD (0.025-0.8 mg/kg, IP) and HTR assessed for 30 min using magnetometer coil recordings. It was found that 1P-LSD produced a dose-dependent increase in HTR counts, and that it had ~38% (ED50  = 349.6 nmol/kg) of the potency of LSD (ED50  = 132.8 nmol/kg). Furthermore, HTR was abolished when 1P-LSD administration followed pretreatment with the selective 5-HT2A receptor antagonist M100907 (0.1 mg/kg, SC), which was consistent with the concept that the behavioural response was mediated by activation of the 5-HT2A receptor. These results indicate that 1P-LSD produces LSD-like effects in mice, consistent with its classification as a serotonergic hallucinogen. Nevertheless, the extent to which 1P-LSD might show psychoactive effects in humans similar to LSD remains to be investigated. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

  18. Preparation of trimethylchlorosilane-modified acid vermiculites for removing diethyl phthalate from water.

    Science.gov (United States)

    Yu, Xu-biao; Wei, Chao-hai; Ke, Lin; Wu, Hai-zhen; Chai, Xin-sheng; Hu, Yun

    2012-03-01

    A hybrid organic-inorganic material based on vermiculite was prepared to remove diethyl phthalate (DEP) from aqueous solution. Natural vermiculite was activated with HCl to improve the specific surface area and was then modified by silanization using trimethylchlorosilane. Organovermiculite prepared by ion exchange with hexadecyl trimethylammonium bromide (HDTMAB) was also tested for comparison. The leaching of 2 mol L(-1) HCl at 80°C increased the specific surface area of vermiculite from 14.4 to 500.0m(2)g(-1), and the average pore-diameter was decreased from 7.90 nm to 2.75 nm. Fourier transform infrared spectroscopy (FTIR) spectra indicated that trimethysilyl groups were grafted covalently on the surface of acid vermiculites. The specific surface area of trimethylchlorosilane-modified acid vermiculites (TMAVs) (355.4 m(2) g(-1)) was much larger than that of organovermiculite (6.0 m(2) g(-1)). The isotherm adsorption experiments of DEP showed that TMAVs exhibited linear isotherms, suggesting that the uptake of DEP was controlled by partitioning mechanism. The maximal partition coefficient (K(d)) of TMAVs was 3.1 times higher than that of organovermiculite, implying that TMAVs had stronger organic affinity than organovermiculite. The results demonstrate that the adsorption capacity and mechanism of organoclays were controlled by the specific surface area and organic loading, whereas the length of alkyl chain of organic modifier was not the key factor.

  19. Electrochemical Polymerization of Carbazole in Acetic Acid Containing Boron Trifluoride Diethyl Etherate

    Institute of Scientific and Technical Information of China (English)

    MIAO,Hua-Ming; ZHANG,Hong-Lin; XU,Jing-Kun; FAN,Chang-Li; DONG,Bin; ZENG,Li-Qiang; ZHAO,Feng

    2008-01-01

    High-quality polycarbazole (PCz) films with an electrical conductivity of 10-2 S·cm-1 were synthesized elec-trochemically by direct anodic oxidation of carbazole in a novel mixed electrolyte of acetic acid containing 26% boron trifluoride diethyl etherate (BTDE) and 5% poly(ethylene glycol) with molar mass of 400 (by volume). The oxidation potential of carbazole in this medium was measured to be only 0.89 V vs. a saturated calomel electrode (SCE), which was much lower than that determined in acetonitrile containing 0.1mol·L-1 Bu4NBF4 (1.36 V vs. SCE). PCz films obtained from this medium showed good electrochemical behavior, good thermal stability, and were partly soluble in strong polar organic solvents such as dimethyl sulfoxide and tetrahydrofuran. The fluorescence spectra implied that PCz obtained from this medium was a good blue-light emitter. FT-IR, 1H NMR and theoretical studies showed that the polymerization of carbazole mainly occurred at the 3,6-positions. To the best of our knowledge, this is the first report on the electrosyntheses of conducting polymers in mixed electrolyte of acetic acid and BTDE.

  20. Antidepressive, anxiolytic, and antiaddictive effects of ayahuasca, psilocybin and lysergic acid diethylamide (LSD): a systematic review of clinical trials published in the last 25 years

    Science.gov (United States)

    dos Santos, Rafael G.; Osório, Flávia L.; Crippa, José Alexandre S.; Riba, Jordi; Zuardi, Antônio W.; Hallak, Jaime E. C.

    2016-01-01

    To date, pharmacological treatments for mood and anxiety disorders and for drug dependence show limited efficacy, leaving a large number of patients suffering severe and persistent symptoms. Preliminary studies in animals and humans suggest that ayahuasca, psilocybin and lysergic acid diethylamide (LSD) may have antidepressive, anxiolytic, and antiaddictive properties. Thus, we conducted a systematic review of clinical trials published from 1990 until 2015, assessing these therapeutic properties. Electronic searches were performed using the PubMed, LILACS, and SciELO databases. Only clinical trials published in peer-reviewed journals were included. Of these, 151 studies were identified, of which six met the established criteria. Reviewed studies suggest beneficial effects for treatment-resistant depression, anxiety and depression associated with life-threatening diseases, and tobacco and alcohol dependence. All drugs were well tolerated. In conclusion, ayahuasca, psilocybin and LSD may be useful pharmacological tools for the treatment of drug dependence, and anxiety and mood disorders, especially in treatment-resistant patients. These drugs may also be useful pharmacological tools to understand psychiatric disorders and to develop new therapeutic agents. However, all studies reviewed had small sample sizes, and half of them were open-label, proof-of-concept studies. Randomized, double-blind, placebo-controlled studies with more patients are needed to replicate these preliminary findings. PMID:27354908

  1. Effect of fluvoxamine on platelet 5-HT2A receptors as studied by [3H]lysergic acid diethylamide ([3H]LSD) binding in healthy volunteers.

    Science.gov (United States)

    Spigset, O; Mjörndal, T

    1997-09-01

    Alterations in platelet 5-HT2A receptor characteristics have been reported in major depression as well as in other psychiatric diseases, and some effort has been made to utilize platelet 5-HT2A receptor status as a biological correlate to antidepressant drug response. In order to investigate whether treatment with a selective serotonin reuptake inhibitor affects platelet 5-HT2A receptors, we have studied platelet [3H]lysergic acid diethylamide ([3H]LSD) binding in healthy subjects treated with fluvoxamine in increasing dosage once weekly for 4 weeks. After 1 week of fluvoxamine treatment (25 mg/day), both Bmax and Kd were significantly lower than before the start of the treatment (19.9 versus 25.5 fmol/mg protein, P = 0.005 for Bmax; 0.45 versus 0.93 nM, P = 0.006 for Kd). Bmax returned to baseline during week 2, whereas Kd was lower than the baseline value throughout the treatment period. After discontinuation of fluvoxamine treatment, there was a significant increase in Kd (0.50 nM before discontinuation vs. 1.14 nM after discontinuation; P = 0.001), but not in Bmax. The study demonstrates that fluvoxamine affects platelet 5-HT2A receptor status irrespective of underlying psychiatric disease, and that this effect is evident already after 1 week at a subtherapeutic fluvoxamine dose.

  2. Advantages of analyzing postmortem brain samples in routine forensic drug screening-Case series of three non-natural deaths tested positive for lysergic acid diethylamide (LSD).

    Science.gov (United States)

    Mardal, Marie; Johansen, Sys Stybe; Thomsen, Ragnar; Linnet, Kristian

    2017-09-01

    Three case reports are presented, including autopsy findings and toxicological screening results, which were tested positive for the potent hallucinogenic drug lysergic acid diethylamide (LSD). LSD and its main metabolites were quantified in brain tissue and femoral blood, and furthermore hematoma and urine when available. LSD, its main metabolite 2-oxo-3-hydroxy-LSD (oxo-HO-LSD), and iso-LSD were quantified in biological samples according to a previously published procedure involving liquid-liquid extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). LSD was measured in the brain tissue of all presented cases at a concentration level from 0.34-10.8μg/kg. The concentration level in the target organ was higher than in peripheral blood. Additional psychoactive compounds were quantified in blood and brain tissue, though all below toxic concentration levels. The cause of death in case 1 was collision-induced brain injury, while it was drowning in case 2 and 3 and thus not drug intoxication. However, the toxicological findings could help explain the decedent's inability to cope with brain injury or drowning incidents. The presented findings could help establish reference concentrations in brain samples and assist in interpretation of results from forensic drug screening in brain tissue. This is to the author's knowledge the first report of LSD, iso-LSD, and oxo-HO-LSD measured in brain tissue samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Antidepressive, anxiolytic, and antiaddictive effects of ayahuasca, psilocybin and lysergic acid diethylamide (LSD): a systematic review of clinical trials published in the last 25 years.

    Science.gov (United States)

    Dos Santos, Rafael G; Osório, Flávia L; Crippa, José Alexandre S; Riba, Jordi; Zuardi, Antônio W; Hallak, Jaime E C

    2016-06-01

    To date, pharmacological treatments for mood and anxiety disorders and for drug dependence show limited efficacy, leaving a large number of patients suffering severe and persistent symptoms. Preliminary studies in animals and humans suggest that ayahuasca, psilocybin and lysergic acid diethylamide (LSD) may have antidepressive, anxiolytic, and antiaddictive properties. Thus, we conducted a systematic review of clinical trials published from 1990 until 2015, assessing these therapeutic properties. Electronic searches were performed using the PubMed, LILACS, and SciELO databases. Only clinical trials published in peer-reviewed journals were included. Of these, 151 studies were identified, of which six met the established criteria. Reviewed studies suggest beneficial effects for treatment-resistant depression, anxiety and depression associated with life-threatening diseases, and tobacco and alcohol dependence. All drugs were well tolerated. In conclusion, ayahuasca, psilocybin and LSD may be useful pharmacological tools for the treatment of drug dependence, and anxiety and mood disorders, especially in treatment-resistant patients. These drugs may also be useful pharmacological tools to understand psychiatric disorders and to develop new therapeutic agents. However, all studies reviewed had small sample sizes, and half of them were open-label, proof-of-concept studies. Randomized, double-blind, placebo-controlled studies with more patients are needed to replicate these preliminary findings.

  4. Immunoassay screening of lysergic acid diethylamide (LSD) and its confirmation by HPLC and fluorescence detection following LSD ImmunElute extraction.

    Science.gov (United States)

    Grobosch, T; Lemm-Ahlers, U

    2002-04-01

    In all, 3872 urine specimens were screened for lysergic acid diethylamide (LSD) using the CEDIA DAU LSD assay. Forty-eight samples, mainly from psychiatric patients or drug abusers, were found to be LSD positive, but only 13 (27%) of these could be confirmed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) following immunoaffinity extraction (IAE). Additional analysis for LSD using the DPC Coat-a-Count RIA was performed to compare the two immunoassay screening methods. Complete agreement between the DPC RIA assay and HPLC-FLD results was observed at concentrations below a cutoff concentration of 500 pg/mL. Samples that were LSD positive in the CEDIA DAU assay but not confirmed by HPLC-FLD were also investigated for interfering compounds using REMEDI HS drug-profiling system. REMEDI HS analysis identified 15 compounds (parent drugs and metabolites) that are believed to cross-react in the CEDIA DAU LSD assay: ambroxol, prilocaine, pipamperone, diphenhydramine, metoclopramide, amitriptyline, doxepine, atracurium, bupivacaine, doxylamine, lidocaine, mepivacaine, promethazine, ranitidine, and tramadole. The IAE/HPLC-FLD combination is rapid, easy to perform and reliable. It can reduce costs when standard, rather than more advanced, HPLC equipment is used, especially for labs that perform analyses for LSD infrequently. The chromatographic analysis of LSD, nor-LSD, and iso-LSD is not influenced by any of the tested cross-reacting compounds even at a concentration of 100 ng/mL.

  5. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

  6. Thiol-functionalized copolymeric polyesters by lipase-catalyzed esterification and transesterification of 1,12-dodecanedioic acid and its diethyl ester, respectively, with 1-thioglycerol

    OpenAIRE

    Fehling, Eberhard; Bergander, Klaus; Klein, Erika; Weber, Nikolaus; Vosmann, Klaus

    2010-01-01

    Abstract Copolymeric polyoxoesters containing branched-chain methylenethiol functions, i.e., poly(1,12-dodecanedioic acid-co-1-thioglycerol) and poly(diethyl 1,12-dodecanedioate-co-1-thioglycerol), were formed by lipase-catalyzed polyesterification and polytransesterification of 1,12-dodecanedioic acid and diethyl 1,12-dodecanedioate, respectively, with 1-thioglycerol (3-mercaptopropane-1,2-diol) using immobilized lipase B from Candida antarctica (Novozym 435) in vacuo without dryi...

  7. Physicochemical and structural properties of glycerin gel prepared using glycyrrhizic acid diethyl ester.

    Science.gov (United States)

    Koga, Kenjiro; Kimura, Toshiyuki; Sakai, Kenichi; Kushida, Hiroshi; Yoshikawa, Nobuji

    2014-01-01

    Glycyrrhizic acid diethyl ester (GZ-DE) was developed as a prodrug of glycyrrhizic acid (GZ), a hepatitis therapeutic drug. We fortuitously found that GZ-DE gels with glycerin selectively while searching for a safe solvent with which to dissolve GZ-DE. Based on this gelation, the aim of this study was to investigate the preparation of the gel and study the rheology, physicochemical and structural properties of the glycerin gel by differential scanning calorimeter (DSC), capillary electrophoresis (CEP), nuclear magnetic resonance (NMR), and small angle X-ray scattering (SAXS). The glycerin gel was prepared by the addition of at least 2.0% w/w GZ-DE. This gel did not flow at room temperature. After mixing glycerin and GZ-DE, a gel was formed after 2 days at 25°C or 3 h at 60°C. Glycerin gel containing 2.4% w/w GZ-DE provided the following results: 1) The glycerin gel exhibited creep at a constant stress of less than 10 Pa, but it is a fragile gel, showing Newtonian flow at 10 Pa stress. 2) Dynamic viscoelastic measurements showed that the elastic modulus (G') exceeds the viscous modulus (G''), indicating that glycerin gel has solid-like properties. 3) DSC showed a significant difference between the glass transition temperature of glycerin and glycerin gel. 4) CEP did not reveal a new compound in the glycerin gel. 5) NMR confirmed that glycerin gel is a physical gel. 6) SAXS measurements revealed that the glycerin gel has an oval-shaped basic frame (119 nm long and 65 nm wide).

  8. Argyreia nervosa (Burm. f.): receptor profiling of lysergic acid amide and other potential psychedelic LSD-like compounds by computational and binding assay approaches.

    Science.gov (United States)

    Paulke, Alexander; Kremer, Christian; Wunder, Cora; Achenbach, Janosch; Djahanschiri, Bardya; Elias, Anderson; Schwed, J Stefan; Hübner, Harald; Gmeiner, Peter; Proschak, Ewgenij; Toennes, Stefan W; Stark, Holger

    2013-07-09

    The convolvulacea Argyreia nervosa (Burm. f.) is well known as an important medical plant in the traditional Ayurvedic system of medicine and it is used in numerous diseases (e.g. nervousness, bronchitis, tuberculosis, arthritis, and diabetes). Additionally, in the Indian state of Assam and in other regions Argyreia nervosa is part of the traditional tribal medicine (e.g. the Santali people, the Lodhas, and others). In the western hemisphere, Argyreia nervosa has been brought in attention as so called "legal high". In this context, the seeds are used as source of the psychoactive ergotalkaloid lysergic acid amide (LSA), which is considered as the main active ingredient. As the chemical structure of LSA is very similar to that of lysergic acid diethylamide (LSD), the seeds of Argyreia nervosa (Burm. f.) are often considered as natural substitute of LSD. In the present study, LSA and LSD have been compared concerning their potential pharmacological profiles based on the receptor binding affinities since our recent human study with four volunteers on p.o. application of Argyreia nervosa seeds has led to some ambiguous effects. In an initial step computer-aided in silico prediction models on receptor binding were employed to screen for serotonin, norepinephrine, dopamine, muscarine, and histamine receptor subtypes as potential targets for LSA. In addition, this screening was extended to accompany ergotalkaloids of Argyreia nervosa (Burm. f.). In a verification step, selected LSA screening results were confirmed by in vitro binding assays with some extensions to LSD. In the in silico model LSA exhibited the highest affinity with a pKi of about 8.0 at α1A, and α1B. Clear affinity with pKi>7 was predicted for 5-HT1A, 5-HT1B, 5-HT1D, 5-HT6, 5-HT7, and D2. From these receptors the 5-HT1D subtype exhibited the highest pKi with 7.98 in the prediction model. From the other ergotalkaloids, agroclavine and festuclavine also seemed to be highly affine to the 5-HT1D

  9. Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour - Determination by high-performance thin-layer chromatography-fluorescence detection.

    Science.gov (United States)

    Oellig, Claudia

    2017-07-21

    Ergot alkaloids are generally determined by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD) or mass selective detection, analyzing the individual compounds. However, fast and easy screening methods for the determination of the total ergot alkaloid content are more suitable, since for monitoring only the sum of the alkaloids is relevant. The herein presented screening uses lysergic acid amide (LSA) as chemical marker, formed from ergopeptine alkaloids, and ergometrine for the determination of the total ergot alkaloids in rye with high-performance thin-layer chromatography-fluorescence detection (HPTLC-FLD). An ammonium acetate buffered extraction step was followed by liquid-liquid partition for clean-up before the ergopeptine alkaloids were selectively transformed to LSA and analyzed by HPTLC-FLD on silica gel with isopropyl acetate/methanol/water/25% ammonium hydroxide solution (80:10:3.8:1.1, v/v/v/v) as the mobile phase. The enhanced native fluorescence of LSA and unaffected ergometrine was used for quantitation without any interfering matrix. Limits of detection and quantitation were 8 and 26μg LSA/kg rye, which enables the determination of the total ergot alkaloids far below the applied quality criterion limit for rye. Close to 100% recoveries for different rye flours at relevant spiking levels were obtained. Thus, reliable results were guaranteed, and the fast and efficient screening for the total ergot alkaloids in rye offers a rapid alternative to the HPLC analysis of the individual compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Lysergic acid diethylamide (LSD) is a partial agonist of D2 dopaminergic receptors and it potentiates dopamine-mediated prolactin secretion in lactotrophs in vitro.

    Science.gov (United States)

    Giacomelli, S; Palmery, M; Romanelli, L; Cheng, C Y; Silvestrini, B

    1998-01-01

    The hallucinogenic effects of lysergic acid diethylamide (LSD) have mainly been attributed to the interaction of this drug with the serotoninergic system, but it seems more likely that they are the result of the complex interactions of the drug with both the serotoninergic and dopaminergic systems. The aim of the present study was to investigate the functional actions of LSD at dopaminergic receptors using prolactin secretion by primary cultures of rat pituitary cells as a model. LSD produced a dose-dependent inhibition of prolactin secretion in vitro with an IC50 at 1.7x10(-9) M. This action was antagonized by spiperone but not by SKF83566 or cyproheptadine, which indicates that LSD has a specific effect on D2 dopaminergic receptors. The maximum inhibition of prolactin secretion achieved by LSD was lower than that by dopamine (60% versus 80%). Moreover, the fact that LSD at 10(-8)-10(-6) M antagonized the inhibitory effect of dopamine (10(-7) M) and bromocriptine (10(-11) M) suggests that LSD acts as a partial agonist at D2 receptors on lactotrophs in vitro. Interestingly, LSD at 10(-13)-10(-10) M, the concentrations which are 10-1000-fold lower than those required to induce direct inhibition on pituitary prolactin secretion, potentiated the dopamine (10(-10)-2.5x10(-9) M)-mediated prolactin secretion by pituitary cells in vitro. These results suggest that LSD not only interacts with dopaminergic receptors but also has a unique capacity for modulating dopaminergic transmission. These findings may offer new insights into the hallucinogenic effect of LSD.

  11. Serotonergic and dopaminergic distinctions in the behavioral pharmacology of (±)-1-(2,5-dimethoxy-4-iodophenyl)-2-aminopropane (DOI) and lysergic acid diethylamide (LSD).

    Science.gov (United States)

    Schindler, Emmanuelle A D; Dave, Kuldip D; Smolock, Elaine M; Aloyo, Vincent J; Harvey, John A

    2012-03-01

    After decades of social stigma, hallucinogens have reappeared in the clinical literature demonstrating unique benefits in medicine. The precise behavioral pharmacology of these compounds remains unclear, however. Two commonly studied hallucinogens, (±)-1-(2,5-dimethoxy-4-iodophenyl)-2-aminopropane (DOI) and lysergic acid diethylamide (LSD), were investigated both in vivo and in vitro to determine the pharmacology of their behavioral effects in an animal model. Rabbits were administered DOI or LSD and observed for head bob behavior after chronic drug treatment or after pretreatment with antagonist ligands. The receptor binding characteristics of DOI and LSD were studied in vitro in frontocortical homogenates from naïve rabbits or ex vivo in animals receiving an acute drug injection. Both DOI- and LSD-elicited head bobs required serotonin(2A) (5-HT(2A)) and dopamine(1) (D(1)) receptor activation. Serotonin(2B/2C) receptors were not implicated in these behaviors. In vitro studies demonstrated that LSD and the 5-HT(2A/2C) receptor antagonist, ritanserin, bound frontocortical 5-HT(2A) receptors in a pseudo-irreversible manner. In contrast, DOI and the 5-HT(2A/2C) receptor antagonist, ketanserin, bound reversibly. These binding properties were reflected in ex vivo binding studies. The two hallucinogens also differed in that LSD showed modest D(1) receptor binding affinity whereas DOI had negligible binding affinity at this receptor. Although DOI and LSD differed in their receptor binding properties, activation of 5-HT(2A) and D(1) receptors was a common mechanism for eliciting head bob behavior. These findings implicate these two receptors in the mechanism of action of hallucinogens. Copyright © 2011 Elsevier Inc. All rights reserved.

  12. Detection of metabolites of lysergic acid diethylamide (LSD) in human urine specimens: 2-oxo-3-hydroxy-LSD, a prevalent metabolite of LSD.

    Science.gov (United States)

    Poch, G K; Klette, K L; Hallare, D A; Manglicmot, M G; Czarny, R J; McWhorter, L K; Anderson, C J

    1999-03-05

    Seventy-four urine specimens previously found to contain lysergic acid diethylamide (LSD) by gas chromatography-mass spectrometry (GC-MS) were analyzed by a new procedure for the LSD metabolite 2-oxo-3-hydroxy-LSD (O-H-LSD) using a Finnigan LC-MS-MS system. This procedure proved to be less complex, shorter to perform and provides cleaner chromatographic characteristics than the method currently utilized by the Navy Drug Screening Laboratories for the extraction of LSD from urine by GC-MS. All of the specimens used in the study screened positive for LSD by radioimmunoassay (Roche Abuscreen). Analysis by GC-MS revealed detectable amounts of LSD in all of the specimens. In addition, isolysergic diethylamide (iso-LSD), a byproduct of LSD synthesis, was quantitated in 64 of the specimens. Utilizing the new LC-MS-MS method, low levels of N-desmethyl-LSD (nor-LSD), another identified LSD metabolite, were detected in some of the specimens. However, all 74 specimens contained O-H-LSD at significantly higher concentrations than LSD, iso-LSD, or nor-LSD alone. The O-H-LSD concentration ranged from 732 to 112 831 pg/ml (mean, 16340 pg/ml) by quantification with an internal standard. The ratio of O-H-LSD to LSD ranged from 1.1 to 778.1 (mean, 42.9). The presence of O-H-LSD at substantially higher concentrations than LSD suggests that the analysis for O-H-LSD as the target analyte by employing LC-MS-MS will provide a much longer window of detection for the use of LSD than the analysis of the parent compound, LSD.

  13. 5-Hydroxytryptamine (serotonin)2A receptors in rat anterior cingulate cortex mediate the discriminative stimulus properties of d-lysergic acid diethylamide.

    Science.gov (United States)

    Gresch, Paul J; Barrett, Robert J; Sanders-Bush, Elaine; Smith, Randy L

    2007-02-01

    d-Lysergic acid diethylamide (LSD), an indoleamine hallucinogen, produces profound alterations in mood, thought, and perception in humans. The brain site(s) that mediates the effects of LSD is currently unknown. In this study, we combine the drug discrimination paradigm with intracerebral microinjections to investigate the anatomical localization of the discriminative stimulus of LSD in rats. Based on our previous findings, we targeted the anterior cingulate cortex (ACC) to test its involvement in mediating the discriminative stimulus properties of LSD. Rats were trained to discriminate systemically administered LSD (0.085 mg/kg s.c.) from saline. Following acquisition of the discrimination, bilateral cannulae were implanted into the ACC (AP, +1.2 mm; ML, +/-1.0 mm; DV, -2.0 mm relative to bregma). Rats were tested for their ability to discriminate varying doses of locally infused LSD (0.1875, 0.375, and 0.75 microg/side) or artificial cerebrospinal fluid (n = 3-7). LSD locally infused into ACC dose-dependently substituted for systemically administered LSD, with 0.75 microg/side LSD substituting completely (89% correct). Systemic administration of the selective 5-hydroxytryptamine (serotonin) (5-HT)(2A) receptor antagonist R-(+)-alpha-(2,3-dimethoxyphenyl)-1-[2-(4-fluorophenylethyl)]-4-piperidine-methanol (M100907; 0.4 mg/kg) blocked the discriminative cue of LSD (0.375 microg/side) infused into ACC (from 68 to 16% drug lever responding). Furthermore, M100907 (0.5 microg/microl/side) locally infused into ACC completely blocked the stimulus effects of systemic LSD (0.04 mg/kg; from 80 to 12% on the LSD lever). Taken together, these data indicate that 5-HT(2A) receptors in the ACC are a primary target mediating the discriminative stimulus properties of LSD.

  14. Repeated lysergic acid diethylamide in an animal model of depression: Normalisation of learning behaviour and hippocampal serotonin 5-HT2 signalling.

    Science.gov (United States)

    Buchborn, Tobias; Schröder, Helmut; Höllt, Volker; Grecksch, Gisela

    2014-06-01

    A re-balance of postsynaptic serotonin (5-HT) receptor signalling, with an increase in 5-HT1A and a decrease in 5-HT2A signalling, is a final common pathway multiple antidepressants share. Given that the 5-HT1A/2A agonist lysergic acid diethylamide (LSD), when repeatedly applied, selectively downregulates 5-HT2A, but not 5-HT1A receptors, one might expect LSD to similarly re-balance the postsynaptic 5-HT signalling. Challenging this idea, we use an animal model of depression specifically responding to repeated antidepressant treatment (olfactory bulbectomy), and test the antidepressant-like properties of repeated LSD treatment (0.13 mg/kg/d, 11 d). In line with former findings, we observe that bulbectomised rats show marked deficits in active avoidance learning. These deficits, similarly as we earlier noted with imipramine, are largely reversed by repeated LSD administration. Additionally, bulbectomised rats exhibit distinct anomalies of monoamine receptor signalling in hippocampus and/or frontal cortex; from these, only the hippocampal decrease in 5-HT2 related [(35)S]-GTP-gamma-S binding is normalised by LSD. Importantly, the sham-operated rats do not profit from LSD, and exhibit reduced hippocampal 5-HT2 signalling. As behavioural deficits after bulbectomy respond to agents classified as antidepressants only, we conclude that the effect of LSD in this model can be considered antidepressant-like, and discuss it in terms of a re-balance of hippocampal 5-HT2/5-HT1A signalling.

  15. [Optimization of alkaline hydrolysis based on the side chain of diethyl ester 4-amino-N(5)-formyl-N(8), N(10)-dideazatetrahydrofolic acid].

    Science.gov (United States)

    Yuan, M M; Wang, M; Liu, J Y; Zhang, Z L

    2017-08-18

    single ester hydrolysis product and amide bond hydrolysis product, but also improve the yield of the hydrolysis reaction. We have developed an efficient reaction for the hydrolysis of diethyl ester 4-amino-N(5)-formyl-N(8), N(10)-dideazatetrahydro. Since the final step of the synthesis of classical folic acid antagonists is always the catalyzed hydrolysis of the side chain glutamate, the reaction also has great significance for anti-folic acid anti-tumor inhibitors synthesis.

  16. Return of the lysergamides. Part II: Analytical and behavioural characterization of N(6) -allyl-6-norlysergic acid diethylamide (AL-LAD) and (2'S,4'S)-lysergic acid 2,4-dimethylazetidide (LSZ).

    Science.gov (United States)

    Brandt, Simon D; Kavanagh, Pierce V; Westphal, Folker; Elliott, Simon P; Wallach, Jason; Colestock, Tristan; Burrow, Timothy E; Chapman, Stephen J; Stratford, Alexander; Nichols, David E; Halberstadt, Adam L

    2017-01-01

    Lysergic acid N,N-diethylamide (LSD) is perhaps one of the most intriguing psychoactive substances known and numerous analogs have been explored to varying extents in previous decades. In 2013, N(6) -allyl-6-norlysergic acid diethylamide (AL-LAD) and (2'S,4'S)-lysergic acid 2,4-dimethylazetidide (LSZ) appeared on the 'research chemicals'/new psychoactive substances (NPS) market in both powdered and blotter form. This study reports the analytical characterization of powdered AL-LAD and LSZ tartrate samples and their semi-quantitative determination on blotter paper. Included in this study was the use of nuclear magnetic resonance (NMR) spectroscopy, gas chromatography-mass spectrometry (GC-MS), low and high mass accuracy electrospray MS(/MS), high performance liquid chromatography diode array detection and GC solid-state infrared analysis. One feature shared by serotonergic psychedelics, such as LSD, is the ability to mediate behavioural responses via activation of 5-HT2A receptors. Both AL-LAD and LSZ displayed LSD-like responses in male C57BL/6 J mice when employing the head-twitch response (HTR) assay. AL-LAD and LSZ produced nearly identical inverted-U-shaped dose-dependent effects, with the maximal responses occurring at 200 µg/kg. Analysis of the dose responses by nonlinear regression confirmed that LSZ (ED50  = 114.2 nmol/kg) was equipotent to LSD (ED50  = 132.8 nmol/kg) in mice, whereas AL-LAD was slightly less potent (ED50  = 174.9 nmol/kg). The extent to which a comparison in potency can be translated directly to humans requires further investigation. Chemical and pharmacological data obtained from NPS may assist research communities that are interested in various aspects related to substance use and forensic identification. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  17. 40 CFR 180.486 - Phosphorothioic acid, 0,0-diethyl 0-(1,2,2,2-tetrachloroethyl) ester; tolerances for residues.

    Science.gov (United States)

    2010-07-01

    ...,2,2,2-tetrachloroethyl) ester; tolerances for residues. 180.486 Section 180.486 Protection of...,2-tetrachloroethyl) ester; tolerances for residues. Tolerances are established permitting the residue of the insecticide phosphorothioic acid, 0,0-diethyl 0-(1,2,2,2-tetrachloroethyl) ester in or...

  18. 76 FR 23898 - Mefenpyr-diethyl; Pesticide Tolerances

    Science.gov (United States)

    2011-04-29

    ...-dihydro-5-methyl-1H-pyrazole-3,5- dicarboxylic acid, diethyl ester) and its dichlorophenyl-pyrazoline...,5- dihydro-5-methyl-1H-pyrazole-3,5-dicarboxylic acid, diethyl ester) and its dichlorophenyl...-pyrazole-3,5-dicarboxylic acid, diethyl ester) and its 2,4-dichlorophenyl-pyrazoline...

  19. Silane Reduction of 5-Hydroxy-6-methyl-pyridine-3,4-dicarboxylic Acid Diethyl Ester: Synthesis of Vitamin B6

    Directory of Open Access Journals (Sweden)

    Andrew G. Gum

    2003-12-01

    Full Text Available Alternative methods for the synthesis of pyridoxine have been investigated. The key intermediate, 5-hydroxy-6-methyl-pyridine-3,4-dicarboxylic acid diethyl ester (5, was reduced with either a silane monomer (MeSiH(OEt2 or a polysiloxane (polymethylhydrosiloxane, PMHS to afford crude pyridoxine. An isolation technique utilizing a commercially available resin was devised, affording the desired product, vitamin B6, in an overall yield of 38-54 % and a purity of 76%.

  20. ELECTROSYNTHESES OF FREE-STANDING POLY(THIOPHENE-3-ACETIC ACID) FILM IN MIXED ELECTROLYTES OF BORON TRIFLUORIDE DIETHYL ETHERATE AND TRIFLUOROACETIC ACID

    Institute of Scientific and Technical Information of China (English)

    Yu He; Wen-juan Guo; Mei-shan Pei; Guang-you Zhang

    2012-01-01

    High quality free-standing poly(thiophene-3-acetic acid) (PTAA),a water-soluble polythiophene derivative,was successfully electrosynthesized in boron trifluoride diethyl etherate (BFEE) + 25% (by volume) trifluoroacetic acid (TFA) at lower potential (0.38 V versus Pt).The carboxyl group makes PTAA highly soluble in water,facilitating its potential application as a blue-light-emitting material.PTAA films with conductivity of 7 S cm-1 obtained from this medium showed better redox activity and thermal stability.The structure and morphology of the polymer were studied by UV-Vis,FT-IR,1H-NMR spectra and scanning electron microscopy,respectively.

  1. Thiol-functionalized copolymeric polyesters by lipase-catalyzed esterification and transesterification of 1,12-dodecanedioic acid and its diethyl ester, respectively, with 1-thioglycerol.

    Science.gov (United States)

    Fehling, Eberhard; Bergander, Klaus; Klein, Erika; Weber, Nikolaus; Vosmann, Klaus

    2010-10-01

    Copolymeric polyoxoesters containing branched-chain methylenethiol functions, i.e., poly(1,12-dodecanedioic acid-co-1-thioglycerol) and poly(diethyl 1,12-dodecanedioate-co-1-thioglycerol), were formed by lipase-catalyzed polyesterification and polytransesterification of 1,12-dodecanedioic acid and diethyl 1,12-dodecanedioate, respectively, with 1-thioglycerol (3-mercaptopropane-1,2-diol) using immobilized lipase B from Candida antarctica (Novozym 435) in vacuo without drying agent in the reaction mixture. After 360-480 h, both polyoxoesters were purified by extraction from the reaction mixtures followed by solvent fractionation. The precipitate of poly(1,12-dodecanedioic acid-co-1-thioglycerol) demonstrated a M(W) of ~170,000 Da, whereas a M(W) of ~7,100 Da only was found for poly(diethyl 1,12-dodecanedioate-co-1-thioglycerol). Both polycondensates were analyzed by GPC/SEC, alkali-catalyzed transmethylation, NMR- and FTIR-spectrometry.

  2. Synthesis of novel 5-alkyl/aryl/heteroaryl substituted diethyl 3,4-dihydro-2H-pyrrole-4,4-dicarboxylates by aziridine ring expansion of 2-[(aziridin-1-yl-1-alkyl/aryl/heteroaryl-methylene]malonic acid diethyl esters

    Directory of Open Access Journals (Sweden)

    U. K. Syam Kumar

    2011-06-01

    Full Text Available A novel synthetic methodology has been developed for the synthesis of diethyl 5-alkyl/aryl/heteroaryl substituted 3,4-dihydro-2H-pyrrole-4,4-dicarboxylates (also called 2-substituted pyrroline-4,5-dihydro-3,3-dicarboxylic acid diethyl esters by iodide ion induced ring expansion of 2-[(aziridin-1-yl-1-alkyl/aryl/heteroaryl-methylene]malonic acid diethyl esters in very good to excellent yields under mild reaction conditions. The electronic and steric impact of the substituents on the kinetics of ring expansion of N-vinyl aziridines to pyrrolines has been studied. Various diversely substituted novel pyrroline derivatives have been synthesized by this methodology and the products can be used as key intermediates in the synthesis of substituted pyrrolines, pyrroles and pyrrolidines.

  3. Automated extraction of lysergic acid diethylamide (LSD) and N-demethyl-LSD from blood, serum, plasma, and urine samples using the Zymark RapidTrace with LC/MS/MS confirmation.

    Science.gov (United States)

    de Kanel, J; Vickery, W E; Waldner, B; Monahan, R M; Diamond, F X

    1998-05-01

    A forensic procedure for the quantitative confirmation of lysergic acid diethylamide (LSD) and the qualitative confirmation of its metabolite, N-demethyl-LSD, in blood, serum, plasma, and urine samples is presented. The Zymark RapidTrace was used to perform fully automated solid-phase extractions of all specimen types. After extract evaporation, confirmations were performed using liquid chromatography (LC) followed by positive electrospray ionization (ESI+) mass spectrometry/mass spectrometry (MS/MS) without derivatization. Quantitation of LSD was accomplished using LSD-d3 as an internal standard. The limit of quantitation (LOQ) for LSD was 0.05 ng/mL. The limit of detection (LOD) for both LSD and N-demethyl-LSD was 0.025 ng/mL. The recovery of LSD was greater than 95% at levels of 0.1 ng/mL and 2.0 ng/mL. For LSD at 1.0 ng/mL, the within-run and between-run (different day) relative standard deviation (RSD) was 2.2% and 4.4%, respectively.

  4. Serotonin 5-HT2A receptor binding in platelets from healthy subjects as studied by [3H]-lysergic acid diethylamide ([3H]-LSD): intra- and interindividual variability.

    Science.gov (United States)

    Spigset, O; Mjörndal, T

    1997-04-01

    In studies on platelet 5-HT2A receptor binding in patients with neuropsychiatric disorders, there has been a marked variability and a considerable overlap of values between patients and controls. The causes of the large variability in 5-HT2A receptor parameters is still unsettled. In the present study, we have quantified the intra- and interindividual variability of platelet 5-HT2A receptor binding in 112 healthy subjects and explored factors that may influence 5-HT2A receptor binding, using [3H]-lysergic acid diethylamide as radioligand. Age, gender, blood pressure, and metabolic capacity of the liver enzymes CYP2D6 and CYP2C19 did not influence Bmax and Kd values. Body weight and body mass index (BMI) showed a negative correlation with Kd (p = .04 and .03, respectively), but not with Bmax. Bmax was significantly lower in the light half of the year than in the dark half of the year (p = .001), and Kd was significantly lower in the fall than in the summer and winter (p < .001). In females, there was a significant increase in Bmax from week 1 to week 2 of the menstrual cycle (p = .03). Females taking contraceptive pills had significantly higher Kd than drug-free females in weeks 1 and 4 of the menstrual cycle (p = .04). This study shows that a number of factors should be taken into account when using platelet 5-HT2A receptor binding in studies of neuropsychiatric disorders.

  5. Reaction of 3-Amino-1,2,4-Triazole with Diethyl Phosphite and Triethyl Orthoformate: Acid-Base Properties and Antiosteoporotic Activities of the Products

    Directory of Open Access Journals (Sweden)

    Patrycja Miszczyk

    2017-02-01

    Full Text Available The reaction of diethyl phosphite with triethyl orthoformate and a primary amine followed by hydrolysis is presented, and the reaction was suitable for the preparation of (aminomethylenebisphosphonates. 3-Amino-1,2,4-triazole was chosen as an interesting substrate for this reaction because it possesses multiple groups that can serve as the amino component in the reaction—namely, the side-chain and triazole amines. This substrate readily forms 1,2,4-triazolyl-3-yl-aminomethylenebisphosphonic acid (compound 1 as a major product, along with N-ethylated bisphosphonates as side products. The in vitro antiproliferative effects of the synthesized aminomethylenebisphosphonic acids against J774E macrophages were determined. These compounds exhibit similar activity to zoledronic acid and higher activity than incadronic acid.

  6. Dimethyl and diethyl esters of 5,6-bis-(pyridin-2-yl)pyrazine-2,3-di-carb-oxy-lic acid: a comparison.

    Science.gov (United States)

    Alfonso, Montserrat; Stoeckli-Evans, Helen

    2016-02-01

    In dimethyl 5,6-bis-(pyridin-2-yl)pyrazine-2,3-di-carboxyl-ate, C18H14N4O4, (I), and diethyl 5,6-bis-(pyridin-2-yl)pyrazine-2,3-di-carboxyl-ate, C20H18N4O4, (II), the dimethyl and diethyl esters of 5,6-bis-(pyridin-2-yl)pyrazine-2,3-di-carb-oxy-lic acid, the orientation of the two pyridine rings differ. In (I), pyridine ring B is inclined to pyrazine ring A by 44.8 (2)° and the pyridine and pyrazine N atoms are trans to one another, while pyridine ring C is inclined to the pyrazine ring by 50.3 (2)°, with the pyridine and pyrazine N atoms cis to one another. In compound (II), the diethyl ester, which possesses twofold rotation symmetry, the pyridine ring is inclined to the pyrazine ring by 40.7 (1)°, with the pyridine and pyrazine N atoms trans to one another. In the crystal of (I), mol-ecules are linked by C-H⋯N hydrogen bonds, forming chains along [001]. The chains are linked by C-H⋯π inter-actions, forming a three-dimensional structure. In the crystal of (II), mol-ecules are linked via C-H⋯O hydrogen bonds, forming a three-dimensional framework. There are C-H⋯π inter-actions present within the framework.

  7. Phospholipase C mediates (±)-1-(2,5-dimethoxy-4-iodophenyl)-2-aminopropane (DOI)-, but not lysergic acid diethylamide (LSD)-elicited head bobs in rabbit medial prefrontal cortex.

    Science.gov (United States)

    Schindler, Emmanuelle A D; Harvey, John A; Aloyo, Vincent J

    2013-01-23

    The phenethylamine and indoleamine classes of hallucinogens demonstrate distinct pharmacological properties, although they share a serotonin(2A) (5-HT(2A)) receptor mechanism of action (MOA). The 5-HT(2A) receptor signals through phosphatidylinositol (PI) hydrolysis, which is initiated upon activation of phospholipase C (PLC). The role of PI hydrolysis in the effects of hallucinogens remains unclear. In order to better understand the role of PI hydrolysis in the MOA of hallucinogens, the PLC inhibitor, 1-[6-((17β-3-methoxyestra-1,3,5(10)-trien-17-yl)amino)hexyl]-1H-pyrrole-2,5-dione (U73122), was used to study the effects of two hallucinogens, the phenethylamine, (±)-1-(2,5-dimethoxy-4-iodophenyl)-2-aminopropane (DOI), and the indoleamine, lysergic acid diethylamide (LSD). PI hydrolysis was quantified through release of [3H]inositol-4-phosphate from living rabbit frontocortical tissue prisms. Head bobs were counted after hallucinogens were infused into the medial prefrontal cortex (mPFC) of rabbits. Both DOI and LSD stimulated PI hydrolysis in frontocortical tissue through activation of PLC. DOI-stimulated PI hydrolysis was blocked by 5-HT(2A/2C) receptor antagonist, ketanserin, whereas the LSD signal was blocked by 5-HT(2B/2C) receptor antagonist, SB206553. When infused into the mPFC, both DOI- and LSD-elicited head bobs. Pretreatment with U73122 blocked DOI-, but not LSD-elicited head bobs. The two hallucinogens investigated were distinct in their activation of the PI hydrolysis signaling pathway. The serotonergic receptors involved with DOI and LSD signals in frontocortical tissue were different. Furthermore, PLC activation in mPFC was necessary for DOI-elicited head bobs, whereas LSD-elicited head bobs were independent of this pathway. These novel findings urge closer investigation into the intracellular mechanism of action of these unique compounds. Published by Elsevier B.V.

  8. Adverse consequences of lysergic acid diethylamide.

    Science.gov (United States)

    Abraham, H D; Aldridge, A M

    1993-10-01

    The continued endemic use of hallucinogenic drugs, and of LSD in particular, raises concern regarding their short and long term adverse consequences. The epidemiology of LSD abuse is reviewed suggesting an increase in LSD use among the young as the prevalence rates for other substances continues to fall. Evidence supports the association of LSD use with panic reactions, prolonged schizoaffective psychoses and post-hallucinogen perceptual disorder, the latter being present continually for as long as 5 years. Evidence does not support claims of genetic disorders arising from hallucinogens. In light of the foregoing, current data confirm earlier findings of long lasting psychopathology arising in vulnerable individuals from the use of LSD. A hypothetical long term molecular mechanism of adverse effects is proposed.

  9. Development and validation of an LC-MS/MS method to quantify lysergic acid diethylamide (LSD), iso-LSD, 2-oxo-3-hydroxy-LSD, and nor-LSD and identify novel metabolites in plasma samples in a controlled clinical trial.

    Science.gov (United States)

    Dolder, Patrick C; Liechti, Matthias E; Rentsch, Katharina M

    2017-05-26

    Lysergic acid diethylamide (LSD) is a widely used recreational drug. The aim of this study was to develop and validate a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the quantification of LSD, iso-LSD, 2-oxo-3-hydroxy LSD (O-H-LSD), and nor-LSD in plasma samples from 24 healthy subjects after controlled administration of 100 μg LSD in a clinical trial. In addition, metabolites that have been recently described in in vitro studies, including lysergic acid monoethylamide (LAE), lysergic acid ethyl-2-hydroxyethylamide (LEO), 2-oxo-LSD, trioxylated-LSD, and 13/14-hydroxy-LSD, should be identified. Separation of LSD and its metabolites was achieved on a reversed phase chromatography column after turbulent-flow online extraction. For the identification and quantification, a triple-stage quadrupole LC-MS/MS instrument was used. The validation data showed slight matrix effects for LSD, iso-LSD, O-H-LSD, or nor-LSD. Mean intraday and interday accuracy and precision were 105%/4.81% and 105%/4.35% for LSD, 98.7%/5.75% and 99.4%/7.21% for iso-LSD, 106%/4.54% and 99.4%/7.21% for O-H-LSD, and 107%/5.82% and 102%/5.88% for nor-LSD, respectively. The limit of quantification was 0.05 ng/mL for LSD, iso-LSD, and nor-LSD and 0.1 ng/mL for O-H-LSD. The limit of detection was 0.01 ng/mL for all compounds. The method described herein was accurate, precise, and the calibration range within the range of expected plasma concentrations. LSD was quantified in the plasma samples of the 24 subjects of the clinical trial, whereas iso-LSD, O-H-LSD, nor-LSD, LAE, LEO, 13/14-hydroxy-LSD, and 2-oxo-LSD could only sporadically be detected but were too low for quantification. © 2017 Wiley Periodicals, Inc.

  10. Measurement of the Absolute Raman Cross Sections of Diethyl Phthalate, Dimethyl Phthalate, Ethyl Cinnamate, Propylene Carbonate, Tripropyl Phosphate, 1,3-Cyclohexanedione, 3’-Aminoacetophenone, 3’-Hydroxyacetophenone, Diethyl Acetamidomalonate, Isovanillin, Lactide, Meldrum’s Acid, p-Tolyl Sulfoxide, and Vanillin

    Science.gov (United States)

    2013-09-13

    Propylene Carbonate , Tripropyl Phosphate, 1,3-Cyclohexanedione, 3’-Aminoacetophenone, 3’-Hydroxyacetophenone, Diethyl Acetamidomalonate, Isovanillin...Cross Sections of Diethyl Phthalate, Dimethyl Phthalate, Ethyl Cinnamate, Propylene Carbonate , Tripropyl Phosphate, 1,3-Cyclohexanedione, 3...been determined for the Raman cross section σR of neat Diethyl phthalate (DEP), dimethyl phthalate (DMP), ethyl cinnamate (EC), propylene carbonate

  11. The quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) in human urine specimens, a metabolite of LSD: comparative analysis using liquid chromatography-selected ion monitoring mass spectrometry and liquid chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Poch, G K; Klette, K L; Anderson, C

    2000-04-01

    This paper compares the potential forensic application of two sensitive and rapid procedures (liquid chromatography-mass spectrometry and liquid chromatography-ion trap mass spectrometry) for the detection and quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) a major LSD metabolite. O-H-LSD calibration curves for both procedures were linear over the concentration range 0-8,000 pg/mL with correlation coefficients (r2) greater than 0.99. The observed limit of detection (LOD) and limit of quantitation (LOQ) for O-H-LSD in both procedures was 400 pg/mL. Sixty-eight human urine specimens that had previously been found to contain LSD by gas chromatography-mass spectrometry were reanalyzed by both procedures for LSD and O-H-LSD. These specimens contained a mean concentration of O-H-LSD approximately 16 times higher than the LSD concentration. Because both LC methods produce similar results, either procedure can be readily adapted to O-H-LSD analysis for use in high-volume drug-testing laboratories. In addition, the possibility of significantly increasing the LSD detection time window by targeting this major LSD metabolite for analysis may influence other drug-free workplace programs to test for LSD.

  12. 硫酸二乙酯酸值对123树脂固化的影响研究%Influence of Acid Value in Diethyl Sulfate on the Curing Process of 123 Resin

    Institute of Scientific and Technical Information of China (English)

    罗雪梅; 左玉芬; 黄黎明; 秦蛟

    2001-01-01

    The curing process of 123 resin was studied by means of microcalorimetry with diethyl sulfate as a curing agent. The results show that the acid value(greater than 1 percent) of diethyl sulfate has an effect on the curing rate and cured degree. When acid values of diethyl sulfates vary in a proper range(less than 1 percent),curing rate,cured degree and curing heat of 123 resin will not be affected.The curing mechanism of 123 resin was studied through FTIR technique. It shows that with the deepening of cured degree,the magnitude of characteristic peaks of CC at 1 651 cm-1 、CH2 at 3 095~3 075 cm-1 and 3 040~3 010 cm-1 attenuates sharply,indicating that the cross-link reaction takes place on the non-saturated double bond within the CC group for monomers Ⅰ and Ⅱ.%用微热量热法研究了用不同酸值的硫酸二乙酯作固化剂时123树脂的固化过程,结果表明,酸值大于1%的硫酸二乙酯对123树脂的固化速率与固化反应深度有较大影响。当酸值小于1%时,固化的速率、深度和热效应基本不变。用FTIR研究了123树脂的固化机理,发现随着固化反应的加深,1 651 cm-1处的CC特征峰、3 095~3 075 cm-1和3 040~3 010 cm-1处的CH2特征峰强度明显减弱,表明交联反应发生在单体的不饱和双键处。

  13. Effect of diethyl ether on the biliary excretion of acetaminophen.

    Science.gov (United States)

    Watkins, J B; Siegers, C P; Klaassen, C D

    1984-10-01

    The biliary and renal excretion of acetaminophen and its metabolites over 8 hr was determined in rats exposed to diethyl ether by inhalation for 1 hr. Additional rats were anesthetized with urethane (1 g/kg ip) while control animals were conscious throughout the experiment (surgery was performed under hexobarbital narcosis: 150 mg/kg ip; 30-min duration). The concentration of UDP-glucuronic acid was decreased 80% in livers from ether-anesthetized rats but was not reduced in urethane-treated animals when compared to that in control rats. The concentration of reduced glutathione was not affected by either urethane or diethyl ether. Basal bile flow was not altered by the anesthetic agents. Bile flow rate after acetaminophen injection (100 mg/kg iv) was increased slightly over basal levels for 2 hr in hexobarbital-treated control rats, was unaltered in urethane-anesthetized animals, and was decreased throughout the 8-hr experiment in rats exposed to diethyl ether for 1 hr. In control and urethane-anesthetized animals, approximately 30-35% of the total acetaminophen dose (100 mg/kg iv) was excreted into bile in 8 hr, while only 16% was excreted in rats anesthetized with diethyl ether. Urinary elimination (60-70% of the dose) was not altered by exposure to ether. Separation of metabolites by reverse-phase high-pressure liquid chromatography showed that ether decreased the biliary elimination of unchanged acetaminophen and its glucuronide, sulfate, and glutathione conjugates by 47, 40, 49, and 73%, respectively, as compared to control rats. Excretion of unchanged acetaminophen and the glutathione conjugate into bile was depressed in urethane-anesthetized animals by 45 and 66%, respectively, whereas elimination of the glucuronide and sulfate conjugates was increased by 27 and 50%, respectively. These results indicate that biliary excretion is influenced by the anesthetic agent and that diethyl ether depresses conjugation with sulfate and glutathione as well as glucuronic

  14. Synthesis, Characterization, and Cytotoxicity of a Novel Gold(III Complex with O,O′-Diethyl Ester of Ethylenediamine-N,N′-Di-2-(4-MethylPentanoic Acid

    Directory of Open Access Journals (Sweden)

    Nebojša Pantelić

    2016-09-01

    Full Text Available A novel gold(III complex, [AuCl2{(S,S-Et2eddl}]PF6, ((S,S-Et2eddl = O,O′-diethyl ester of ethylenediamine-N,N′-di-2-(4-methylpentanoic acid was synthesized and characterized by IR, 1D (1H and 13C, and 2D (H,H-COSY and H,H-NOESY NMR spectroscopy, mass spectrometry, and elemental analysis. Density functional theory calculations confirmed that (R,R-N,N′ diastereoisomer was energetically the most stable isomer. In vitro antitumor action of ligand precursor [(S,S-H2Et2eddl]Cl2 and corresponding gold(III complex was determined against tumor cell lines: human adenocarcinoma (HeLa, human colon carcinoma (LS174, human breast cancer (MCF7, non-small cell lung carcinoma cell line (A549, and non-cancerous cell line human embryonic lung fibroblast (MRC-5 using microculture tetrazolium test (MTT assay. The results indicate that both ligand precursor and gold(III complex have showed very good to moderate cytotoxic activity against all tested malignant cell lines. The highest activity was expressed by [AuCl2{(S,S-Et2eddl}]PF6 against the LS174 cells, with IC50 value of 7.4 ± 1.2 µM.

  15. 活性炭负载磷钨酸催化合成丙二酸二乙酯的研究%Synthesis of Diethyl Malonate over Phosphotungstic Acid Catalytst Supported on Activated Carbon

    Institute of Scientific and Technical Information of China (English)

    樊亚娟

    2011-01-01

    文章以无水乙醇和丙二酸为原料,以活性炭负载磷钨酸催化剂在不同的条件下酯化合成丙二酸二乙酯。选用L9(33)正交表考察合成丙二酸二乙酯的最优化条件,数据表明醇酸比3.0∶1,活性炭负载磷钨酸0.75 g,反应时间为100 min,带水剂甲苯10 mL时酯化收率可达91.86%。同时研究了不同的反应时间、醇酸比和催化剂用量对酯化收率的影响,并考察了负载型磷钨酸催化剂的重复使用情况,效果较好。%In the paper,diethyl malonate was synthesized by ethanol and malonic acid as raw materials and phosphotungstic acid catalyst supported on activated carbon under different conditions.The table of L9(33) orthogonal was used to selected the optimum conditions.The result showed that when the condition was that the alkyd ratio was 3.0∶1,and the catalyst was 0.75 g,and the reaction time was 100 min,and aqueous toluene was 10 mL,the esterification rate reached to 91.86 %.It also studied the effection of different reaction time,alkyd ratio and the mass of catalyst on the esterification yield.In addition,it studied the reuse of this catalyst,and the data showed it worked well.

  16. Compound list: diethyl maleate [Open TG-GATEs

    Lifescience Database Archive (English)

    Full Text Available diethyl maleate DEM 00A05 ftp://ftp.biosciencedbc.jp/archive/open-tggates/LATEST/Human/in_vitro/diethyl_male...ate.Human.in_vitro.Liver.zip ftp://ftp.biosciencedbc.jp/archive/open-tggates/LATEST/Rat/in_vitro/diethyl_mal...eate.Rat.in_vitro.Liver.zip ftp://ftp.biosciencedbc.jp/archive/open-tggates/LATEST/Rat/in_vivo/Liver/Single/diethyl_maleate.Rat.in_vivo.Liver.Single.zip ...

  17. ELECTROCHEMICAL POLYMERIZATION OF 5-CYANOINDOLE IN MIXED ELECTROLYTES OF BORON TRIFLUORIDE DIETHYL ETHERATE AND DIETHYL ETHER

    Institute of Scientific and Technical Information of China (English)

    Jing-kun Xu; Wei-qiang Zhou; Jian Hou; Shou-zhi Pu; Jing-wu Wang; Liu-shui Yan

    2006-01-01

    High quality poly(5-cyanoindole) (P5CI) films were electrosynthesized by direct anodic oxidation of 5-cyanoindole on stainless steel sheet in the mixed electrolytes of boron trifluoride diethyl etherate (BFEE) and diethyl ether (EE) (by volume 1:1) + 0.05 mol L-1 Bu4NBF4. The film formed can be peeled off the electrode into freestanding films. The addition of EE into BFEE can improve the solubility of monomer. P5CI films obtained from this medium showed excellent electrochemical behavior with conductivity of 10-2 Scm-1. Structural studies showed that the polymerization of 5-cyanoindole occurred at the 2,3 position. As-formed P5CI films were thoroughly soluble in strong polar organic solvent dimethyl sulfoxide (DMSO) while partly soluble in tetrahydrofuran (THF) or acetone. Fluorescence spectral studies indicated that P5CI was a good blue-light emitter.

  18. Adsorption of diethyl phthalate ester to clay minerals.

    Science.gov (United States)

    Wu, Yanhua; Si, Youbin; Zhou, Dongmei; Gao, Juan

    2015-01-01

    Phthalate esters are a group of plasticizers, which have been widely detected in China's agricultural and industrial soils. In this study, batch adsorption experiments were conducted to investigate the environmental effects on the adsorption of diethyl phthalate ester (DEP) to clay minerals. The results showed that DEP adsorption isotherms were well fitted with the Freundlich model; the interlayer spacing of K(+) saturated montmorillonite (K-mont) was the most important adsorption area for DEP, and di-n-butyl ester (DnBP) was limited to intercalate into the interlayer of K-mont due to the bigger molecular size; there was no significant effect of pH and ionic strength on DEP adsorption to K-mont/Ca-mont, but to Na-mont clay. The adsorption to kaolinite was very limited. Data of X-ray diffraction and FTIR spectra further proved that DEP molecules could intercalate into K-/Ca-mont interlayer, and might interact with clay through H-bonding between carbonyl groups and clay adsorbed water. Coated humic acid on clay surface would enhance DEP adsorption at low concentration, but not at high concentration (eg. Ce>0.26 mM). The calculated adsorption enthalpy (ΔHobs) and adsorption isotherms at varied temperatures showed that DEP could be adsorbed easier as more adsorbed. This study implied that clay type, compound structure, exchangeable cation, soil organic matter and temperature played important roles in phthalate ester's transport in soil.

  19. Development of an extractive spectrophotometric method for estimation of uranium in ore leach solutions using 2-ethylhexyl phosphonic acid-mono-2-ethylhexyl ester (PC88A) and tri-n-octyl phosphine oxide (TOPO) mixture as extractant and 2-(5-bromo-2-pyridylozo)-5-diethyl aminophenol (Br-PADAP) as chromophore.

    Science.gov (United States)

    Biswas, Sujoy; Pathak, P N; Roy, S B

    2012-06-01

    An extractive spectrophotometric analytical method has been developed for the determination of uranium in ore leach solution. This technique is based on the selective extraction of uranium from multielement system using a synergistic mixture of 2-ethylhexyl phosphonic acid-mono-2-ethylhexyl ester (PC88A) and tri-n-octyl phosphine oxide (TOPO) in cyclohexane and color development from the organic phase aliquot using 2-(5-Bromo-2-pyridylazo)-5-diethyl aminophenol (Br-PADAP) as chromogenic reagent. The absorption maximum (λ(max)) for UO(2)(2+)-Br-PADAP complex in organic phase samples, in 64% (v/v) ethanol containing buffer solution (pH 7.8) and 1,2-cyclohexylenedinitrilotetraacetic acid (CyDTA) complexing agent, has been found to be at 576 nm (molar extinction coefficient, ɛ: 36,750 ± 240 L mol(-1)cm(-1)). Effects of various parameters like stability of complex, ethanol volume, ore matrix, interfering ions etc. on the determination of uranium have also been evaluated. Absorbance measurements as a function of time showed that colored complex is stable up to > 24h. Presence of increased amount of ethanol in colored solution suppresses the absorption of a standard UO(2)(2+)-Br-PADAP solution. Analyses of synthetic standard as well as ore leach a solution show that for 10 determination relative standard deviation (RSD) is ore leach solutions and results were compared with standard methods like inductively coupled plasma emission spectrometry (ICPAES). The determined values of uranium concentrations by these methods are within ± 2%. This method can be used to determine 2.5-250 μg mL(-1) uranium in ore leach solutions with high accuracy and precision.

  20. Proton and deuterium NMR experiments in zero field. [Perdeuterated p-demethoxybenzene, perdeuterated malonic acid, diethyl terephthalate-d4, nonadecane-2,2'-D2, sodium propionate-D2

    Energy Technology Data Exchange (ETDEWEB)

    Millar, J.M.

    1986-02-01

    High field solid-state NMR lineshapes suffer from inhomogeneous broadening since resonance frequencies are a function of molecular orientation. Time domain zero field NMR is a two-dimensional field-cycling technique which removes this broadening by probing the evolution of the spin system under zero applied field. The simplest version, the sudden transition experiment, induces zero field evolution by the sudden removal of the applied magnetic field. Theory and experimental results of this experiment and several variations using pulsed dc magnetic fuelds to initiate zero field evolution are presented. In particular, the pulsed indirect detection method allows detection of the zero field spectrum of one nuclear spin species via another (usually protons) by utilizing the level crossings which occur upon adiabatic demagnetization to zero field. Experimental examples of proton/deuteron systems are presented which demonstrate the method results in enhanced sensitivity relative to that obtained in sudden transition experiments performed directly on deuterium. High resolution /sup 2/H NQR spectra of a series of benzoic acid derivatives are obtained using the sudden transition and indirect detection methods. Librational oscillations in the water molecules of barium chlorate monohydrate are studied using proton and deuterium ZF experiments. 177 refs., 88 figs., 2 tabs.

  1. Diethyl Ether Production Process with Various Catalyst Type

    Directory of Open Access Journals (Sweden)

    Widayat

    2013-01-01

    Full Text Available Several H-zeolite and HZSM-5 catalysts was preparated and their characters have also been investigated. H-zeolit Catalyst was preparated from Natural Zeolite that obtained from Malang District and Gunung Kidul District. Diethyl ether was produced by Ethanol with concentration of 95%. This research use fixed bed reactor that 1 gram of catalyst as bed catalyst, atmospheric pressure and temperature 140oC as the operating condition. Ethanol vapor from vaporization tank was driven by 200 ml/min Nitrogen stream. The responds in this research is liquid product concentration; diethyl ether, ethanol, methanol and water concentration. The results showed that the largest ethanol conversion was produced by the use of 56.44% HZSM-5 and the largest yield of diethyl ether diethyl was produced by the use of alumina and H-zeolite catalyst. The larger ratio between natural zeolite with HCl solvent will produce the larger surface area of catalyst and ethanol conversion. The largest ethanol conversion was produced at reactan ratio 1:20.

  2. Derivatives of cardanol through the ene reaction with diethyl azodicarboxylate

    Science.gov (United States)

    Cardanol is an alkyl/alkenyl phenolic material obtained from cashew nut shell liquid (CNSL), which is a byproduct of cashew nut processing. In an effort to develop new uses, cardanol was derivatized for the first time with diethyl azodicarboxylate (DEAD) through the ene reaction. The reaction was fa...

  3. Atmospheric Oxidation Mechanisms for Diethyl Ether and its Oxidation Products, Ethyl Formate and Ethyl Acetate.

    Science.gov (United States)

    Orlando, J. J.; Tyndall, G. S.

    2006-12-01

    Carbon-containing compounds are present in the earth's atmosphere as the result of emissions from natural and anthropogenic sources. Their oxidation in the atmosphere, initiated by such oxidants as OH, ozone, and nitrate radicals, leads to potentially harmful secondary pollutants such as ozone, carbonyl species, organic acids and aerosols. Ethers and esters are two classes of compounds that contribute to the complex array of organic compounds found in anthropogenically-influenced air. Additional ester is present as a result of the oxidation of the ethers. In this paper, the oxidation of diethyl ether and its two main oxidation products, ethyl formate and ethyl acetate, are studied over ranges of temperature, oxygen partial pressure, and NOx concentration, using an environmental chamber / FTIR absorption technique. Major end-products (the esters from diethyl ether; organic acids and anhydrides from the esters) are quantified, and these data are interpreted in terms of the chemistry of the various alkoxy and peroxy radicals generated. Emphasis is placed on the effects of chemical activation on the behavior of the alkoxy radicals, as well as on a novel peroxy radical rearrangement that may contribute to the observed products of ether oxidation under some conditions. Finally, the data are used, in conjunction with data on similar species, to provide a general representation of ether and ester oxidation in the atmosphere.

  4. Reaction of Grignard Reagents with Diethyl Perfluoroacyl( 1-Cyanoethyl ) phosphonates. Synthesis of Perfluoroalkylated α, β-Unsaturated Nitriles with Predominant Z-Selectivity

    Institute of Scientific and Technical Information of China (English)

    SHEN,Yan-Chang(沈延昌); JIANG,Guo-Fang(江国防)

    2002-01-01

    Diethyl (1-cyanoethyl)phosphonate 1 was reacted with n-butyllithium in tetrahydrofuran ( THF ) at - 78 ℃ and the resulting carbanion 2 reacted with perfluoroalkanoic acid anhydride to afford perfluoroacylated phosphonate 3. Without isolation 3was attacked by Grognard reagents giving perfluoroalkylated α,β-unsaturated nitries in 46%-88% yields with high Zstereoselectivity(Z:E=89-62:11-38).

  5. The Photocatalysis of N,N-diethyl-m-toluamide (DEET) Using Dispersions of Degussa P-25 TiO2 Particles

    Science.gov (United States)

    The photocatalysis of N,N-diethyl-meta-toluamide (DEET) was examined using aqueous Degussa P-25 TiO2 dispersions and a 350 nm high pressure Hg lamp UV reactor. Various concentrations of humic acid (HA) were added to the photocatalytic sample matrix in order to simulat...

  6. Pyridinium 5-[(1,3-diethyl-6-hydroxy-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidin-5-yl(2-methoxyphenylmethyl]-1,3-diethyl-4,6-dioxo-2-thioxopyrimidin-5-ide

    Directory of Open Access Journals (Sweden)

    Abdullah Mohamed Asiri

    2009-08-01

    Full Text Available 1,3-Diethyl-2-thiobarbituric acid reacts with 2-anisaldehyde to form the Michael addition product 2-anisylbis(1,3-diethyl-2-thiobarbitur-5-ylmethanate, which crystallizes as the title pyridinium salt, C5H6N+·C24H29N4O5S2−, when it reacts with the pyridine used to catalyse the reaction. There are two independent ion pairs in the crystal structure. The anion features a methine C atom connected to three six-membered rings; one of the rings carries a hydroxy group, which engages in hydrogen bonding with the carbonyl group belonging to another ring. The monoclinic unit cell emulates an orthorhombic unit cell, and is a twin with a minor twin component of 35%.

  7. Effective utilization of B20 blend with diethyl ether and ethanol as oxygenated additives

    Directory of Open Access Journals (Sweden)

    Upadrasta-Satya Vara-Prasad

    2011-01-01

    Full Text Available In the recent times' fatty acid methyl ester popularly called as biodiesel has become more prominent alternate fuel for compression ignition engines based on a single fuel concept. Since, use of neat biodiesel on a large scale is raising certain difficulties and is being adopted in a blended form with petro-diesel fuel and B20 blend has become standardized. However, the HC and NOx emissions of B20 are still on the higher side. Present work aims at experimental evaluation of a single cylinder water-cooled diesel engine by adopting various proportions of ethanol and diethyl ether blends in order to improve performance and emission characteristics of B20 blend. Besides employing different amounts of ethanol and diethyl ether, simultaneous influence of injector nozzle hole size and fuel injection pressure are also investigated to arrive at an optimum configuration. Brake specific fuel consumption and hydrocarbon emissions values are lower with B20 and DEE 5 whereas B20 with DEE15 yielded lower NOx emissions. It is observed that addition of oxygenates have improved the combustion process and lower emissions are obtained. The present investigation revealed that blends with oxygenated additives having higher Cetane rating are superior to neat blend.

  8. THE CHARACTERISTIC RESPONSE OF POLYMERIZED METHYL ACRYLIC ACID PHOTONIC CRYSTAL AND ITS APPLICATION TO DETECTING DIETHYL-STILBESTROL%聚甲基丙烯酸反蛋白石光子晶体反应特性及其检测己烯雌酚的应用

    Institute of Scientific and Technical Information of China (English)

    周彩虹; 郭纯; 刘建青; 洪小迪; 柳明; 宁保安; 高志贤

    2013-01-01

    目的 制备聚甲基丙烯酸(PMAA)反蛋白石光子晶体,观察其在不同环境因素刺激下的反应特性,并初步尝试将己烯雌酚(DES)印迹的PMAA光子晶体应用于检测小分子DES,为此类传感器检测小分子提供新的技术.方法 制备DES印迹的PMAA反蛋白石光子晶体.首先采用垂直沉积法制备二氧化硅蛋白石光子晶体模板,通过向模板中灌入预聚合液聚合形成薄膜,再除去二氧化硅模板和目标分子,得到印迹的反蛋白石光子晶体.在光纤光谱仪下观察pH等环境因素对光子晶体反射峰信号的影响.在体积比1∶1的甲醇和水中检测DES.结果 环境因素溶剂乙醇、离子强度、温度对光子晶体的反射峰信号影响较大,pH对其基本没有影响;印迹光子晶体对DES有明显的吸附反应,检测范围为1~500 ng/ml.结论 制备的DES分子印迹反蛋白石光子晶体对环境因素刺激反应灵敏,并且能够检测微量的DES.%Objective To prepare polymerized methyl acrylic acid ( PMAA) photonic crystal, and to observe its characteristic response to different environmental factors, as well as to try to apply it to detecting diethyl-stilbestrol (DES) ,so as to provide a new method for this kind of sensor to detect small molecules. Methods A colloidal crystal template was prepared from monodisperse SiO2 nanospheres by vertical deposition method first. Then the precursors were infused into the void spaces of the SiO2 templates and aggregated at 60 ℃ for 4 h. The template and the imprinted DES were removed,and then molecularly imprinted photonic polymers were prepared. The effects of pH, concentration of ethanol, temperature, and ionic strength on this photonic crystal property were observed using a fiber-optic spectrometer. Finally, DES in the aqueous solution of ethanol ( 1 : 1) was detected. Results The environmental factors such as ethanol solvent,ionic strength, and temperature markedly affected the reflection peak signal

  9. Study of moving bed biofilm reactor in diethyl phthalate and diallyl phthalate removal from synthetic wastewater.

    Science.gov (United States)

    Ahmadi, Ehsan; Gholami, Mitra; Farzadkia, Mahdi; Nabizadeh, Ramin; Azari, Ali

    2015-05-01

    Phthalic acid esters have received significant attention over the last few years since they are considered as priority pollutants. In this study, effects of different operation conditions including hydraulic retention time, phthalates loading rates and aeration rate on process performance of moving bed biofilm reactor (MBBR) for removing diethyl phthalate (DEP) and diallyl phthalate (DAP) from synthetic wastewater was evaluated. In optimum conditions, 94.96% and 93.85% removal efficiency were achieved for DEP and DAP, respectively. Moreover, MBBR achieved to remove more than 92% of COD for both phthalates. The results showed that DEP had a higher biodegradation rate compared to DAP, according to the selected parameters such as half saturation constant, overall reaction rate and maximum specific growth rate. The Grau second order model found as the best model for predicting MBBR performance due to its high correlation coefficients and more conformity of its kinetic coefficients to the results.

  10. Hepatic blood flow determination. A comparison of 99mTc-diethyl-IDA and indocyanine green as hepatic blood flow indicators in man

    DEFF Research Database (Denmark)

    Henriksen, Jens Henrik Sahl; Winkler, K

    1987-01-01

    99mTc-diethyl-acetanilide-iminodiacetic acid (IDA) was compared with indocyanine green (ICG) as an indicator of hepatic blood flow (HBF). Twelve subjects (8 with cirrhosis, 2 with fatty liver, one with pancreatitis, and one with intestinal angina) were studied during hepatic vein catheterization....... In 9 subjects the HBF measurements (indirect Fick-principle) were within 0.8-1.9 l/min, and no significant difference was observed between the values obtained by ICG and 99mTc-diethyl-IDA (mean 1.24 vs 1.26 l/min, P greater than 0.4). In 2 subjects with cirrhosis very high but almost identical values...... were found with the two indicators. In one subject ICG could not be measured in plasma because of hyperlipidaemia, but HBF was easily determined by 99mTc-diethyl-IDA. The results indicate that 99mTc-diethyl-IDA can be used as an indicator of HBF. This indicator is not superior to ICG in patients...

  11. Bis[diethyl(hydroxyammonium] benzene-1,4-dicarboxylate

    Directory of Open Access Journals (Sweden)

    De-Ming Xie

    2010-08-01

    Full Text Available In the centrosymmetric title compound, 2C4H12NO+·C8H4O42−, two N,N-diethyl(hydroxyammonium cations are linked to a benzene-1,4-dicarboxylate dianion by a combination of O—H...O and N—H...O hydrogen bonds, which can be described in graph-set terminology as R22(7. The crystal structure is further stabilized by C—H...O hydrogen bonds, leading to the fomation of a ribbon-like network.

  12. Long-term toxicity of diethyl carbonate in mice.

    Science.gov (United States)

    Brown, D; Gaunt, I F; Hardy, J; Kiss, I S; Butterworth, K R

    1978-07-01

    Groups of 48 male and 50 female mice were given drinking-water containing 0, 50, 250 or 1000 ppm diethyl carbonate for 83 weeks. There was no effect on mortality, rate of body-weight gain or the incidence of histopathological findings, including tumors. There were isolated differences between treated and control mice in the findings of the haematological examinations and in the liver weights of female mice but these were not considered to be related treatment. It is concluded that no carcinogenic effect could be detected and that the no-untoward-effect level is 1000 ppm (approx. 140 mg/kg/day).

  13. Convenient synthesis of β-allenic α-difluoromethylenephosphonic acid monoesters: Potential synthons for cyclic phosphate mimics

    Institute of Scientific and Technical Information of China (English)

    Yun Lin; Jin Tao Liu

    2007-01-01

    β-Allenic α-difluoromethylenephosphonic acid monoesters were prepared under mild conditions for the first time by hydrolyzing the corresponding diethyl phosphonates in aqueous sodium hydroxide solution.

  14. Diethyl Phthalate Causes Oxidative Stress: An in Vitro Study

    Directory of Open Access Journals (Sweden)

    Heena Prajapati

    2014-03-01

    Full Text Available Background: Phthalates are a group of multifunctional chemicals. Diethyl phthalate (DEP is one of the most frequently used phthalates in solvents and fixatives for numerous industrial products. Method: The present experiment was designed to assess oxidative stress, if any, caused by diethyl phthalate. For this the homogenates of liver and kidney were treated with different concentrations ( 10-40 µg/mL of DEP. 10% liver and kidney homogenates were prepared in phosphate buffered saline and used for estimation of lipid peroxidation.In final step lipid peroxidation and total protein content were analyzed. Results: The result revealed significant and dose - dependent increase in lipid peroxidation, whereas protein content reduced significantly. Maximum increase in LPO and decrease in protein content was observed at 40 µg/mL of DEP concentration. Conclusion: From this study, it can be concluded that different concentrations of DEP leads to dose- dependent significant increase in lipid peroxidation and decrease protein content.So at the different concentration of DEP cause oxidative stress.

  15. Experimental Analysis of Performance of Diesel Engine Using Kusum Methyl Ester With Diethyl Ether as Additive

    Directory of Open Access Journals (Sweden)

    Sandip S. Jawre,

    2014-05-01

    Full Text Available The fossile fuels are widely used in diesel engine and continually depleting with increasing consumption and prices day by day. The fatty acid methyl ester has become an effective alternative to diesel. Various types of vegetable oil such as Jatropha, karanja, cottonseed, neem, sunflower, palm, mahuva, coconut etc. can be used as fuel in diesel engine. Kusum oil is one of the fuel used in present work. The viscosity of kusum oil is very high, so it was reduced by Transesterification process. This study presents effect of diethyl ether as additive to biodiesel of kusum (schliechera oleosa methyl ester on the performance and emission of diesel engine at different load and constant speed and two different injection pressure (170 and 190 bar. From literature it was observed that very few studies had been conducted on use of neat biodiesel and diethyl ether blends and use of kusum methyl ester (KME in diesel engine found to be very less as compared to different biodiesel. Hence this topic was taken under study. The fuels and its blends used are 100% diesel, B100 (100% KME, BD-1 (95% KME, 5% DEE, BD-2 (90% KME, 10% DEE, BD-3 (85% KME, 15% DEE respectively. It was observed that the performance of engine increases at high injection pres-sure. The results indicate that lower BSFC was observed with BD-3 as compared to B100, BD-1 and BD-2. Brake thermal efficiency of BD-3 decreased at 170 bar injection pressure but it increase at 190 bar. Drastic re-duction in smoke is observed with all blends at higher engine loads. DEE addition to biodiesel reflects better engine performance compared to neat biodiesel.

  16. Methods for synthesizing diethyl carbonate from ethanol and supercritical carbon dioxide by one-pot or two-step reactions in the presence of potassium carbonate

    OpenAIRE

    Gasc, Fabien; Thiebaud-Roux, Sophie; Mouloungui, Zephirin

    2009-01-01

    Carbon dioxide sequestration was studied by synthesizing diethyl carbonate (DEC) from ethanol and CO2 under supercritical conditions in the presence of potassium carbonate as a base. The co-reagent was ethyl iodide or a concentrated strong acid. This sequestration reaction occurs in two steps, which were studied separately and in a one-pot reaction. An organic-inorganic carbonate hybrid, potassium ethyl carbonate (PEC) is generated at the end of the first step. This intermediate was character...

  17. 77 FR 15015 - Revocation of Tolerance Exemptions for Diethyl Phthalate and Methyl Ethyl Ketone; No Data Being...

    Science.gov (United States)

    2012-03-14

    ... AGENCY 40 CFR Part 180 Revocation of Tolerance Exemptions for Diethyl Phthalate and Methyl Ethyl Ketone... diethyl phthalate and methyl ethyl ketone when used as inert ingredients in pesticide products because... tolerance exemptions for residues of diethyl phthalate and methyl ethyl ketone in or on raw agricultural...

  18. Picosecond pulse radiolysis of the liquid diethyl carbonate.

    Science.gov (United States)

    Torche, Fayçal; El Omar, Abdel Karim; Babilotte, Philippe; Sorgues, Sébastien; Schmidhammer, Uli; Marignier, Jean-Louis; Mostafavi, Mehran; Belloni, Jacqueline

    2013-10-24

    The diethyl carbonate, DEC, is an ester that is used as a solvent in Li-ion batteries, but its behavior under ionizing radiation was unknown. The transient optical absorption spectra, the decay kinetics, and the influence of various scavengers have been studied by using the picosecond laser-triggered electron accelerator ELYSE. In neat DEC, the intense near-IR (NIR) absorption spectrum is assigned to the solvated electron. It is overlapped in the visible range by another transient but longer-lived and less intense band that is assigned to the oxidized radical DEC(-H). The solvated electron molar absorption coefficients and radiolytic yield evolution from 25 ps, the geminate recombination kinetics, and the rate constants of electron transfer reactions to scavengers are determined. The radiolytic mechanism, indicating a certain radioresistance of DEC, is compared with that for other solvents.

  19. Enhancement of pectinase production by ultraviolet irradiation and diethyl sulfate mutagenesis of a Fusarium oxysporum isolate.

    Science.gov (United States)

    Yin, L B; Zhang, C F; Xia, Q L; Yang, Y; Xiao, K; Zhao, L Z

    2016-09-23

    Fusarium oxysporum strain BM-201 was treated with ultraviolet (UV) radiation to obtain a high pectinase-producing strain. Mutant UV-10-41 was obtained and then treated by diethyl sulfate. Next, the mutant UV-diethyl sulfate-43 derived from UV-10-41 was selected as high pectinase-producing strain. Mutant UV-diethyl sulfate-43 was incubated on slant for 10 generations, demonstrating that the pectinase-producing genes were stable. Pectinase activity reached 391.2 U/mL, which is 73.6% higher than that of the original strain.

  20. Influence of the Functionalization Degree of Acidic Ion-Exchange Resins on Ethyl Octyl Ether Formation

    OpenAIRE

    Guilera, J.; Hanková, L. (Libuše); Jeřábek, K.; E Ramírez; Tejero, J.

    2014-01-01

    Ethyl octyl ether (EOE) can be obtained by the ethylation of 1-octanol by means of ethanol or diethyl carbonate over acidic ion-exchange resins. However, EOE formation has to compete with the less steric demanding formation of diethyl ether, by-product obtained from ethanol dehydration or diethyl carbonate decomposition. In the present work, the influence of the resin functionalization degree on EOE formation has been evaluated. A series of partially sulfonated resins were prepared by the sul...

  1. Direct Electrosynthesis and Characterization of a New Soluble Polythiophene Derivative Containing Carboxyl Groups in Boron Trifluoride Diethyl Etherate

    Science.gov (United States)

    He, Yu; Guo, Wenjuan; Pei, Meishan; Zhang, Guangyou; Jiang, Junzi

    2012-09-01

    High-quality poly(3-thiophenemalonic acid) (P3TMA), a water-soluble polythiophene derivative, was successfully electrosynthesized in boron trifluoride diethyl etherate + 50% (by volume) trifluoroacetic acid at lower potential (0.1 V versus Pt). The carboxyl groups make P3TMA highly soluble in water, facilitating its potential application as a blue-light-emitting material. P3TMA film with conductivity of 16 S cm-1 obtained from this medium showed better redox activity and thermal stability. The structure and morphology of the polymer were studied by ultraviolet-visible, Fourier-transform infrared, and nuclear magnetic resonance spectroscopy and scanning electron microscopy, respectively. To the best of our knowledge, this is the first report on electrosynthesis of P3TMA film.

  2. Synthesis of 0,0-diethyl-α-(p-toluenesulphonamido) phosphonates by Mannich-type reaction

    Institute of Scientific and Technical Information of China (English)

    陈茹玉; 戴庆; 张殿坤; 杨秀凤

    1995-01-01

    A series of O,O-diethyl-α-(p-toluenesulphonamido)phosphonates have been synthesized by theMannich-type reaction of p-toluenesulphonamide,substituted benzaldehydes and diethyl phosphite with acetylchloride as the solvent.The mechanism of the reaction is suggested,and the structures of new products areconfirmed by 1H NMR,31p NMR,elemental analysis and X-ray diffraction.The results of preliminarybioassay showed that some of them possess herbicidal activities.

  3. Photocatalytic Degradation of Diethyl Phthalate with Surfactant Addition

    Institute of Scientific and Technical Information of China (English)

    ZHANG Tianyong; HU Juan; ZHANG Youlan; LI Bin; FEI Xuening

    2006-01-01

    This paper studies the adsorption of diethyl phthalate (DEP,an environmental hormone) on the surface of nanoscale TiO2, effects of pH value of solutions, initial concentrations of DEP and additive surfactant on photocatalytic degradation and dynamics of DEP. Under ultra violet illumination, the interaction between DEP and surfactants including DBS (sodium dodecylbenzenesulfonate), CTAB (cetyltrimethylammonium bromide), and OP-10 (nonylphenol polyoxyethylene ether)was exploited from the perspective of degradation speed calculated by the data of high pressure liquid chromatography (HPLC) and UV-Vis spectra, respectively. Photocatalytic degradation of DEP followed pseudo first-order reaction kinetics. DEP as substrate degraded fast when its initial concentration was 130 mg/L. TiO2 had certain adsorption ability of DEP. TiO2 could adsorb the most DEP at the approximately neutral pH of 6.91. Degradation of DEP was not affected obviously by ad ditives OP-10 and JBS. Degradation rate of DEP was not enhanced greatly in the presence of surfactants, but degradation of DBS was sped up. Degradation rate of DEP was depressed in the presence of additive CTAB. The more CTAB was added, the less DEP was degraded. Degradation rate of CTAB became slow with the increase of initial CTAB concentration. The possible adsorption models among TiO2, DEP and surfactants were given.

  4. N,N-diethyl-m-toluamide transformation in river water.

    Science.gov (United States)

    Calza, P; Medana, C; Raso, E; Giancotti, V; Minero, C

    2011-09-01

    The paper deals with the aqueous environmental fate of N,N-diethyl-m-toluamide (DEET), one of the most widespread and efficient mosquito repellents. The investigation involved monitoring of the DEET decomposition and the identification of intermediate compounds. Initially, control experiments in the dark and under illumination were performed on sterilized and river water spiked with DEET, with the aim to simulate all possible transformation processes occurring in aquatic system. Under illumination, DEET was degraded and transformed into numerous organic intermediate compounds, 37 of which could be identified. Several isomeric species were formed and characterized by analysing MS and MS(n) spectra, and by comparison with parent molecule fragmentation pathways. These laboratory simulation experiments were verified in the field to check the mechanism previously supposed. River water was sampled and analysed at eight sampling points. Among the transformation products (TPs) identified in river water spiked with DEET, twelve of them were also found in natural river water. The transformation occurring in aquatic systems involved dealkylation, mono- and poly-hydroxylation followed by oxidation of the hydroxyl groups and cleavage of the alkyl chains. Two TPs were principally formed in dark condition, while the others are mainly produced through indirect photolysis processes mediated by natural photosensitizers. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Adsorptive removal of phthalate ester (Di-ethyl phthalate) from aqueous phase by activated carbon: a kinetic study.

    Science.gov (United States)

    Venkata Mohan, S; Shailaja, S; Rama Krishna, M; Sarma, P N

    2007-07-19

    Adsorptive studies were carried out on Di-ethyl phthalate (DEP) removal from aqueous phase onto activated carbon. Batch sorption studies were performed and the results revealed that activated carbon demonstrated ability to adsorb DEP. Influence of varying experimental conditions such as DEP concentration, pH of aqueous solution, and dosage of adsorbent were investigated on the adsorption process. Sorption interaction of DEP onto activated carbon obeyed the pseudo second order rate equation. Experimental data showed good fit with both the Langmuir and Freundlich adsorption isotherm models. DEP sorption was found to be dependent on the aqueous phase pH and the uptake was observed to be greater at acidic pH.

  6. An experimental and modeling study of diethyl carbonate oxidation

    KAUST Repository

    Nakamura, Hisashi

    2015-04-01

    Diethyl carbonate (DEC) is an attractive biofuel that can be used to displace petroleum-derived diesel fuel, thereby reducing CO2 and particulate emissions from diesel engines. A better understanding of DEC combustion characteristics is needed to facilitate its use in internal combustion engines. Toward this goal, ignition delay times for DEC were measured at conditions relevant to internal combustion engines using a rapid compression machine (RCM) and a shock tube. The experimental conditions investigated covered a wide range of temperatures (660-1300K), a pressure of 30bar, and equivalence ratios of 0.5, 1.0 and 2.0 in air. To provide further understanding of the intermediates formed in DEC oxidation, species concentrations were measured in a jet-stirred reactor at 10atm over a temperature range of 500-1200K and at equivalence ratios of 0.5, 1.0 and 2.0. These experimental measurements were used to aid the development and validation of a chemical kinetic model for DEC.The experimental results for ignition in the RCM showed near negative temperature coefficient (NTC) behavior. Six-membered alkylperoxy radical (RO˙2) isomerizations are conventionally thought to initiate low-temperature branching reactions responsible for NTC behavior, but DEC has no such possible 6- and 7-membered ring isomerizations. However, its molecular structure allows for 5-, 8- and 9-membered ring RO˙2 isomerizations. To provide accurate rate constants for these ring structures, ab initio computations for RO˙2⇌Q˙OOH isomerization reactions were performed. These new RO˙2 isomerization rate constants have been implemented in a chemical kinetic model for DEC oxidation. The model simulations have been compared with ignition delay times measured in the RCM near the NTC region. Results of the simulation were also compared with experimental results for ignition in the high-temperature region and for species concentrations in the jet-stirred reactor. Chemical kinetic insights into the

  7. 76 FR 17778 - Control of Ergocristine, a Chemical Precursor Used in the Illicit Manufacture of Lysergic Acid...

    Science.gov (United States)

    2011-03-31

    ... threshold for domestic and international transactions of ergocristine. As such, all transactions involving... microgram amounts are required to produce overt hallucinations. It induces a heightened awareness of sensory... threshold for domestic and import transactions of ergocristine pursuant to the provisions of 21 CFR 1310.04...

  8. 75 FR 8287 - Control of Ergocristine, a Chemical Precursor Used in the Illicit Manufacture of Lysergic Acid...

    Science.gov (United States)

    2010-02-24

    ... threshold for domestic and international transactions of ergocristine. As such, all transactions involving... 1960s. It induces a heightened awareness of sensory input that is accompanied by an enhanced sense of..., 1310, 1313, and 1316. This rulemaking does not propose the establishment of a threshold for domestic...

  9. Decreased mental time travel to the past correlates with default-mode network disintegration under lysergic acid diethylamide.

    Science.gov (United States)

    Speth, Jana; Speth, Clemens; Kaelen, Mendel; Schloerscheidt, Astrid M; Feilding, Amanda; Nutt, David J; Carhart-Harris, Robin L

    2016-04-01

    This paper reports on the effects of LSD on mental time travel during spontaneous mentation. Twenty healthy volunteers participated in a placebo-controlled crossover study, incorporating intravenous administration of LSD (75 μg) and placebo (saline) prior to functional magnetic resonance imaging (fMRI). Six independent, blind judges analysed mentation reports acquired during structured interviews performed shortly after the functional magnetic resonance imaging (fMRI) scans (approximately 2.5 h post-administration). Within each report, specific linguistic references to mental spaces for the past, present and future were identified. Results revealed significantly fewer mental spaces for the past under LSD and this effect correlated with the general intensity of the drug's subjective effects. No differences in the number of mental spaces for the present or future were observed. Consistent with the previously proposed role of the default-mode network (DMN) in autobiographical memory recollection and ruminative thought, decreased resting-state functional connectivity (RSFC) within the DMN correlated with decreased mental time travel to the past. These results are discussed in relation to potential therapeutic applications of LSD and related psychedelics, e.g. in the treatment of depression, for which excessive reflection on one's past, likely mediated by DMN functioning, is symptomatic.

  10. Photocatalytic Oxidation of Diethyl Sulfide Vapor over TiO2-Based Composite Photocatalysts

    Directory of Open Access Journals (Sweden)

    Dmitry Selishchev

    2014-12-01

    Full Text Available Composite TiO2/activated carbon (TiO2/AC and TiO2/SiO2 photocatalysts with TiO2 contents in the 10 to 80 wt. % range were synthesized by the TiOSO4 thermal hydrolysis method and characterized by AES, BET, X-ray diffraction and FT-IR ATR methods. All TiO2 samples were in the anatase form, with a primary crystallite size of about 11 nm. The photocatalytic activities of the TiO2/AC and TiO2/SiO2 samples were tested in the gas-phase photocatalytic oxidation (PCO reaction of diethyl sulfide (DES vapor in a static reactor by the FT-IR in situ method. Acetaldehyde, formic acid, ethylene and SO2 were registered as the intermediate products which finally were completely oxidized to the final oxidation products – H2O, CO2, CO and SO42− ions. The influence of the support on the kinetics of DES PCO and on the TiO2/AC and TiO2/SiO2 samples’ stability during three long-term DES PCO cycles was investigated. The highest PCO rate was observed for TiO2/SiO2 photocatalysts. To evaluate the activity of photocatalysts the turnover frequency values (TOF were calculated for three photocatalysts (TiO2, TiO2/AC and TiO2/SiO2 for the same amount of mineralized DES. It was demonstrated that the TOF value for composite TiO2/SiO2 photocatalysts was 3.5 times higher than for pure TiO2.

  11. Photocatalytic oxidation of diethyl sulfide vapor over TiO2-based composite photocatalysts.

    Science.gov (United States)

    Selishchev, Dmitry; Kozlov, Denis

    2014-12-19

    Composite TiO2/activated carbon (TiO2/AC) and TiO2/SiO2 photocatalysts with TiO2 contents in the 10 to 80 wt. % range were synthesized by the TiOSO4 thermal hydrolysis method and characterized by AES, BET, X-ray diffraction and FT-IR ATR methods. All TiO2 samples were in the anatase form, with a primary crystallite size of about 11 nm. The photocatalytic activities of the TiO2/AC and TiO2/SiO2 samples were tested in the gas-phase photocatalytic oxidation (PCO) reaction of diethyl sulfide (DES) vapor in a static reactor by the FT-IR in situ method. Acetaldehyde, formic acid, ethylene and SO2 were registered as the intermediate products which finally were completely oxidized to the final oxidation products - H2O, CO2, CO and SO42- ions. The influence of the support on the kinetics of DES PCO and on the TiO2/AC and TiO2/SiO2 samples' stability during three long-term DES PCO cycles was investigated. The highest PCO rate was observed for TiO2/SiO2 photocatalysts. To evaluate the activity of photocatalysts the turnover frequency values (TOF) were calculated for three photocatalysts (TiO2, TiO2/AC and TiO2/SiO2) for the same amount of mineralized DES. It was demonstrated that the TOF value for composite TiO2/SiO2 photocatalysts was 3.5 times higher than for pure TiO2.

  12. Species-dependent chelation of (241)Am by DTPA Di-ethyl ester.

    Science.gov (United States)

    Huckle, James E; Sadgrove, Matthew P; Mumper, Russell J; Jay, Michael

    2015-04-01

    Diethylenetriaminepentaacetic acid (DTPA) is an FDA-approved chelating agent for enhancing the elimination of transuranic elements such as americium from the body. Early access to therapy minimizes deposition of these radionuclides in tissues such as the bone. Due to its poor oral bioavailability, DTPA is administered as an IV injection, delaying access. Therefore, a diethyl-ester analog of DTPA, named C2E2, was synthesized as a means to increase oral absorption. As a hexadentate ligand, it was hypothesized that C2E2 was capable of binding americium directly. Therefore, the protonation constants and americium stability constant for C2E2 were determined by potentiometric titration and a solvent extraction method, respectively. C2E2 was shown to bind americium with a log K of 19.6. The concentrations of C2E2, its metabolite C2E1, and DTPA required to achieve effective binding in rat, beagle, and human plasma were studied in vitro. Dose response curves for each ligand were established, and the 50% maximal effective concentrations were determined for each species. As expected, higher concentrations of C2E2 were required to achieve the same degree of binding as DTPA. The results indicated that chelation in beagle plasma is more representative of the human response than rats. Finally, the pharmacokinetics of C2E2 were investigated in beagles, and the data was fit to a two-compartment model with elimination from the central compartment, along with first-order absorption. Based on the in vitro data, a 100 mg kg dose of C2E2 can be expected to have an effective duration of action of 3.8 h in beagles.

  13. Species-Dependent Chelation of 241Am by DTPA Di-ethyl Ester

    Science.gov (United States)

    Huckle, James E.; Sadgrove, Matthew P.; Mumper, Russell J.; Jay, Michael

    2014-01-01

    Diethylenetriaminepentaacetic acid (DTPA) is an FDA approved chelating agent for enhancing the elimination of transuranic elements such as americium from the body. Early access to therapy minimizes deposition of these radionuclides in tissues such as the bone. Due to its poor oral bioavailability, DTPA is administered as an IV injection, delaying access. Therefore a diethyl-ester analog of DTPA, named C2E2, was synthesized as a means to increase oral absorption. As a hexadentate ligand, it was hypothesized that C2E2 was capable of binding americium directly. Therefore, the protonation constants and americium stability constant for C2E2 were determined by potentiometric titration and a solvent extraction method, respectively. C2E2 was shown to bind americium with a log K of 19.6. The concentrations of C2E2, its metabolite C2E1, and DTPA required to achieve effective binding in rat, beagle, and human plasma were studied in vitro. Dose response curves for each ligand were established and the 50% maximal effective concentrations were determined for each species. As expected, higher concentrations of C2E2 were required to achieve the same degree of binding as DTPA. The results indicated that chelation in beagle plasma is more representative of the human response than rats. Finally, the pharmacokinetics of C2E2 were investigated in beagles and the data was fit to a two-compartment model with elimination from the central compartment, along with first-order absorption. Based on the in vitro data, a 100 mg kg−1 dose of C2E2 can be expected to have an effective duration of action of 3.8 hours in beagles. PMID:25706138

  14. Hydrolysis of Carbonyl Sulfide in Binary Mixture of Diethylene Glycol Diethyl Ether and Water

    Institute of Scientific and Technical Information of China (English)

    李新学; 刘迎新; 魏雄辉

    2005-01-01

    The solubility and hydrolysis of carbonyl sulfide in binary mixture of diethylene glycol diethyl ether and water are studied as a function of composition. The use of an aqueous solution of diethylene glycol diethyl ether enhances the solubility and hydrolysis rate of carbonyl sulfide compared with that in pure water. The composition of the mixture with maximum hydrolysis rate varies with temperature. The thermophysical properties including density, viscosity, and surface tension as a function of composition at 20℃ under atmospheric pressure as well as liquid-liquid equilibrium (LLE) data over the temperature range from 28℃ to 90℃ are also measured for the binary mixture.

  15. Synthesis and Crystal Structure of Diethyl-2,6-dimethyl-3,5-diyl-(1-(2-chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate)-pyridine

    Institute of Scientific and Technical Information of China (English)

    QIAN Qun; ZHANG Min; LI Zhi-Fen; CAO Wei-Guo; ZHANG Jun; SHAO Min; XIA Yi-Ben

    2008-01-01

    The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-(1-2(chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate) pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P, with a = 1.0342(11), b = 1.2211(12), c = 1.5013(15) nm, α = 82.5190(10), β = 85.7960(10), γ = 85.3150(10)°, V = 1.8697(3) nm3, Dc = 1.173 g/cm3, μ = 0.219 mm-1, F(000) = 684, Z = 2, the final R = 0.0720 and wR = 0.2211.

  16. Synthesis of Diethyl Oxalate by a Coupling-Regeneration Reaction of Carbon Monoxide

    Institute of Scientific and Technical Information of China (English)

    Fandong Meng; Genhui Xu; Baowei Wang; Xinbin Ma

    2002-01-01

    This article describes a process for the synthesis of diethyl oxalate by a coupling reaction ofcarbon monoxide, catalyzed by palladium in the presence of ethyl nitrite. The kinetics and mechanism ofthe coupling and regeneration reaction are also discussed. This paper presents the results of a scale-uptest of the catalyst and the process based on an a priori computer simulation.

  17. Thermal behavior of epoxidized cardanol diethyl phosphate as novel renewable plasticizer for poly(vinyl chloride)

    Science.gov (United States)

    A novel plasticizer, epoxidized cardanol diethyl phosphate (ECEP), based on cardanol was synthesized. Chemical structure of ECEP was characterized by fourier transform infrared (FTIR), 1H-nuclear magnetic resonance(1H NMR) and 13C-nuclear magnetic resonance(13C NMR) spectroscopy. Effects of ECEP sub...

  18. A diethyl phosphonate containing oxazoline: Synthesis and characterization of monomer and homopolymer

    Energy Technology Data Exchange (ETDEWEB)

    Hermes, R.E.; Thompson, R.D.; Valdez, L.S.

    1995-05-01

    A diethyl phosphonate oxazoline monomer and its polymer have been synthesized. The monomer appears to polymerize via a ring-opening mechanism giving the expected polyethyleneimine backbone with pendant carbonyl groups. Two distinct molecular weights were produced during polymerization suggesting two mechanisms of chain growth. Studies are underway to elucidate the reasons for this. This polymer has potential as a metal-chelating agent.

  19. THE DECOMPOSITION OF DIETHYL PEROXIDE IN THE PRESENCE OF NITRIC OXIDE AND ETHYL NITRITE

    Science.gov (United States)

    substantial amounts. Studies were made of the reactions of ethoxyl radicals (produced by the decomposition of diethyl peroxide at 181 deg C) with ethyl nitrite...and NO. The reaction rate between the ethoxyl radicals and NO was much greater than that between the radicals the nitrite.

  20. Endocrine stress response in rats subjected to singular orbital puncture while under diethyl-ether anaesthesia

    NARCIS (Netherlands)

    van Herck, H; Baumans, V; de Boer, S.F.; van der Gugten, J; van Woerkom, A B; Beynen, A C

    1991-01-01

    In an attempt to assess possible discomfort in rats subjected to orbital puncture while under diethyl-ether anaesthesia, their endocrine stress response was determined. Concentrations of corticosterone, adrenaline and noradrenaline were measured in plasma obtained via a jugular catheter from rats su

  1. Diluted isoflurane as a suitable alternative for diethyl ether for rat anaesthesia in regular toxicology studies.

    Science.gov (United States)

    Nagate, Toshiaki; Chino, Tomonobu; Nishiyama, Chizuru; Okuhara, Daisuke; Tahara, Toru; Maruyama, Yoshimasa; Kasahara, Hiroko; Takashima, Kayoko; Kobayashi, Sayaka; Motokawa, Yoshiyuki; Muto, Shin-ichi; Kuroda, Junji

    2007-11-01

    Despite its explosive properties and toxicity to both animals and humans, diethyl ether is an agent long used in Japan in the anaesthesia jar method of rat anaesthetises. However, in response to a recent report from the Science Council of Japan condemning diethyl ether as acceptable practice, we searched for an alternative rat anaesthesia method that provided data continuous with pre-existing regular toxicology studies already conducted under diethyl ether anaesthesia. For this, we examined two candidates; 30% isoflurane diluted with propylene glycol and pentobarbitone. Whereas isoflurane is considered to be one of the representatives of modern volatile anaesthetics, the method of propylene glycol-diluted 30% isoflurane used in this study was our modification of a recently reported method revealed to have several advantages as an inhalation anaesthesia. Intraperitoneal pentobarbitone has long been accepted as a humane method in laboratory animal anaesthesiology. These 2 modalities were scrutinized in terms of consistency of haematology and blood chemistry with previous results using ether. We found that pentobarbitone required a much longer induction time than diethyl ether, which is suspected to be the cause of fluctuations in several haematological and blood chemical results. Conversely, only calcium ion concentration showed a slight difference from traditional results in the case of 30% isoflurane. Additionally, serum prolactin and corticosterone levels indicated that 30% isoflurane induced less stress than ether, confirming that 30% isoflurane can both provide results consistent with diethyl ether, while at the same time remove its disadvantages. As such 30% isoflurane appears to be a strong alternative anaesthetic agent for future regular toxicology studies in Japan.

  2. Studies of the enzymic mechanism of the metabolism of diethyl 4-nitrophenyl phosphorothionate (parathion) by rat liver microsomes

    Science.gov (United States)

    Neal, R. A.

    1967-01-01

    1. The metabolism of parathion by rat liver microsomes is affected by various enzyme inhibitors in a manner quite typical of the `mixed-function oxidase' enzyme systems. 2. With many of these inhibitors (p-chloromercuribenzoate, Cu2+, 8-hydroxyquinoline) the conversion of parathion into diethyl hydrogen phosphorothionate is less inhibited than conversion into diethyl 4-nitrophenyl phosphate (paraoxon). 3. Compounds containing reduced sulphur stimulate the overall metabolism of parathion. However, the conversion of parathion into diethyl hydrogen phosphorothionate is stimulated more than its conversion into paraoxon. 4. The metabolism of parathion to diethyl hydrogen phosphorothionate is also stimulated by EDTA, Ca2+ and Ba2+, but these stimulatory effects are not additive. 5. The electron acceptors FAD, riboflavine, menadione and methylene blue exhibit a concentration-dependent differential inhibition of the metabolism of parathion to diethyl hydrogen phosphorothionate and to paraoxon. 6. The concentration of parathion required for the half-maximal rate of production of diethyl hydrogen phosphorothionate is significantly different from the concentration required for half-maximal rate of production of paraoxon. 7. The results are discussed in terms of either two separate enzyme systems metabolizing parathion to diethyl hydrogen phosphorothionate and to paraoxon or two different binding sites for parathion, which share a common electron-transport pathway. PMID:4964764

  3. Degradation mechanism of diethyl phthalate with electrogenerated hydroxyl radical on a Pd/C gas-diffusion electrode

    Energy Technology Data Exchange (ETDEWEB)

    Wang Hui, E-mail: wanghui616@gmail.com [College of Environmental Science and Engineering, Beijing Forestry University, Beijing 100083 (China); Sun Dezi [College of Environmental Science and Engineering, Beijing Forestry University, Beijing 100083 (China); Bian Zhaoyng, E-mail: bzy@mail.ipc.ac.cn [Key Laboratory of Photochemical Conversion and Optoelectronic Materials, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190 (China)

    2010-08-15

    Using a self-made Pd/C gas-diffusion electrode as the cathode and a Ti/IrO{sub 2}/RuO{sub 2} anode, the degradation of diethyl phthalate (DEP) has been investigated in an undivided electrolysis device by electrochemical oxidation processes. Hydroxyl radical (HO{center_dot}) was determined in the reaction mixture by the electron spin resonance spectrum (ESR). The result indicated that the Pd/C catalyst in Pd/C gas-diffusion electrode system accelerated the two-electron reduction of fed O{sub 2} to H{sub 2}O{sub 2}, which is in favor of producing HO{center_dot}. Additionally, the percentage removal of DEP and COD reached about 80.9 and 40.2% after 9 h electrolysis, respectively. It suggested that most of DEP were oxidized to intermediates using the Pd/C gas-diffusion electrode. Furthermore, the ratio of BOD{sub 5}/COD of resulted solutions was three times larger than the initial ones. Hence, the electrochemical oxidation enhanced the biodegradation character of the DEP solution. Finally, main aromatic intermediates (e.g., monoethyl phthalate (MEP) and phthalic acid (PA)) and main aliphatic carboxylic intermediates (e.g., formic, mesoxalic, oxalic, malonic, succinic, maleic, dodecanoic, and hexadecanoic acids) were identified by GC-MS. Moreover, a reaction scheme involving all these intermediates was proposed.

  4. Degradation mechanism of diethyl phthalate with electrogenerated hydroxyl radical on a Pd/C gas-diffusion electrode.

    Science.gov (United States)

    Wang, Hui; Sun, De-Zhi; Bian, Zhao-Yong

    2010-08-15

    Using a self-made Pd/C gas-diffusion electrode as the cathode and a Ti/IrO(2)/RuO(2) anode, the degradation of diethyl phthalate (DEP) has been investigated in an undivided electrolysis device by electrochemical oxidation processes. Hydroxyl radical (HO) was determined in the reaction mixture by the electron spin resonance spectrum (ESR). The result indicated that the Pd/C catalyst in Pd/C gas-diffusion electrode system accelerated the two-electron reduction of fed O(2) to H(2)O(2), which is in favor of producing HO. Additionally, the percentage removal of DEP and COD reached about 80.9 and 40.2% after 9h electrolysis, respectively. It suggested that most of DEP were oxidized to intermediates using the Pd/C gas-diffusion electrode. Furthermore, the ratio of BOD(5)/COD of resulted solutions was three times larger than the initial ones. Hence, the electrochemical oxidation enhanced the biodegradation character of the DEP solution. Finally, main aromatic intermediates (e.g., monoethyl phthalate (MEP) and phthalic acid (PA)) and main aliphatic carboxylic intermediates (e.g., formic, mesoxalic, oxalic, malonic, succinic, maleic, dodecanoic, and hexadecanoic acids) were identified by GC-MS. Moreover, a reaction scheme involving all these intermediates was proposed. Copyright 2010 Elsevier B.V. All rights reserved.

  5. Orally administered DTPA di-ethyl ester for decorporation of (241)Am in dogs: Assessment of safety and efficacy in an inhalation-contamination model.

    Science.gov (United States)

    Huckle, James E; Sadgrove, Matthew P; Pacyniak, Erik; Leed, Marina G D; Weber, Waylon M; Doyle-Eisele, Melanie; Guilmette, Raymond A; Agha, Bushra J; Susick, Robert L; Mumper, Russell J; Jay, Michael

    2015-07-01

    Currently two injectable products of diethylenetriaminepentaacetic acid (DTPA) are U.S. Food and Drug Administration (FDA)-approved for decorporation of (241)Am; however, an oral product is considered more amenable in a mass casualty situation. The di-ethyl ester of DTPA, named C2E2, is being developed as an oral drug for treatment of internal radionuclide contamination. Single-dose decorporation efficacy of C2E2 administered 24-h post contamination was determined in beagle dogs using a (241)Am nitrate inhalation contamination model. Single and multiple dose toxicity studies in beagle dogs were performed as part of an initial safety assessment program. In addition, the genotoxic potential of C2E2 was evaluated by the in vitro bacterial reverse mutation Ames test, mammalian cell chromosome aberration cytogenetic assay and an in vivo micronucleus test. Oral administration of C2E2 significantly increased (241)Am elimination over untreated controls and significantly reduced the retention of (241)Am in tissues, especially liver, kidney, lung and bone. Daily dosing of 200 mg/kg/day for 10 days was well tolerated in dogs. C2E2 was found to be neither mutagenic or clastogenic. The di-ethyl ester of DTPA (C2E2) was shown to effectively enhance the elimination of (241)Am after oral administration in a dog inhalation-contamination model and was well tolerated in toxicity studies.

  6. Orally Administered DTPA Di-ethyl Ester for Decorporation of 241Am in dogs: Assessment of Safety and Efficacy in an Inhalation-Contamination Model

    Science.gov (United States)

    Huckle, James E.; Sadgrove, Matthew P.; Pacyniak, Erik; Leed, Marina G. D.; Weber, Waylon M.; Doyle-Eisele, Melanie; Guilmette, Raymond A.; Agha, Bushra J.; Susick, Robert L.; Mumper, Russell J.; Jay, Michael

    2016-01-01

    Purpose Currently two injectable products of diethylenetriaminepentaacetic acid (DTPA) are U.S. Food and Drug Administration (FDA) approved for decorporation of 241Am, however, an oral product is considered more amenable in a mass casualty situation. The diethyl ester of DTPA, named C2E2, is being developed as an oral drug for treatment of internal radionuclide contamination. Materials and methods Single dose decorporation efficacy of C2E2 administered 24-hours post contamination was determined in beagle dogs using a 241Am nitrate inhalation contamination model. Single and multiple dose toxicity studies in beagle dogs were performed as part of an initial safety assessment program. In addition, the genotoxic potential of C2E2 was evaluated by the in vitro bacterial reverse mutation Ames test, mammalian cell chromosome aberration cytogenetic assay and an in vivo micronucleus test. Results Oral administration of C2E2 significantly increased 241Am elimination over untreated controls and significantly reduced the retention of 241Am in tissues, especially liver, kidney, lung and bone. Daily dosing of 200 mg/kg/day for 10 days was well tolerated in dogs. C2E2 was found to be neither mutagenic or clastogenic. Conclusions The di-ethyl ester of DTPA (C2E2) was shown to effectively enhance the elimination of 241Am after oral administration in a dog inhalation-contamination model and was well tolerated in toxicity studies. PMID:25912343

  7. Application of the Beauveria bassiana Strain for the Enantioselective Oxidation of the Diethyl 1-Hydroxy-1-Phenylmethanephosphonate

    OpenAIRE

    2010-01-01

    Biotransformation of diethyl 1-hydroxy-1-phenylmethanephosphonate using fungi Beauveria bassiana allowed resolving the racemic mixture of the substrate and due to the biocatalyst and reaction conditions modifications, leading to desired optical isomer.

  8. Experimental Analysis and Energetic Evaluation for Mahua Oil Methyl Ester with Diethyl Ether

    Directory of Open Access Journals (Sweden)

    Bhanu Pratap SINGH

    2014-11-01

    Full Text Available A theoretical method based on various existing process models has been developed for the performance evaluation of a compression ignition engine by using diesel and Mahua oil as an input fuel. Experimental evaluations of Mahua oil methyl ester/diesel along with diethyl ether were tested on a single cylinder naturally-aspirated indirect-injection diesel engine. The purpose of using diethyl ether with diesel/biodiesel is to control the emission from the diesel engine and to improve its performance. The effect of test fuels at different volumetric proportion and loads are also analyzed on the engine performance and emission. The comparisons of theoretical and experimental results are discussed. Engine performance characteristics predicted by this model are in closer approximation to that of experimental results. Engineering equation solver has been used to validate the model with the experimental results.

  9. Synthesis of Diethyl Oxalate by a Coupling—Regeneration Reaction of Carbon Monoxide

    Institute of Scientific and Technical Information of China (English)

    FandongMeng; GenhuiXu; 等

    2002-01-01

    This article describes a process for the synthesis of diethyl oxalate by a copling reaction of carbon monoxide,catalyzed by palladium in the presence of ethyl nitrite ,The kinetics and mechanism of the coupling and regeneration reaction are also discussed ,This paper presents the results of a scale-up test of the catalyst and the process based on an a priori computer simulation.

  10. A Novel Conformation Investigation on Newly Synthesized Compound of Diethyl Puerarin-7-yl Phosphate

    Institute of Scientific and Technical Information of China (English)

    YUAN Jin-Wei; CHEN Xiao-Lan; QU Ling-Bo; TANG Ming-Sheng; LIANG Rui-Ling; ZHAO Yu-Fen

    2006-01-01

    A novel compound, diethyl puerarin-7-yl phosphate, was synthesized through a simplified Atheron-Todd reaction for the first time. The structure of this compound was elucidated by IR, ESI-MS and NMR. Two conformations of the compound were testified by 2D NMR (HSQC and HMBC) and dynamic NMR. Furthermore, we carried out the conformational analysis using chemical calculation by the Gaussian 03. Finally, we obtained two preferred conformations and energy values.

  11. EFFECTS INDUCED BY DIETHYL SULPHATE ON SOME CYTOGENETICAL PARAMETERS AND LENGTH GROWTH OF HEMP PLANTLETS

    Directory of Open Access Journals (Sweden)

    Elena Truta

    2007-08-01

    Full Text Available The hemp seeds were treated with diethyl sulphate, in four concentrations (0.1%, 0.25%, 0.5%, and 1% and in two variants of alkylant exposure (3 and 6 hours. The length growth of plantlets, mitotic index and frequency of chromosomal aberrations were the analyzed parameters. Significant modifications were obtained at the level of parameters in variants treated with DES, comparatively with control.

  12. Conjugate addition of diethyl 1-fluoro-1-phenylsulfonylmethanephosphonate to α,β-unsaturated compounds.

    Science.gov (United States)

    Opekar, Stanislav; Pohl, Radek; Eigner, Václav; Beier, Petr

    2013-05-03

    Diethyl 1-fluoro-1-phenylsulfonylmethanephosphonate (1) in the presence of cesium carbonate undergoes efficient 1,4-addition to Michael acceptors having terminal double bonds such as α,β-unsaturated ketones, esters, sulfones, sulfoxides, and phosphonates to yield the corresponding adducts in good to excellent yields. In the presence of sodium hydride, 1 reacts with α,β-enones to provide γ-fluoro-γ-phenylsulfonylenol phosphates arising from 1,4-addition followed by phosphonate to phosphate rearrangement.

  13. Removal of the insect repellent N,N-diethyl-m-toluamide (DEET) by laccase-mediated systems.

    Science.gov (United States)

    Tran, Ngoc Han; Hu, Jiangyong; Urase, Taro

    2013-11-01

    Numerous efforts have been made to remove emerging trace organic contaminants, such as pharmaceuticals and personal care products (PPCPs). This study examined the removal of N,N-diethyl-m-toluamide (DEET) by Trametes versicolor laccase and its laccase-mediator systems. Experimental results showed that DEET was poorly removed by laccase alone. The poor removal efficiency of DEET by laccase may be attributed to the presence of strong withdrawing electron group (-CO-N [CH2-CH3]2) in the chemical structure of DEET. Experimental results also indicated that DEET might be indirectly oxidized by laccase-mediator systems. More than 50% initial DEET amount was removed by laccase in the presence of a redox mediator, such as 2,2'-azino-bis[3-ethylbenzothiazoline-6-sulphonic acid] (ABTS) or 1-hydroxybenzotriazole (HBT). However, laccase activity was considerably decreased in the presence of a redox mediator (ABTS or HBT). Further studies on identification of degradation byproducts and degradation pathways are recommended.

  14. Thermo-responsive, UV-active poly(phenyl acrylate-b-poly(diethyl acrylamide block copolymers

    Directory of Open Access Journals (Sweden)

    M. Maric

    2013-12-01

    Full Text Available The homopolymerization of phenyl acrylate (PA was investigated for the first time by nitroxide mediated polymerization (NMP with the succinimidyl form of the SG1-based unimolecular initiator 2-[N-tert-butyl-2,2-(dimethylpropyl-aminooxy]propionic acid (BlocBuilder MA. The control of PPA homopolymerization was improved by the use of 15 mol% additional free nitroxide SG1 ([tert-butyl[1-(diethoxyphosphoryl-2,2-dimethylpropyl]amino]oxidanyl and dispersities, Mw/Mn, of around 1.2 were achieved. A PPA homopolymer was then successfully chain-extended with diethyl acrylamide (DEAAm to form a block copolymer of PPA-b-PDEAAm where the PDEAAm segment is thermo-responsive, while the PPA block is potentially UV-active. The thermo-responsive behavior of the block copolymer in 0.5 wt% aqueous solution was studied by UV-Vis spectrometry and dynamic light scattering (DLS, indicating cloud point temperatures of 26–30°C, close to that reported for PDEAAm homopolymers.

  15. Effects of Subchronic Exposure to N,N-Diethyl-m-toluamide on Selected Biomarkers in Common Carp (Cyprinus carpio L.

    Directory of Open Access Journals (Sweden)

    Andrea Slaninova

    2014-01-01

    Full Text Available DEET (N,N-diethyl-m-toluamide is the most common active ingredient in the insect repellents commonly detected in European groundwater. The aim of this study was to investigate the effect of subchronic DEET exposure on biochemical and haematological parameters, antioxidant enzymes, including catalase, glutathione peroxidase, glutathione reductase, and glutathione S-transferase, and the amount of thiobarbituric acid reactive substances (TBARS in common carp (Cyprinus carpio L.. Two specific proinflammatory and anti-inflammatory cytokine genes were selected to assess an immunological status of the fish. Fish were exposed for 28 days to three concentrations of DEET (1.0 µg/L, 0.1 mg/L, and 1.0 mg/L where 1 µg/L is corresponding to the concentration found in the environment. DEET had a significant (P<0.05 effect on increased RBC, decreased mean corpuscular volume (MCV, and mean corpuscular haemoglobin value (MCH compared to control groups in the concentration of 1 mg/L. A significant decline (P<0.05 in triacylglycerols (TAG in plasma was found in the concentration of 1 mg/L compared to the control groups. The parameters of oxidative stress in tissues of common carp were weekly affected and immunological parameters were not affected.

  16. Crystal structure, vibrational, spectral investigation, quantum chemical DFT calculations and thermal behavior of Diethyl [hydroxy (phenyl) methyl] phosphonate

    Science.gov (United States)

    Ouksel, Louiza; Chafaa, Salah; Bourzami, Riadh; Hamdouni, Noudjoud; Sebais, Miloud; Chafai, Nadjib

    2017-09-01

    Single Diethyl [hydroxy (phenyl) methyl] phosphonate (DHPMP) crystal with chemical formula C11H17O4P, was synthesized via the base-catalyzed Pudovik reaction and Lewis acid as catalyst. The results of SXRD analyzes indicate that this compound crystallizes into a mono-clinic system with space group P21/n symmetry and Z = 4. The crystal structure parameters are a = 9.293 Å, b = 8.103 Å, c = 17.542 Å, β = 95.329° and V = 1315.2 Å3, the structure displays one inter-molecular O-H⋯O hydrogen bonding. The UV-Visible absorption spectrum shows that the crystal exhibits a good optical transmission in the visible domain, and strong absorption in middle ultraviolet one. The vibrational frequencies of various functional groups present in DHPMP crystal have been deduced from FT-IR and FT-Raman spectra and then compared with theoretical values performed with DFT (B3LYP) method using 6-31G (p, d) basis sets. Chemical and thermodynamic parameters such as: ionization potential (I), electron affinity (A), hardness (σ), softness (η), electronegativity (χ) and electrophilicity index (ω), are also calculated using the same theoretical method. The thermal decomposition behavior of DHPMP, studied by using thermogravimetric analysis (TDG), shows a thermal stability until to 125 °C.

  17. Composition and toxicity of diethyl ether soluble lipids from Nocardia asteroides GUH-2 and Nocardia asteroides 10905.

    Science.gov (United States)

    Ioneda, T; Beaman, B L; Viscaya, L; Almeida, E T

    1993-10-01

    Virulent Nocardia asteroides GUH-2 and avirulent N. asteroides 10905 contained 8.2% and 10.6% of diethyl ether soluble lipids (DESL) per dry cell mass, respectively. Intraperitoneal (i.p.) inoculation of 250 micrograms of DESL from GUH-2 dissolved in mineral oil was toxic to mice, resulting in weight loss and death of 100% of the animals (20/20) within 20 days. In contrast, DESL from 10905 had very little toxicity, and only one mouse (1/10) died within 30 days. Three fractions resulted from DESL by silicic acid column chromatography: (1) neutral lipids and fatty acids (NFA); (2) glycolipids (GL); and (3) phospholipids (PL). Each fraction dissolved in mineral oil was inoculated into mice as described above. The NFA and PL were not toxic. GL from 10905 had low toxicity (30% of the animals died, 3/10) whereas GL from GUH-2 expressed high toxicity (100% of the animals became cachetic and died, 10/10). GL from 10905 represented a minor component (0.6% of dry cell weight) whereas GL from GUH-2 was more prominent (1.5% of dry cell wt.). Approximately 95% of GL from GUH-2 had properties of an authentic trehalose-6,6'-dimycolate standard. Infrared spectrum of the major glycolipid (GUH-2 GL) had characteristic absorptions in the fingerprint region between 800 cm-1 and 1500 cm-1. Upon alkaline hydrolysis GUH-2 GL released 76% mycolic acids in the C50 size range plus 24% trehalose.(ABSTRACT TRUNCATED AT 250 WORDS)

  18. 2-Furaldehyde diethyl acetal from tender coconut water (Cocos nucifera) attenuates biofilm formation and quorum sensing-mediated virulence of Chromobacterium violaceum and Pseudomonas aeruginosa.

    Science.gov (United States)

    Sethupathy, Sivasamy; Nithya, Chari; Pandian, Shunmugiah Karutha

    2015-01-01

    The aim of this study was to evaluate the anti-biofilm and quorum sensing inhibitory (QSI) potential of tender coconut water (TCW) against Chromobacterium violaceum and Pseudomonas aeruginosa. TCW significantly inhibited the QS regulated violacein, virulence factors and biofilm production without affecting their growth. qRT-PCR analysis revealed the down-regulation of autoinducer synthase, transcriptional regulator and virulence genes. Mass-spectrometric analysis of a petroleum ether extract of the TCW hydrolyte revealed that 2-furaldehyde diethyl acetal (2FDA) and palmitic acid (PA) are the major compounds. In vitro bioassays confirmed the ability of 2FDA to inhibit the biofilm formation and virulence factors. In addition, the combination of PA with 2FDA resulted in potent inhibition of biofilm formation and virulence factors. The results obtained strongly suggest that TCW can be exploited as a base for designing a novel antipathogenic drug formulation to treat biofilm mediated infections caused by P. aeruginosa.

  19. Protonated/deprotonated properties of a room temperature ionic liquid-water system: N, N-Diethyl-N-methyl-N-2-methoxyethyl ammonium tetrafluoroborate

    Science.gov (United States)

    Aono, Masami; Abe, Hiroshi; Takekiyo, Takahiro; Yoshimura, Yukihiro

    2014-04-01

    The pH oscillations related to the protonation/deprotonation process in a room temperature ionic liquid (RTIL)-water system were observed at fixed temperatures. The RTIL was hydrophilic N, N-diethyl-N-methyl-N-2-methoxyethyl ammonium tetrafluoroborate ([DEME][BF4]). The rhythmic oscillations of pH were observed only at a water concentration of approximately 90 mol%, where the equilibrated pH value was approximately 3. In contrast, in the water-poor region from 6 to 10 mol% H2O, the pH was almost constant at approximately 8 within the investigated timeframe. The acid-base properties of the [DEME][BF4]-water mixture are related to particular aggregations in the liquid phase.

  20. Synergic effects in the extraction of paracetamol from aqueous NaCl solution by the binary mixtures of diethyl ether and low molecular weight primary alcohols

    Science.gov (United States)

    Nikolić, G. M.; Živković, J. V.; Atanasković, D. S.; Nikolić, M. G.

    2013-12-01

    Liquid-liquid extraction of paracetamol from aqueous NaCl solutions was performed with diethyl ether, 1-propanol, 1-butanol, isobutanol, 1-pentanol, and binary mixtures diethyl ether/1-propanol, diethyl ether/1-butanol, and diethyl ether/isobutanol. Among the pure solvents investigated in this study best extraction efficacy was obtained with 1-butanol. Synergic effects in the extraction with binary mixtures was investigated and compared with some other systems used for the extraction of poorly extractable compounds. Results obtained in this study may be of both fundamental and practical importance.

  1. Crystal structure and identification of resonance forms of diethyl 2-(3-oxoiso-1,3-dihydrobenzofuran-1-ylidenemalonate

    Directory of Open Access Journals (Sweden)

    Mikhail S. Tyumentsev

    2017-10-01

    Full Text Available The reaction of diethyl malonate with phthaloyl chloride in acetonitrile in the presence of triethylamine and magnesium chloride results in the formation of the title compound, diethyl 2-(3-oxo-1,3-dihydro-2-benzofuran-1-ylidenepropanedioate, C15H14O6. One of the ester groups of the diethyl malonate fragment is almost coplanar with the isobenzofuran unit, while the plane of the other group is perpendicular to it [dihedral angles = 5.45 (3 and 83.30 (3°, respectively]. The C—C and C—O distances both in the heterocyclic furan ring and the diethyl malonate fragment are indicative of the dipolar delocalization occurring within the isobenzofuran unit. This delocalization is likely to be responsible for the unusual intermolecular O...O contact [2.756 (2 Å], established between the O atom of the furan ring and the carbonyl O atom of the diethyl malonate fragment. In the crystal, weak C—H...O interactions are observed, which link the molecules into [100] chains.

  2. Fe(III) solar light induced degradation of diethyl phthalate (DEP) in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Mailhot, G.; Caceres, J.; Malato, S.; Bolte, M.

    2003-07-01

    The degradation of diethyl phthalate (DEP) photoinduced by Fe(III) in aqueous solution has been investigated under solar irradiation in the CPC reactor at Plataforma Solar de Almeria. Hydroxyl radicals OH, responsible of the degradation, are formed via an intramolecular photo redox process in excited Fe(III) aqua complexes. For prolonged irradiations DEP and its photoproducts are completely mineralized due to the regeneration of the absorbing species and the continuous formation of OH radicals that confers a catalytic aspect to the process. Consequently, the degradation photoinduced by Fe(III) could be an efficient method of DEP removal from water. (Author) 28 refs.

  3. The super- and sub-critical effects for dielectric constant in diethyl ether

    Science.gov (United States)

    Drozd-Rzoska, Aleksandra; Rzoska, Sylwester J.

    2016-06-01

    Results of dielectric constant (ɛ) studies in diethyl ether for the surrounding of the gas - liquid critical point, TC - 130 K curve, along its diameter (d(T)) and in the supercritical domain for T > TC. For the ultrasound sonicated system, the split into coexisting phases disappeared and dielectric constant approximately followed the pattern of the diameter. This may indicate the possibility of the extension of the "supercritical technology" into the ultrasound "homogenized" subcritical domain: the "strength" and the range of the precritical effect of d(T) are ca. 10× larger than for ɛ (T > TC).

  4. A High Temperature Kinetic Study for the Thermal Unimolecular Decomposition of Diethyl Carbonate

    KAUST Repository

    AlAbbad, Mohammad

    2017-07-08

    Thermal unimolecular decomposition of diethyl carbonate (DEC) was investigated in a shock tube by measuring ethylene concentration with a CO2 gas laser over 900 - 1200 K and 1.2 – 2.8 bar. Rate coefficients were extracted using a simple kinetic scheme comprising of thermal decomposition of DEC as initial step followed by rapid thermal decomposition of the intermediate ethyl-hydrogen-carbonate. Our results were further analysed using ab initio and master equation calculations to obtain pressure- and temperature- dependence of rate coefficients. Similar to alkyl esters, unimolecular decomposition of DEC is found to undergo six-center retro-ene elimination of ethylene in a concerted manner.

  5. A high temperature kinetic study for the thermal unimolecular decomposition of diethyl carbonate

    Science.gov (United States)

    AlAbbad, Mohammed; Giri, Binod Raj; Szőri, Milan; Viskolcz, Béla; Farooq, Aamir

    2017-09-01

    Thermal unimolecular decomposition of diethyl carbonate (DEC) was investigated in a shock tube by measuring ethylene concentration with a CO2 gas laser over 900-1200 K and 1.2-2.8 bar. Rate coefficients were extracted using a simple kinetic scheme comprising of thermal decomposition of DEC as initial step followed by rapid thermal decomposition of the intermediate ethyl hydrogen carbonate. Our results were further analysed using ab initio and master equation calculations to obtain pressure- and temperature-dependence of rate coefficients. Similar to alkyl esters, unimolecular decomposition of DEC is found to undergo six-center retro-ene elimination of ethylene in a concerted manner.

  6. Preferential intramolecular ring closure of aminoalcohols with diethyl carbonate to oxazolidinones.

    Science.gov (United States)

    Fujisaki, Fumiko; Oishi, Marumi; Sumoto, Kunihiro

    2007-05-01

    The closure by cyclization with diethyl carbonate (EtO)(2)CO from aminoalcohols 1 as starting material can lead to the oxazolidinones 2a, b and 2c, respectively. In the reaction of trans-isomer (6) and (EtO)(2)CO, isolated products were also only 5-membered oxazolidinone derivative (7), containing its dehydrated derivative 8. The preferential formation of the 5-membered oxazolidinone ring system apparently indicated that this process (5-Exo-Trig ring closure) is more favorable than that of 6- or 7-membered ring derivative (3 or 9) by 6- or 7-Exo-Trig ring closure.

  7. Degradation mechanisms of the ethylene carbonate/diethyl carbonate mixture studied by radiolysis

    OpenAIRE

    Wang, Furong; Varenne, Fanny; Ortiz, Daniel; Pinzio, Valentin; Mostafavi, Mehran; Le Caer, Sophie

    2017-01-01

    International audience; The reactivity of ethylene carbonate (EC) and of the ethylene carbonate/diethyl carbonate (DEC) mixture is studied under ionizing radiation in order to mimic aging phenomena occurring in lithium-ion batteries. Picosecond pulse radiolysis experiments show that the attachment of the electron on EC molecule is ultrafast (k(e-EC + EC) = 1.3  109 L mol-1 s-1 at 46°C). In the case of the 50/50 EC/DEC mixture, just after the electron pulse, the electron is solvated by a mixt...

  8. Phase Equilibria of Ternary and Quaternary Systems Containing Diethyl Carbonate with Water

    OpenAIRE

    Chen, Yao; Wen, Caiyu; Zhou, Xiaoming; Zeng, Jun

    2014-01-01

    In this study liquid phase equilibrium compositions were measured at 298.15 K under atmospheric pressure for (water + propan-1-ol + diethyl carbonate (DEC) + benzene or cyclohexane or heptane) quaternary systems and (water + DEC + propan-1-ol or benzene or cyclohexane) ternary systems. Good correlation of the experimental LLE data was seen for the measured systems by both modified and extended UNIQUAC models. The solubility of DEC in aqueous and organic phases is shown by equilibrium distribu...

  9. Phase Equilibria of Ternary and Quaternary Systems Containing Diethyl Carbonate with Water.

    Science.gov (United States)

    Chen, Yao; Wen, Caiyu; Zhou, Xiaoming; Zeng, Jun

    2014-01-01

    In this study liquid phase equilibrium compositions were measured at 298.15 K under atmospheric pressure for (water + propan-1-ol + diethyl carbonate (DEC) + benzene or cyclohexane or heptane) quaternary systems and (water + DEC + propan-1-ol or benzene or cyclohexane) ternary systems. Good correlation of the experimental LLE data was seen for the measured systems by both modified and extended UNIQUAC models. The solubility of DEC in aqueous and organic phases is shown by equilibrium distribution coefficients calculated from the LLE data.

  10. STUDY ON THE THERMODYNAMIC PROPERTIES OF ADSORPTION OF ETHYL BENZOATE AND DIETHYL PHTHALATE BY PHENOLIC RESIN ADSORBENTS

    Institute of Scientific and Technical Information of China (English)

    Zhong Wang; Zuo-qing Shi; Rong-fu Shi; Yun-ge Fan; Yi-zhong Yang

    2004-01-01

    This paper presents experimental observations on the adsorption of individual solutes by a simple thermodynamic framework, and the equilibrium adsorption of ethyl benzoate and diethyl phthalate on phenolic resin adsorbent in hexane solutions within the temperature range of 293-313 K. The experimental results show that the Freundlich adsorption law is applicable to the adsorption of ethyl benzoate and diethyl phthalate on the adsorbent, since all the correlative factors R' are larger than 0.99. The negative values of all the isosteric adsorption enthalpies for ethyl benzoate and diethyl phthalate indicate that they undergo exothermic processes, while their magnitudes (19-28 kJ/mol) manifest a hydrogen bonding sorption process. Other thermodynamic properties: the free energy changes and the entropy change associated with the adsorption have been calculated from the Gibbs adsorption equation and the Gibbs-Helmholtz equation.

  11. Dynamic observation of surface reactions of lithium foils immersed in diethyl carbonate electrolytes by using in-situ FTIR measurement

    Energy Technology Data Exchange (ETDEWEB)

    Kanamura, K.; Takezawa, H. [Kyoto Univ., Kyoto (Japan). Graduate School; Shiraishi, S.; Takehara, Z. [Gunma Univ., Maebashi (Japan). Faculty of Engineering

    1998-03-05

    Rechargeable lithium batteries with lithium metal anodes are very attractive for various applications, however, they have not been applied to practical batteries, due to low cycleability and safety of lithium metal anodes. This problem may be related to the surface state of lithium metal immersed in nonaqueous electrolytes. Several fundamental studies have been carried out, however, the high reactivity of diethyl carbonate with lithium metal has not been clarified yet. In this study, the dynamic behavior of diethyl carbonate containing 1.0 mol dm{sup -3} LiAsF6, LiBF4 and LiCF3SO3 at the interface on lithium foils was observed by using in-situ FTIR spectroscopy. The in-situ FTIR spectra indicated that these diethyl carbonate electrolytes can easily penetrate into the surface film on the lithium foil and directly touch to lithium metal. 28 refs., 8 figs.

  12. Thermophysical properties for (diethyl carbonate + p-xylene + octane) ternary system

    Energy Technology Data Exchange (ETDEWEB)

    Mosteiro, L. [Departamento de Fisica Aplicada, Facultad de Ciencias Experimentales, Universidad de Vigo, Lagoas Marcosende s/n, 36310 Vigo (Spain); Casas, L.M., E-mail: lmcasas@uvigo.es [Departamento de Fisica Aplicada, Facultad de Ciencias Experimentales, Universidad de Vigo, Lagoas Marcosende s/n, 36310 Vigo (Spain); Curras, M.R. [Departamento de Fisica Aplicada, Facultad de Ciencias Experimentales, Universidad de Vigo, Lagoas Marcosende s/n, 36310 Vigo (Spain); Mariano, A.B. [Laboratorio de Fisicoquimica, Departamento de Quimica, Facultad de Ingenieria, Universidad Nacional de Comahue, 8300 Neuquen (Argentina); Legido, J.L. [Departamento de Fisica Aplicada, Facultad de Ciencias Experimentales, Universidad de Vigo, Lagoas Marcosende s/n, 36310 Vigo (Spain)

    2011-12-15

    Highlights: > Thermophysical properties of (diethyl carbonate + p-xylene + octane) were measured. > Excess molar volumes and isentropic compressibilities were determined and correlated. > Ternary surface tension deviations were correlated using Cibulka equation. > Intermolecular interactions based on the derived properties trend were discussed. - Abstract: The density and speed of sound of the ternary mixture (diethyl carbonate + p-xylene + octane) have been measured at atmospheric pressure and in the temperature range T = (288.15 to 308.15) K. Besides, surface tension has been also determined for the same mixture at T = 298.15 K. The experimental measurements have allowed the calculation of the corresponding derived properties: excess molar volumes, excess isentropic compressibilities, and surface tension deviations. Excess properties have been correlated using Nagata and Tamura equation and correlation for the surface tension deviation has been done with the Cibulka equation. Good accuracy has been obtained. Based on the variations of the derived properties values with composition, a qualitative discussion about the intermolecular interactions was drawn.

  13. Design of new and potent diethyl thiobarbiturates as urease inhibitors: a computational approach.

    Science.gov (United States)

    Wadood, Abdul; Riaz, Muhammad; Mulk, Amir Ul; Khan, Momin; Haleem, Sobia Ahsan; Shams, Sulaiman; Gul, Sahib; Ahmed, Ayaz; Qasim, Muhammad; Ali, Farman; Ul-Haq, Zaheer

    2014-01-01

    Urease is an important enzyme both in agriculture and medicine research. Strategies based on urease inhibition is critically considered as the first line treatment of infections caused by urease producing bacteria. Since, urease possess agro-chemical and medicinal importance, thus, it is necessary to search for the novel compounds capable of inhibiting this enzyme. Several computational methods were employed to design novel and potent urease inhibitors in this work. First docking simulations of known compounds consists of a set of arylidine barbiturates (termed as reference) were performed on the Bacillus pasteurii (BP) urease. Subsequently, two fold strategies were used to design new compounds against urease. Stage 1 comprised of the energy minimization of enzyme-ligand complexes of reference compounds and the accurate prediction of the molecular mechanics generalized born (MMGB) interaction energies. In the second stage, new urease inhibitors were then designed by the substitution of different groups consecutively in the aryl ring of the thiobarbiturates and N, N-diethyl thiobarbiturates of the reference ligands.. The enzyme-ligand complexes with lowest interaction energies or energies close to the calculated interaction energies of the reference molecules, were selected for the consequent chemical manipulation. This was followed by the substitution of different groups on the 2 and 5 positions of the aryl ring. As a result, several new and potent diethyl thiobarbiturates were predicted as urease inhibitors. This approach reflects a logical progression for early stage drug discovery that can be exploited to successfully identify potential drug candidates.

  14. Daucus carota Pentane/Diethyl Ether Fraction Inhibits Motility and Reduces Invasion of Cancer Cells.

    Science.gov (United States)

    Zgheib, Perla; Daher, Costantine F; Mroueh, Mohamad; Nasrallah, Anita; Taleb, Robin I; El-Sibai, Mirvat

    2014-01-01

    Daucus carota (DC) is a herb used in folklore medicine in Lebanon to treat numerous diseases including cancer. Recent studies in our laboratory on DC oil and its fractions revealed potent anticancer activities in vitro and in vivo. The present study aims to investigate the effect of the most potent DC fraction, pentane/diethyl ether (50:50), on lung, skin, breast and glioblastoma cancer cell motility and invasion. Upon treatment, a pronounced decrease in cancer cell motility was observed in the 4 cell lines. The treatment also led to a decrease in cancer cell invasion and an increased cell adhesion. Additionally, the DC fraction caused a decrease in the activation of the ρ-GTPases Rac and CDC42, a finding that may partially explain the treatment-induced decrease in cell motility. The current study demonstrates a crucial effect of the DC pentane/diethyl ether fraction on cancer cell motility and metastasis, making it a potential candidate for cancer therapy specifically targeting cancer motility and metastasis. © 2015 S. Karger AG, Basel.

  15. N,N-Diethyl-1-Tosyl-3-Indoleglyoxylamide as a Dienophile in Diels-Alder Reactions. Hyperbaric vs. Thermal Conditions

    Directory of Open Access Journals (Sweden)

    B. Biolatto

    2000-03-01

    Full Text Available Under high pressure conditions, the Diels-Alder reaction involving N,N-diethyl-1-tosyl-3-indoleglyoxylamide and 1-(N-acetyl-N-propylamino-1,3-butadiene produces a highly functionalized intermediate for the synthesis of Indole Alkaloids, in shorter times and higher yields than under thermal conditions.

  16. Determination of Diethyl Phthalate and Polyhexamethylene Guanidine in Surrogate Alcohol from Russia

    Directory of Open Access Journals (Sweden)

    Yulia B. Monakhova

    2011-01-01

    Full Text Available Analytical methods based on spectroscopic techniques were developed and validated for the determination of diethyl phthalate (DEP and polyhexamethylene guanidine (PHMG, which may occur in unrecorded alcohol. Analysis for PHMG was based on UV-VIS spectrophotometry after derivatization with Eosin Y and 1H NMR spectroscopy of the DMSO extract. Analysis of DEP was performed with direct UV-VIS and 1H NMR methods. Multivariate curve resolution and spectra computation methods were used to confirm the presence of PHMG and DEP in the investigated beverages. Of 22 analysed alcohol samples, two contained DEP or PHMG. 1H NMR analysis also revealed the presence of signals of hawthorn extract in three medicinal alcohols used as surrogate alcohol. The simple and cheap UV-VIS methods can be used for rapid screening of surrogate alcohol samples for impurities, while 1H NMR is recommended for specific confirmatory analysis if required.

  17. FTIR spectroscopic studies of lithium tetrafluoroborate in propylene carbonate + diethyl carbonate mixtures

    Science.gov (United States)

    Zhang, Binbin; Zhou, Yuan; Li, Xiang; Ren, Xiufeng; Nian, Hongen; Shen, Yue; Yun, Qiang

    2014-03-01

    FTIR (Fourier transformed infrared) spectra have been collected and analyzed for solutions of lithium tetrafluoroborate in propylene carbonate (PC), diethyl carbonate (DEC), and PC + DEC mixtures. It has been shown that the carbonyl stretch bands of PC and DEC, the ring of PC and the ether oxygen stretch bands of DEC are all very sensitive to the interaction between Li+ and the solvent molecules. New shoulders appear and the original bands split with the addition of LiBF4, indicating that a strong interaction between Li+ and molecules of PC and DEC exists through the oxygen group of Cdbnd O and ring of PC and both Cdbnd O oxygen and ether oxygen atoms of DEC. In addition, no preferential solvation of Li+ in LiBF4/PC + DEC solutions was detected.

  18. Transdermal uptake of diethyl phthalate and di(n-butyl) phthalate directly from air: Experimental verification

    DEFF Research Database (Denmark)

    Weschler, Charles J.; Bekö, Gabriel; Koch, Holger M.;

    2015-01-01

    Background: Fundamental considerations indicate that, for certain phthalate esters, dermal absorption from air is an uptake pathway that is comparable to or greater than inhalation. Yet this pathway has not been experimentally evaluated and has been largely overlooked when assessing uptake...... of phthalate esters. Objectives: This study investigated transdermal uptake, directly from air, of diethyl phthalate (DEP) and di(n-butyl) phthalate (DnBP) in humans. Methods: In a series of experiments, six human participants were exposed for 6 hr in a chamber containing deliberately elevated air...... concentrations of DEP and DnBP. The participants either wore a hood and breathed air with phthalate concentrations substantially below those in the chamber or did not wear a hood and breathed chamber air. All urinations were collected from initiation of exposure until 54 hr later. Metabolites of DEP and Dn...

  19. Solid form of indapamide recrystallized from acetonitrile/diethyl ether solvent mixture

    Science.gov (United States)

    Rus, Lucia M.; Kacso, Irina; Borodi, Gheorghe; Aluas, Mihaela; Tomuta, Ioan; Iuga, Cristina; Simon, Simion; Bratu, Ioan; Bojita, Marius

    2012-02-01

    Indapamide (IDP) is a non-thiazide sulphonamide diuretic drug generally used for the treatment of essential hypertension. The aim of this work was to obtain and to characterize new solid forms of IDP. In this respect, the recrystallization of IDP from different solvent or solvent mixtures was carried out. Thermoanalytical techniques (differential scanning calorimetry (DSC) and thermogravimetry (TG)), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR), solid state nuclear magnetic resonance (NMR) spectroscopy and scanning electron microscopy (SEM) were used for structural characterization of the new obtained solid forms. Based on the results of these techniques we can conclude that IDP recrystallized from acetonitrile+ diethyl ether solvent mixture presents a different structure and physical properties as compared with the starting IDP.

  20. 8,8-Diethyl-1,4,5,8-tetrahydronaphthalene-1,4,5-trione

    Directory of Open Access Journals (Sweden)

    Ramiro Araya-Maturana

    2009-02-01

    Full Text Available The title molecule, C14H14O3, contains two fused six-membered carbon rings with keto groups at positions 1, 4 and 5 and a gem-diethyl group at position 8. The molecule is close to planar (maximum deviation = 0.044 Å, with one ethyl group at each side of the molecular plane, with exception of the keto group at position 1 which is slightly deviated from the plane and disordered over two positions one on each side of it (occupancies 0.80/0.20. The packing of the molecule shows weak bonded chains along a through C—H...O contacts and two intramolecular C—H...O interactions are also present.

  1. 苯甲醛、2-异丁腈与丙二酸二乙酯的三组分Passerini反应%Three components Passerini reactions of Benzaldehyde, 2 -Isobutyronitrile and Diethyl Malonate

    Institute of Scientific and Technical Information of China (English)

    陈懿; 谢兵; 高斌

    2012-01-01

    The paper explores three multieomponent Passerini reactions by using diethyl malonate instead of car- boxylic acid or alcohol. The significant applied value of compounds including double functional group diethyl malonate derivative from benzaldehyde, 2 - isobutyrenitrile and diethyl malonate was synthesized by one - pot in moderate yield by using H2SO4 as catalyst at microwave and heat under free - solvent. The optimized reaction condition follows the aspects: 2mL H2SO4 as catalyst; reaction temperature was 120 ℃, power rating for micrwave was 300 W and reaction time was 40 min.%探索用丙二酸二乙酯替代羧酸或醇进行三组分Passerini反应。在无溶剂条件下,用浓硫酸作为催化剂,苯甲醛、2-异丁腈和丙二酸二乙酯通过微波辅助和加热,一锅法进行三组分Passerini反应,以中等收率得到具有重要应用价值的双官能团化合物丙二酸二乙酯衍生物。该反应的最佳条件为:以浓硫酸为催化剂,催化剂用量为2mL,反应温度为120℃,微波功率为BOOW,反应时间为40min。

  2. Removal of diethyl phthalate from aqueous phase using magnetic poly(EGDMA-VP) beads

    Energy Technology Data Exchange (ETDEWEB)

    Tuemay Oezer, Elif [Department of Chemistry, Uludag University, Bursa (Turkey); Osman, Bilgen, E-mail: bilgeno@uludag.edu.tr [Department of Chemistry, Uludag University, Bursa (Turkey); Kara, Ali; Besirli, Necati; Guecer, Seref [Department of Chemistry, Uludag University, Bursa (Turkey); Soezeri, Hueseyin [TUBITAK-UME, National Metrology Institute, PO Box 54 TR-41470, Gebze/Kocaeli (Turkey)

    2012-08-30

    Highlights: Black-Right-Pointing-Pointer Magnetic beads were prepared for removal of diethyl phthalate (DEP). Black-Right-Pointing-Pointer Total capacity of the beads was determined as 98.9 mg DEP per gram polymer. Black-Right-Pointing-Pointer Magnetic beads were regenerated easily and reused for DEP adsorption. Black-Right-Pointing-Pointer Adsorption isotherms, kinetics and thermodynamics were elucidated. - Abstract: The barium hexaferrite (BaFe{sub 12}O{sub 19}) containing magnetic poly(ethylene glycol dimethacrylate-vinyl pyridine), (mag-poly(EGDMA-VP)) beads (average diameter = 53-212 {mu}m) were synthesized and characterized. Their use as an adsorbent in the removal of diethyl phthalate (DEP) from an aqueous solution was investigated. The mag-poly(EGDMA-VP) beads were prepared by copolymerizing of 4-vinyl pyridine (VP) with ethylene glycol dimethacrylate (EGDMA). The mag-poly(EGDMA-VP) beads were characterized by N{sub 2} adsorption/desorption isotherms (BET), vibrating sample magnetometer (VSM), X-ray powder diffraction (XRD), elemental analysis, scanning electron microscope (SEM) and swelling studies. At a fixed solid/solution ratio, the various factors affecting the adsorption of DEP from aqueous solutions such as pH, initial concentration, contact time and temperature were analyzed. The maximum DEP adsorption capacity of the mag-poly(EGDMA-VP) beads was determined as 98.9 mg/g at pH 3.0, 25 Degree-Sign C. All the isotherm data can be fitted with both the Langmuir and the Dubinin-Radushkevich isotherm models. The pseudo first-order, pseudo-second-order, Ritch-second-order and intraparticle diffusion models were used to describe the adsorption kinetics. The thermodynamic parameters obtained indicated the exothermic nature of the adsorption. The DEP adsorption capacity did not change after 10 batch successive reactions, demonstrating the usefulness of the magnetic beads in applications.

  3. Synthesis and Characterization of Novel (E-tert-butyl 7-(4-methoxyphenyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-ylhept-2-enoate and (E-diethyl (6-(4-methoxyphenyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-ylhex-1-en-1-ylphosphonate; Application of Olefin Cross Metathesis

    Directory of Open Access Journals (Sweden)

    *H. Hussain

    2013-12-01

    Full Text Available Two novel compounds (E-tert-butyl 7-(4-methoxyphenyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-ylhept-2-enoate and (E-diethyl (6-(4-methoxyphenyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-ylhex-1-en-1-ylphosphonate were synthesized in excellent yields by olefin cross metathesis (CM. 3-(4-methoxyphenylpropyl diisopropylcarbamate and allylboronic acid pinacol ester were reacted in the presence of s-BuLi/N,N,N,N-tetramethylethyllenediamine (TMEDA to form sec. boronic ester which was further reacted with tert-butyl acrylate and diethyl vinylphosphonate respectively to get the desired products. Both novel compounds have applications as reactants for cyclopropanation and cyclopentataion for asymmetric synthesis.

  4. Mefenpyr-diethyl action on fenoxaprop-p-ethyl detoxification in wheat varieties Ação de mefenpyr-diethyl sobre a desintoxicação de fenoxaprop-´p-ethyl em variedades de trigo

    Directory of Open Access Journals (Sweden)

    A.C. Cataneo

    2013-06-01

    Full Text Available Safeners protect crops against herbicide injury. The aim of this study was to examine the differential susceptibility of five wheat (Triticum aestivum varieties to the herbicide fenoxaprop-p-ethyl, as well as the performance of mefenpyr-diethyl on minimizing herbicide injury and on lipid contents. Varieties BRS 49, CD 104, CEP 24, IAPAR 78 and Rubi were sprayed with fenoxaprop-p-ethyl (69 g ha¹, fenoxaprop-p-ethyl + mefenpyr-diethyl (69 g + 18.75 g ha-1, or mefenpyr-diethyl (18.75 g ha-1. Plants were evaluated visually for injury at 7 and 14 days after treatment (DAT. Glutathione S-transferase (GST activity was assayed in aerial parts at 7 DAT, and lipid content was measured at 14 DAT. Varieties CEP 24, IAPAR 78 and Rubi were more tolerant to fenoxaprop-p-ethyl than BRS 49, and CD 104 rapidly recovering from the slight phytotoxicity symptoms produced by the herbicide. Mefenpyr-diethyl prevented crop injury associated with the herbicide. GST activity did not correlate directly with fenoxaprop-p-ethyl detoxification. However, lipid content was related to the susceptibility of wheat to fenoxaprop-p-ethyl treatment.Protetores ou safeners protegem culturas contra a injúria de herbicidas. O propósito deste estudo foi investigar a suscetibilidade diferencial de cinco variedades de trigo (Triticum aestivum ao herbicida fenoxaprop-p-ethyl e o efeito do protetor mefenpyr-diethyl na minimização da injúria do herbicida e sobre o conteúdo de lipídios. As variedades BRS 49, CD 104, CEP 24, IAPAR 78 e Rubi foram pulverizadas com fenoxaprop-p-ethyl (69 g ha-1, fenoxaprop-p-ethyl + mefenpyr‑diethyl (69 g + 18,75 g ha¹ ou mefenpyr-diethyl (18,75 g ha¹. A injúria das plantas foi avaliada visualmente aos 7 e 14 dias após o tratamento (DAT. A atividade da glutationa S-transferase (GST foi analisada na parte aérea aos 7 DAT, e o conteúdo de lipídios, aos 14 DAT. As variedades CEP 24, IAPAR 78 e Rubi foram mais tolerantes ao fenoxaprop-p-ethyl do que

  5. Volumetric Properties of the Mixture Trichloromethane CHCl3 + C4H10O Diethyl ether (VMSD1211, LB3412_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Trichloromethane CHCl3 + C4H10O Diethyl ether (VMSD1211, LB3412_V)' providing data from direct low-pressure dilatometric measurement of molar excess volume at variable mole fraction and constant temperature.

  6. Di-μ-iodido-bis[(diethyl ether-κO(η5-1,3-di-tert-butylcyclopentadienylytterbium(II

    Directory of Open Access Journals (Sweden)

    Madeleine Schultz

    2008-01-01

    Full Text Available The half-sandwich title compound, [Yb2(C13H212I2(C4H10O2], crystallizes as a centrosymmetric dimer. The Yb atom is coordinated in a three-legged piano-stool geometry by a cyclopentadienyl ring, two I anions and the O atom of a diethyl ether molecule. The central Yb2I2 core is an approximate square.

  7. 2,2-Diethyl 4-methyl 5-(4-nitrophenyl-4-phenylpyrrolidine-2,2,4-tricarboxylate

    Directory of Open Access Journals (Sweden)

    Long He

    2011-10-01

    Full Text Available The title compound, C24H26N2O8, was synthesized by the cycloaddition reaction of methyl 2-phenylacrylate, diethyl 2-aminomalonate and 4-nitrobenzaldehyde. The pyrrolidine ring exhibits an envelope conformation. The two benzene rings are located on opposite sides of the pyrrolidine ring and subtend a dihedral angle of 59.16 (14°. The crystal packing is stabilized by N—H...O and weak C—H...O hydrogen bonding.

  8. Inorganic polarography in organic solvents-II: polarographic examination of the molybdenum(V) thiocyanate complex in diethyl ether.

    Science.gov (United States)

    Afghan, B K; Dagnall, R M

    1967-02-01

    A procedure involving the solvent extraction of molybdenum(V) thiocyanate into diethyl ether followed by a direct polarographic examination of the organic phase offers a selective method for the determination of molybdenum down to 0.5 ppm. Only molybdenum, amongst 21 elements examined, is observed to give a reduction wave under the recommended conditions. The method is evaluated with respect to various experimental factors and is applied to the determination of molybdenum in mild and alloy steels.

  9. New synthesis and characterization of (+)-lysergic acid diethylamide (LSD) derivatives and the development of a microparticle-based immunoassay for the detection of LSD and its metabolites.

    Science.gov (United States)

    Li, Z; Goc-Szkutnicka, K; McNally, A J; Pilcher, I; Polakowski, S; Vitone, S; Wu, R S; Salamone, S J

    1997-01-01

    In this paper are reported the synthesis and characterization of three LSD derivatives. On the basis of several analytical characterization studies, the most stable derivative has been selected and a procedure to covalently link the derivative to polystyrene microparticles through a carrier protein has been developed. In addition, two new LSD immunogens have been synthesized and characterized, and from these immunogens antibodies that recognize not only LSD but also several major LSD metabolites have been generated. Using the selected derivative and antibody, a homogeneous microparticle-based immunoassay has been developed for the detection of LSD in human urine with the required sensitivity and specificity for an effective screening assay. The performance of this LSD OnLine assay has been evaluated using the criteria of precision, cross-reactivity, correlation to the Abuscreen LSD RIA and GC/MS/MS, assay specificity, and limit of detection.

  10. Determination of lysergic acid diethylamide (LSD) by application of online 77 K fluorescence spectroscopy and a sweeping technique in micellar electrokinetic chromatography.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Lin, Cheng-Huang

    2002-10-16

    The principal advantage of the use of Shopl'skii effect (low temperature spectrum) is that spectral sharpening occurs both in absorption and emission. However, thus far using the technique of capillary electrophoresis/low temperature fluorescence spectroscopy (CE/LTFS) either at 77 or 4.2 K remains difficult to obtain an on-line spectrum, if the analyte is present at low concentration. This paper examines the feasibility of combining the techniques of online concentration and CE/LTFS to identify LSD and related compounds in urine at 77 K. To improve sensitivity, sweeping-micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were used for on-line concentration which resulted in detection limits of approximately 20 approximately 60 ppt, respectively.

  11. short communication facile, mild and selective silica sulfuric acid ...

    African Journals Online (AJOL)

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    as a mild, efficient and reusable solid acid catalyst was used to afford the ... and overcome typical problems that occur during oxidation and accept wide rang of ... synthetic and natural organic and inorganic compounds in aqueous solution and it .... (CCl4), dichloromethane (CH2Cl2), chloroform (CHCl3), diethyl ether and.

  12. Diethyl phosphates accumulation in rabbits' hair as an indicator of long term exposure to diazinon and chlorpyrifos.

    Science.gov (United States)

    Maravgakis, George; Tzatzarakis, Manolis N; Alegakis, Athanasios K; Stivaktakis, Polychronis D; Tsatsakis, Aristidis M

    2012-05-10

    Long term exposure to organophosphate pesticides can be evaluated by quantitative analysis of their non-specific metabolites in hair matrix. The aim of this study was to determine whether these metabolites can be internally incorporated into the hair of rabbits exposed to diazinon and chlorpyrifos. The influence of dose and dose duration of each pesticide dosage were investigated. Three groups of rabbits were exposed to different dosages of diazinon (3.0 and 6.0mg/kg/day) and chlorpyrifos (18.0mg/kg/day) via drinking water. Hair samples were collected every month and analyzed for diethyl phosphate (DEP) and diethyl thiophosphate (DETP) by gas chromatography-mass spectrometry (GC-MS). The mean concentrations of the low-dose treated group, ranged from 112 to 257pg/mg for DEP and from 295 to 515pg/mg for DETP in hair. The high-dose treated group demonstrated a range of mean concentrations from 142 to 585pg/mg for DEP and from 406 to 988pg/mg for DETP in hair. For the chlorpyrifos treated group, the concentrations ranged from 138 to 1070 for DEP and from 554 to 886pg/mg for DETP. Analysis revealed the incorporation of these metabolites into the rabbit hair in a dosage and dose duration-dependent manner. These data confirms the ability of using hair analysis for diethyl phosphates to assess long-term OP exposure.

  13. Adsorption and reactions of dimethyl and diethyl ethers on Mo 2C/Mo(1 0 0)

    Science.gov (United States)

    Farkas, A. P.; Solymosi, F.

    2008-04-01

    The adsorption, desorption and dissociation of dimethyl ether and diethyl ether on Mo 2C/Mo(1 0 0) have been investigated by work function, thermal desorption (TPD) and high resolution electron energy loss spectroscopy (HREELS). The adsorption of both molecules at 100 K caused a significant decrease in the work function of the Mo 2C/Mo(1 0 0) surface. In the case of dimethyl ether almost 90% of the adsorbed monolayer desorbed intact with a Tp = 286 K. Another part decomposed to CO ( Tp = 330 and 960 K) and H 2 ( Tp = 330 and 400 K). The desorption of diethyl ether at monolayer occurred with Tp = 256 and 340 K. Another fraction underwent decomposition as indicated by the release of CO ( Tp = 336 and 436 K) and H 2 ( Tp = 400 K). In addition, the formation of ethylene ( Tp = 342 K) and a very small amount of methane ( Tp = 380 K) was also observed. HREEL spectra of both ethers confirmed their molecular adsorption at 100 K. From the spectral changes occurred upon increasing the exposures and in off-specular direction some conclusions were drawn on the bonding of the adsorbed molecules. Analysis of the HREEL spectra of the annealed layers suggested that in the primary steps the adsorbed ethers dissociate to methyl and methoxy (dimethyl ether), and to ethyl and ethoxy (diethyl ether) species, which react further to yield the desorption products.

  14. Inhibition of diethyl ether degradation in Rhodococcus sp. strain DEE5151 by glutaraldehyde and ethyl vinyl ether.

    Science.gov (United States)

    Kim, Yong-Hak; Engesser, Karl-Heinrich

    2005-02-15

    Alkyl ether-degrading Rhodococcus sp. strain DEE5151, isolated from activated sewage sludge, has an activity for the oxidation of a variety of alkyl ethers, aralkyl ethers and dibenzyl ether. The whole cell activity for diethyl ether oxidation was effectively inhibited by 2,3-dihydrofurane, ethyl vinyl ether and glutaraldehyde. Glutaraldehyde of less than 30 microM inhibited the activity by a competitive manner with the inhibition constant, K(I) of 7.07+/-1.36 microM. The inhibition type became mixed at higher glutaraldehyde concentrations >30 microM, probably due to the inactivation of the cell activity by the Schiff-base formation. Structurally analogous ethyl vinyl ether inhibited the diethyl ether oxidation activity in a mixed manner with decreasing the apparent maximum oxidation rate, v(max)(app), and increasing the apparent Michaelis-Menten constant, K(M)(app). The mixed type inhibition by ethyl vinyl ether seemed to be introduced not only by the structure similarity with diethyl ether, but also by the reactivity of the vinyl ether with cellular components in the whole cell system.

  15. Gamma irradiation effects on the grafting of low-density polyethylene with diethyl maleate

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Y. [Centro de Quimica, Laboratorio de Polimeros, Instituto Venezolano de Investigaciones Cientificas (IVIC) (Venezuela); Albano, C. [Centro de Quimica, Laboratorio de Polimeros, Instituto Venezolano de Investigaciones Cientificas (IVIC) (Venezuela) and Universidad Central de Venezuela, Facultad de Ingenieria, Escuela de Ingenieria Quimica, P.O. Box 48146, Los Chaguaramos, Caracas 1041 A (Venezuela)]. E-mail: calbano@ivic.ve; Karam, A. [Centro de Quimica, Laboratorio de Polimeros, Instituto Venezolano de Investigaciones Cientificas (IVIC) (Venezuela)]. E-mail: akaram@quimica.ivic.ve; Perera, R. [Departamento de Mecanica, Universidad Simon Bolivar (Venezuela); Silva, P. [Centro de Fisica, Laboratorio de Fisica de la Materia Condensada, Instituto Venezolano de Investigaciones Cientificas (IVIC) (Venezuela); Gonzalez, J. [Departamento de Mecanica, Universidad Simon Bolivar (Venezuela)

    2005-07-01

    In this work, a low-density polyethylene (LDPE) was grafted with diethyl maleate (DEM) using gamma-rays from a Cobalt-60 source at different absorbed doses and monomer concentrations between 5 and 30 wt.%. This process was carried out in a decalin solution at 10 w/v% to obtain a homogeneous dispersion of the monomer into the polyethylene matrix. It was found that the grafting degree increases with the absorbed doses, as a consequence of the increased amount of energy given to the system, which made the grafting process more favorable. The grafting degree also increases with the concentration of DEM, because a higher concentration makes the insertion easier due to the increased availability of the free monomer. The highest grafting degree was obtained at 200 kGy of absorbed dose and with 30 wt.% of DEM. The melt flow index (MFI) values showed a decreasing trend as the absorbed dose was increased. This fact reveals that crosslinking and grafting are taking place simultaneously, this behavior being remarkable at higher irradiation doses. The results from thermogravimetric analysis (TGA) showed that the initial degradation temperatures remained almost unchanged with the absorbed dose.

  16. Regulated and unregulated emissions from a diesel engine fueled with diesel fuel blended with diethyl adipate

    Science.gov (United States)

    Zhu, Ruijun; Cheung, C. S.; Huang, Zuohua; Wang, Xibin

    2011-04-01

    Experiments were carried out on a four-cylinder direct-injection diesel engine operating on Euro V diesel fuel blended with diethyl adipate (DEA). The blended fuels contain 8.1%, 16.4%, 25% and 33.8% by volume fraction of DEA, corresponding to 3%, 6%, 9% and 12% by mass of oxygen in the blends. The engine performance and exhaust gas emissions of the different fuels were investigated at five engine loads at a steady speed of 1800 rev/min. The results indicated an increase of brake specific fuel consumption and brake thermal efficiency when the engine was fueled with the blended fuels. In comparison with diesel fuel, the blended fuels resulted in an increase in hydrocarbon (HC) and carbon monoxide (CO), but a decrease in particulate mass concentrations. The nitrogen oxides (NO x) emission experienced a slight variation among the test fuels. In regard to the unregulated gaseous emissions, formaldehyde and acetaldehyde increased, while 1,3-butadiene, ethene, ethyne, propylene and BTX (benzene, toluene and xylene) in general decreased. A diesel oxidation catalyst (DOC) was found to reduce significantly most of the investigated unregulated pollutants when the exhaust gas temperature was sufficiently high.

  17. Excess Molar Volumes and Viscosities of Binary Mixture of Diethyl Carbonate+Ethanol at Different Temperatures

    Institute of Scientific and Technical Information of China (English)

    MA Peisheng; LI Nannan

    2005-01-01

    The purpose of this work was to report excess molar volumes and dynamic viscosities of the binary mixture of diethyl carbonate (DEC)+ethanol. Densities and viscosities of the binary mixture of DEC+ethanol at temperatures 293.15 K-343.15 K and atmospheric pressure were determined over the entire composition range. Densities of the binary mixture of DEC+ethanol were measured by using a vibrating U-shaped sample tube densimeter. Viscosities were determined by using Ubbelohde suspended-level viscometer. Densities are accurate to 1.0×10-5 g·cm-3, and viscosities are reproducible within ±0.003 mPa·s. From these data, excess molar volumes and deviations in viscosity were calculated. Positive excess molar volumes and negative deviations in viscosity for DEC+ethanol system are due to the strong specific interactions.All excess molar vo-lumes and deviations in viscosity fit to the Redlich-Kister polynomial equation.The fitting parameters were presented,and the average deviations and standard deviations were also calculated.The errors of correlation are very small.It proves that it is valuable for estimating densities and viscosities of the binary mixture by the correlated equation.

  18. Enhanced bioremediation of soil from Tianjin, China, contaminated with polybrominated diethyl ethers.

    Science.gov (United States)

    Zhang, Zhiyuan; Wang, Cuiping; Li, Jing; Wang, Baolin; Wu, Jianyu; Jiang, Yan; Sun, Hongwen

    2014-12-01

    This work aimed to evaluate the effectiveness of nutrients, H2O2, and tourmaline on the bioremediation of fields where the soil was contaminated with polybrominated diethyl ethers (PBDEs). The results showed that 39.2, 38.3, and 48.1 % of total PBDE removal was observed in microcosms with the addition of nutrients, such as NaNO3, NH4Cl, and NH4NO3, respectively, compared to only 15.2 and 5.8 % of PBDE removal from soil with added Aspergillus niger and control soil, respectively, after 50 days of incubation. In addition, 50.8 and 56.5 % of total PBDE removal were observed in microcosms with 0.5 and 1 μL H2O2. The addition of tourmaline increased total PBDE removal to 32.4 %. Significant increases in soil enzymatic activity with PBDE degraders and bacterial communities were observed using polymerase chain reaction (PCR)--denaturing gradient gel electrophoresis (DGGE). These observations suggested that the combination of inorganic nutrients with chemical, mineral, and biological treatment could improve the PBDE removal efficiency. However, the combination of H2O2 and biological treatment processes is the most efficient technology. This combination of technologies would not cause adverse effects on the subsequent bioremediation process. Therefore, this work offers a potential alternative for the remediation of soil contaminated with PBDE pollutants.

  19. Microencapsulation decreases the skin absorption of N,N-diethyl-m-toluamide (DEET).

    Science.gov (United States)

    Kasting, Gerald B; Bhatt, Varsha D; Speaker, Tycho J

    2008-03-01

    The insect repellent N,N-diethyl-3-methylbenzamide (DEET) is widely used and is generally regarded as safe when used according to label instructions. Yet many studies have shown it to be absorbed through the skin. The objective of this study was to determine whether the skin absorption rate of DEET could be decreased while maintaining an evaporation rate consistent with effective repellency. To this end, an aqueous suspension containing 14C-DEET (15%w/w) entrapped in walled polysaccharide microcapsules was prepared and tested for skin absorption in vitro using modified Franz cells maintained in a fume hood. The control formulation was 15%w/w DEET in ethanol. Two doses (3 microL and 5 microL per 0.79 cm2 cell) of each formulation were applied to split-thickness human cadaver skin (n=8/dose), and permeation was monitored for 24h. The microencapsulated DEET formulation lead to a 25-35% reduction of radiolabel permeation compared to the ethanolic DEET formulation. Skin levels of radioactivity at 24h were comparable, indicating that DEET evaporation from the microencapsulated formulation was comparable to or greater than that from ethanol. Hence microencapsulation increased the ratio of DEET evaporation rate to skin penetration rate relative to unencapsulated control in this in vitro study.

  20. (E-N,N-Diethyl-2,6-diisopropyl-4-[2-(4-nitrophenylethenyl]aniline

    Directory of Open Access Journals (Sweden)

    Heiner Detert

    2013-12-01

    Full Text Available The title compound, C24H32N2O2, was prepared by Horner olefination of 4-diethylamino-3,5-diisopropylbenzaldehyde and diethyl p-nitrobenzylphosphonate. There are two independent molecules (A and B in the asymmetric unit. Their main axes, defined by the line connecting the N atoms of the nitro and amino groups, open an angle of 79.42 (3°. Steric hindrance around the amino group is reflected in a long aryl C—N bond [1.434 (3 Å for molecule A and 1.440 (3 Å for molecule B], a pyramidal geometry [angle sum = 350.0 (2° for molecule A and 349.6 (2° for molecule B], and dihedral angles between the phenylene group and the plane defined by the CH2—N—CH2 unit of 86.9 (3° for molecule A and 88.3 (3° for molecule B. This gives structural support for the electronic decoupling of the amino group from the nearly planar nitrostilbene moiety (r.m.s. deviation for C, N and O atoms = 0.097 for molecule A and 0.107 Å for molecule B.

  1. Removal of diethyl phthalate from aqueous phase using magnetic poly(EGDMA-VP) beads.

    Science.gov (United States)

    Özer, Elif Tümay; Osman, Bilgen; Kara, Ali; Beşirli, Necati; Gücer, Seref; Sözeri, Hüseyin

    2012-08-30

    The barium hexaferrite (BaFe(12)O(19)) containing magnetic poly(ethylene glycol dimethacrylate-vinyl pyridine), (mag-poly(EGDMA-VP)) beads (average diameter=53-212 μm) were synthesized and characterized. Their use as an adsorbent in the removal of diethyl phthalate (DEP) from an aqueous solution was investigated. The mag-poly(EGDMA-VP) beads were prepared by copolymerizing of 4-vinyl pyridine (VP) with ethylene glycol dimethacrylate (EGDMA). The mag-poly(EGDMA-VP) beads were characterized by N(2) adsorption/desorption isotherms (BET), vibrating sample magnetometer (VSM), X-ray powder diffraction (XRD), elemental analysis, scanning electron microscope (SEM) and swelling studies. At a fixed solid/solution ratio, the various factors affecting the adsorption of DEP from aqueous solutions such as pH, initial concentration, contact time and temperature were analyzed. The maximum DEP adsorption capacity of the mag-poly(EGDMA-VP) beads was determined as 98.9 mg/g at pH 3.0, 25°C. All the isotherm data can be fitted with both the Langmuir and the Dubinin-Radushkevich isotherm models. The pseudo first-order, pseudo-second-order, Ritch-second-order and intraparticle diffusion models were used to describe the adsorption kinetics. The thermodynamic parameters obtained indicated the exothermic nature of the adsorption. The DEP adsorption capacity did not change after 10 batch successive reactions, demonstrating the usefulness of the magnetic beads in applications.

  2. Interaction of diethyl aniline methylphosphonate with DNA: Spectroscopic and isothermal titration calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Lu Yan, E-mail: yanlu2001@sohu.co [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang, Henan 453007 (China); Xu Meihua; Wang Gongke; Zheng Yun [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang, Henan 453007 (China)

    2011-05-15

    In this study the diethyl aniline methylphosphonate (DAM) was synthesized, the interaction of DAM with ct-DNA has been investigated by fluorescence spectra, UV spectra, molecular modeling and isothermal titration calorimetry (ITC). The binding constant of DAM to ct-DNA calculated from both isothermal titration calorimetry and fluorescence spectra were found to be in the 10{sup 4} M{sup -1} range. According to the ethidium bromide displacement studies, UV spectra and isothermal titration calorimetry experimental results, it can be concluded that DAM is an intercalator that can slide into the G-C rich region of ct-DNA. Furthermore, the results obtained from molecular modeling corroborated the experimental results obtanied from spectroscopic and ITC investigations. At the same time, fluorescence spectra suggested that the mechanism of the interaction of DAM to ct-DNA was a static enhancing type. ITC data showed that ct-DNA/DAM binding is enthalpy controlled. - Research highlights: The interaction of DAM with ct-DNA is a static enhancing type. DAM can slide into the G-C rich region of ct-DNA. The binding of DAM to ct-DNA is enthalpy controlled. The hydrogen bonding forces play an essential role in the binding process.

  3. Tween as a Substitute for Diethyl Ether in the Formalin-Ether Sedimentation Technique

    Directory of Open Access Journals (Sweden)

    NA Ahmadi

    2007-10-01

    Full Text Available Background: Tween as a substitute for diethyl ether in the formalin-ether sedimentation technique was evaluated for para­site detection.Methods: Fresh fecal material free of parasites with 10% formalin to prepare standardized specimen was thoroughly pooled. This specimen was divided into 5 equal portions; one was without infection, and each of the others was individually seeded with Entamoeba coli, and Giardia lamblia cysts, ova of Ascaris lumbericoides, and Hymenolepis nana. Six hundred and eighty four slides including 228 stool samples for each of formalin-tween, formalin-ether and direct wet mount proce­dures were examined.Results: The sensitivity of above mentioned procedures were computed 72.1%, 55% and 30 %; their negative predictive value were 69.3%, 58.3% and 47.3%; and their false negative error rate were 27.9%, 45% and 70%, respectively. There were no false-positive results among the 264 specimens previously identified as negative for the presence of intestinal para­sites. Therefore, specificity for each technique was 100%.Conclusion: In the range of our study, formalin-tween method proved to be equivalent to or better than formalin-ether tech­nique in concentrating parasite eggs, and cysts, as well as in maintaining characteristic morphology. Tween is more stable, safer, cheaper, and less flammable than that of ether; and promises to be a useful alternative to ether.

  4. A multiple shock tube and chemical kinetic modeling study of diethyl ether pyrolysis and oxidation.

    Science.gov (United States)

    Yasunaga, K; Gillespie, F; Simmie, J M; Curran, H J; Kuraguchi, Y; Hoshikawa, H; Yamane, M; Hidaka, Y

    2010-09-02

    The pyrolysis and oxidation of diethyl ether (DEE) has been studied at pressures from 1 to 4 atm and temperatures of 900-1900 K behind reflected shock waves. A variety of spectroscopic diagnostics have been used, including time-resolved infrared absorption at 3.39 mum and time-resolved ultraviolet emission at 431 nm and absorption at 306.7 nm. In addition, a single-pulse shock tube was used to measure reactant, intermediate, and product species profiles by GC samplings at different reaction times varying from 1.2 to 1.8 ms. A detailed chemical kinetic model comprising 751 reactions involving 148 species was assembled and tested against the experiments with generally good agreement. In the early stages of reaction the unimolecular decomposition and hydrogen atom abstraction of DEE and the decomposition of the ethoxy radical have the largest influence. In separate experiments at 1.9 atm and 1340 K, it is shown that DEE inhibits the reactivity of an equimolar mixture of hydrogen and oxygen (1% of each).

  5. Pharmacokinetic profile of a new matrix-type transdermal delivery system: diclofenac diethyl ammonium patch.

    Science.gov (United States)

    Devi, K; Paranjothy, K L

    1999-05-01

    A transdermal delivery system containing the anti-inflammatory analgesic diclofenac diethyl ammonium in an ethyl hexyl acrylate and vinyl acetate pressure-sensitive adhesive system was developed for percutaneous absorption. These patches were subjected to in vitro permeation and permeation enhancement studies through rat skin using a specially designed diffusion cell. Further, the work deals with percutaneous absorption studies carried out on both animals and human volunteers. The pharmacokinetic parameters calculated from the blood levels of the drug reveal a profile typical of a sustained-release formulation, with the ability to maintain adequate plasma levels for 24 hr (i.e., up to the next application). (Area under the curve [AUC]: 4.356 +/- 1.3 mcg/ml.hr in animals and 0.442 +/- 0.053 mcg/ml.hr in humans; Tmax was 8 hr in both the cases, whereas Cmax was 0.288 +/- 0.088 mcg/ml in animals and 0.034 +/- .008 mcg/ml in human volunteers.) The amount of the drug bioavailable for targeting the sites of action is lower than via the oral route, but the absorbed dose appears to be adequate for therapeutic use, particularly because of the absence of side effects.

  6. Dissipation of diethyl aminoethyl hexanoate (DA-6) residues in pakchoi, cotton crops and soil.

    Science.gov (United States)

    Jiang, Yaping; Jiang, Yuting; He, Shun; Zhang, Heli; Pan, Canping

    2012-04-01

    QuEChERS procedure and acetonitrile extraction, oscillation and ultrasonic procedure followed by GC-MS and LC-MS/MS (QqQ) detections were established for determination of diethyl aminoethyl hexanoate (DA-6) residues in pakchoi, cotton leaf, cotton seed and soil. At concentration levels of 0.005-1 mg kg(-1), recoveries were in the range of 80.5%-103.3%, with a RSD less than 14.2%. The LOQs of methods were 0.005, 0.003, 0.005 and 0.001 mg kg(-1) for the pakchoi, cotton leaf, soil and cotton seed samples, respectively. DA-6 was applied in supervised field trials at GAP conditions to pakchoi and cotton. It was found that the dissipation half-lives of DA-6 were 5.4-8.2 days and 1.1-2.2 days and 1.5-1.9 days in cotton crop, pakchoi and soil respectively. At harvest, no detectable residues (cotton samples. However, residues was detected in pakchoi (0.007-0.013 mg/kg) in Beijing and soil (0.008-0.014 mg/kg) in Changsha in 2008.

  7. Anticancer activity of Cynodon dactylon L. root extract against diethyl nitrosamine induced hepatic carcinoma

    Directory of Open Access Journals (Sweden)

    R Kowsalya

    2015-01-01

    Full Text Available Background: Hepatocellular carcinoma is one of the most common cancers and a lethal disease. In view of the limited treatment and a grave prognosis of liver cancer, preventive control has been emphasized. Materials and Methods: The methanolic extract of roots of Cynodon dactylon was screened for its hepato-protective activity in diethyl nitrosamine (DEN induced liver cancer in Swiss albino mice. The plant extract at a dose of 50 mg/kg was administered orally once a week, up to 30 days after DEN administration. The animals were sacrificed; blood sample and liver tissue were collected and used for enzyme assay such as, asparatate amino transferase (AST, alanine aminotransferase (ALT, catalase (CAT, glutathione peroxidase (GPx and glutathione-S-transferase (GST. The liver marker enzymes AST and ALT produced signifi cant results in the protective action. Results: The antioxidant enzyme assay results concerning the improved activity of GPx, GST and CAT. These results concluded that enhanced levels of antioxidant enzyme and reduced amount of serum amino transaminase, which are suggested to be the major mechanisms of C. dactylon root extract in protecting the mice from hepatocarcinoma induced by DEN. These biochemical observations were supplemented by histopathological examination of liver sections. Conclusion: The methanolic extract of C. dactylon possesses signifi cant anticancer properties

  8. Modification by chloramphenicol of diethyl sulphate-induced male recombination frequency in Drosophila melanogaster.

    Science.gov (United States)

    Miglani, G S; Kaur, N P

    1995-06-01

    To study the effect of chloramphenicol (CPL, an inhibitor of protein synthesis) on diethyl sulphate (DES, a potent mutagen) induced male recombination frequency, the F1 (+/aristaless dumpy black cinnabar, al dp b cn) larvae of D. melanogaster were given a pre- or post-treatment of CPL with DES during the first or second half of larval life. In order to determine sensitivity of different germ cell stages to the induction and modification of male recombination frequency, five 3-day broods were taken from every F1 male. DES showed toxic effect on egg-to-adult development. DES was found to be a potent recombinogen. Several cases of non-reciprocal male recombination were recorded. The most frequent recombinant phenotype observed was b cn followed by cn and al. Majority of the recombinants appeared in clusters suggesting their pre-meiotic origin. DES produced male recombination at a stage where only primary spermatocytes were present in the larval testes. CPL when given as a pre- or post-treatment with DES revealed highest frequency of male recombination in broods that represented effect of treatment on spermatogonia predominantly. CPL enhanced the overall level of male recombination produced by DES in both pre- and post-treatments. The results suggested the role of protein synthesis in induction of male recombination in D. melanogaster. In addition, the present experiments give a methodology of enhancing the frequency of chemically-induced male recombination.

  9. Environmental release, environmental concentrations, and ecological risk of N,N-Diethyl-m-toluamide (DEET).

    Science.gov (United States)

    Aronson, Dallas; Weeks, John; Meylan, Bill; Guiney, Patrick D; Howard, Philip H

    2012-01-01

    N,N-Diethyl-m-toluamide's (DEET) commercial use as an insect repellent and other reported uses are reviewed. Evidence that DEET is reaching the environment mainly from consumer use of DEET-containing insect repellent includes studies reporting higher concentrations of DEET in surface water and wastewater samples during the summer months, the presence of DEET in on-site septic tank effluent at concentrations similar to that reported in wastewater treatment plant (WWTP) influent, and changes in WWTP effluent concentrations before and after the introduction of a DEET replacement in Germany. Its detected concentrations in influent and effluent of WWTP and surface water worldwide are reviewed and correlations between DEET usage and wastewater effluent concentrations are analyzed. The removability during wastewater treatment is also evaluated. A correlation between commercial DEET use in a metropolitan area and concentrations in WWTP effluents was assessed, and 2 different models were used to predict DEET concentrations in rivers and streams throughout the United States. Ecological toxicity data are reviewed for acute studies and for chronic values that are available for Daphnia magna and algae. The ecological risk of DEET usage is evaluated by examining the relationship of the expected dose/response to observed concentrations. Copyright © 2011 SETAC.

  10. Effect of aging process on adsorption of diethyl phthalate in soils amended with bamboo biochar.

    Science.gov (United States)

    Zhang, Xiaokai; Sarmah, Ajit K; Bolan, Nanthi S; He, Lizhi; Lin, Xiaoming; Che, Lei; Tang, Caixian; Wang, Hailong

    2016-01-01

    Biochar is a carbonaceous sorbent and can be used as a potential material to reduce the bioavailability of organic pollutants in contaminated soils. In the present study, the adsorption and desorption of diethyl phthalate (DEP) onto soils amended with bamboo biochar was investigated with a special focus on the effect of biochar application rates and aging conditions on the adsorption capacity of the soils. Biochar amendment significantly enhanced the soil adsorption of DEP that increased with increasing application rates of biochar. However, the adsorption capacity decreased by two aging processes (alternating wet and dry, and constantly moist). In the soil with low organic carbon (OC) content, the addition of 0.5% biochar (without aging) increased the adsorption by nearly 98 times compared to the control, and exhibited the highest adsorption capacity among all the treatments. In the soil with high OC content, the adsorption capacity in the treatment of 0.5% biochar without aging was 3.5 and 3 times greater than those of the treatments of biochar aged by alternating wet and dry, and constantly moist, respectively. Moreover, constantly moist resulted in a greater adsorption capacity than alternating wet and dry treatments regardless of biochar addition. This study revealed that biochar application enhanced soil sorption of DEP, however, the enhancement of the adsorption capacity was dependent on the soil organic carbon levels, and aging processes of biochar.

  11. Synthesis, crystal structure, crystal growth and physical properties of N,N-diethyl anilinium picrate

    Science.gov (United States)

    Subramaniyan @ Raja, R.; Anandha Babu, G.; Ramasamy, P.

    2011-11-01

    Crystalline substance of N,N-diethyl anilinium picrate (NNDEAP) has been synthesized and single crystals of NNDEAP were successfully grown for the first time by the slow evaporation solution growth technique at room temperature with dimensions 14×10×10 mm3. The formation of the new crystal has been confirmed by single crystal X-ray diffraction studies. The structural perfection of the grown crystal was analyzed by high resolution X-ray diffraction (HRXRD) measurements. The functional groups of NNDEAP have been identified by Fourier transform infrared spectral studies. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) have also been carried out and the thermal behavior of NNDEAP has been studied. The UV-vis-NIR studies have been carried out to identify the optical transmittance and the cut off wavelength of NNDEAP is identified. The dielectric loss and the dielectric constant as a function of frequency and temperature were measured for the grown crystal and the nature of variation of dielectric constant εr and dielectric losses (tan δ) were studied. Vicker's hardness test has been carried out on NNDEAP to measure the load dependent hardness. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser.

  12. Neurotoxicity and mode of action of N, N-diethyl-meta-toluamide (DEET.

    Directory of Open Access Journals (Sweden)

    Daniel R Swale

    Full Text Available Recent studies suggest that N, N-diethyl-meta-toluamide (DEET is an acetylcholinesterase inhibitor and that this action may result in neurotoxicity and pose a risk to humans from its use as an insect repellent. We investigated the mode of action of DEET neurotoxicity in order to define the specific neuronal targets related to its acute toxicity in insects and mammals. Although toxic to mosquitoes (LD50 ca. 1.5 µg/mg, DEET was a poor acetylcholinesterase inhibitor (<10% inhibition, even at a concentration of 10 mM. IC50 values for DEET against Drosophila melanogaster, Musca domestica, and human acetylcholinesterases were 6-12 mM. Neurophysiological recordings showed that DEET had excitatory effects on the housefly larval central nervous system (EC50: 120 µM, but was over 300-fold less potent than propoxur, a standard anticholinesterase insecticide. Phentolamine, an octopamine receptor antagonist, completely blocked the central neuroexcitation by DEET and octopamine, but was essentially ineffective against hyperexcitation by propoxur and 4-aminopyridine, a potassium channel blocker. DEET was found to illuminate the firefly light organ, a tissue utilizing octopamine as the principal neurotransmitter. Additionally, DEET was shown to increase internal free calcium via the octopamine receptors of Sf21 cells, an effect blocked by phentolamine. DEET also blocked Na(+ and K(+ channels in patch clamped rat cortical neurons, with IC50 values in the micromolar range. These findings suggest DEET is likely targeting octopaminergic synapses to induce neuroexcitation and toxicity in insects, while acetylcholinesterase in both insects and mammals has low (mM sensitivity to DEET. The ion channel blocking action of DEET in neurons may contribute to the numbness experienced after inadvertent application to the lips or mouth of humans.

  13. Experimental and Numerical Investigation of Ethanol/Diethyl Ether Mixtures in a CI Engine

    KAUST Repository

    Sivasankaralingam, Vedharaj

    2016-10-17

    The auto-ignition characteristics of diethyl ether (DEE)/ethanol mixtures are investigated in compression ignition (CI) engines both numerically and experimentally. While DEE has a higher derived cetane number (DCN) of 139, ethanol exhibits poor ignition characteristics with a DCN of 8. DEE was used as an ignition promoter for the operation of ethanol in a CI engine. Mixtures of DEE and ethanol (DE), i.e., DE75 (75% DEE + 25% ethanol), DE50 (50% DEE + 50% ethanol) and DE25 (25% DEE + 75% ethanol), were tested in a CI engine. While DE75 and DE50 auto-ignited at an inlet air pressure of 1.5 bar, DE25 failed to auto-ignite even at boosted pressure of 2 bar. The peak in-cylinder pressure for diesel and DE75 were comparable, while DE50 showed reduced peak in-cylinder pressure with delayed start of combustion (SOC). Numerical simulations were conducted to study the engine combustion characteristics of DE mixture. A comprehensive detailed chemical kinetic model was created to represent the combustion of DE mixtures. The detailed mechanism was then reduced using standard direct relation graph (DRG-X) method and coupled with 3D CFD code, CONVERGE, to simulate the experimental data. The simulation results showed that the effects of physical properties on DE50 combustion are negligible. Simulations of DE50 mixture revealed that the combustion is nearly homogenous, while diesel (n-heptane used as a surrogate) and DE75 showed similar combustion behavior with flame liftoff and diffusion controlled combustion. Diesel exhibited auto-ignition at an equivalence ratio of 2, while DE75 and DE50 showed auto-ignition in the equivalence ratio range of 1-1.5 and 0-1, respectively. The experiments and numerical simulations demonstrate how the high reactivity of DEE supports the auto-ignition of ethanol, while ethanol acts as a radical scavenger.

  14. Impact of the safener Mefenpyr-diethyl on herbicide resistance evolution in Alopecurus myosuroides (Huds. biotypes

    Directory of Open Access Journals (Sweden)

    Rosenhauer, Maria

    2016-02-01

    Full Text Available The evolution of herbicide resistance is an important topic in plant protection and agricultural practice. Safeners are commonly used in herbicides to protect crops against herbicidal damage. Although no effect on the weed control is expected, it has been theorized that the rate of evolution of non-target site resistance (NTSR in weeds in cereals may be enhanced by use of herbicide products containing safeners. One of the most important safeners in cereals is mefenpyr-diethyl. Therefore, the possible influence of mefenpyr on herbicide resistance was studied in cooperative trials between Bayer CropScience (BCS, F-Höchst and FH Bingen. The trials tested in parallel different herbicide resistant black-grass (Alopecurus myosuroides (Huds. biotypes under greenhouse conditions. The biotypes where chosen due to known NTSR against Atlantis WG® (4 highly resistant and 5 moderately resistant as well as two susceptible biotypes. The populations were treated with the following three herbicide/safener regimes in six concentrations adjusted according to the anticipated biotype resistance levels. (1 mesosulfuron + iodosulfuron + without safener formulation, (2 mesosulfuron + iodosulfuron + constant mefenpyr concentration (45g/ha, (3 mesosulfuron + iodosulfuron + varying mefenpyr concentrations (ratio 5:1:15. The treatments were applied in post-emergence based on mesosulfuron to iodosulfuron ratios in Atlantis WG® (5:1. The trials were assessed visually (% effect and by fresh weight. Dose-response curves were performed and ED50 values for each treatment and biotype were calculated. Results showed a varying effect of safeners which was in the most cases negligible. Depending on the biotypes mostly no impact on the safener was found for herbicide resistance. In conclusion, the trials from Bingen and F-Höchst gave evidence, that there is no significant and consistent influence of the safener mefenpyr on evolution of NTSR black-grass.

  15. Degradation of an Ethylene Carbonate/Diethyl Carbonate Mixture by Using Ionizing Radiation.

    Science.gov (United States)

    Wang, Furong; Varenne, Fanny; Ortiz, Daniel; Pinzio, Valentin; Mostafavi, Mehran; Le Caër, Sophie

    2017-04-16

    The reactivity of ethylene carbonate (EC) and of a EC/diethyl carbonate (DEC) mixture was studied under ionizing radiation to mimic the aging phenomena that occur in lithium-ion batteries. Picosecond-pulse radiolysis experiments showed that the attachment of the electron to the EC molecule is ultrafast (k(e(-)EC +EC)=1.3×10(9)  L mol(-1)  s(-1) at 46 °C). This reaction rate is accelerated by a factor of 5.7 compared with the electron attachment to propylene carbonate, which implies that the presence of the methyl group significantly slows the reaction. In a 50:50 EC/DEC mixture, just after the electron pulse the electron is solvated by a mixture of EC and DEC molecules, but its fast decay is attributed exclusively to electron attachment to the EC molecule. Stable products detected after steady-state irradiation were mainly H2 , CH4 , CO, and CO2 . The evolution of the radiolytic yields with the EC fraction shows that H2 and CH4 did not exhibit linear behavior, whereas CO and CO2 did. Indeed, H2 and CH4 mainly arise from the excited state of DEC, the formation of which is significantly affected by the evolution of the dielectric constant of the mixture and by the electron attachment to EC. CO formation is mainly due to the reactivity of the EC molecule, which is not affected in the mixture, as proven by pulse-radiolysis experiments. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Composition at the CuInSe{sub 2}/ZnO interface: Copper depletion induced by diethyl-zinc

    Energy Technology Data Exchange (ETDEWEB)

    Hofmann, A.; Janocha, E.; Kelleter, F.; Pettenkofer, C. [Helmholtz-Zentrum-Berlin, Institute for Silicon Photovoltaics, Albert-Einstein-Str. 15, 12489, Berlin (Germany)

    2014-09-15

    The interface formation between epitaxial CuInSe{sub 2}(112) films and ZnO deposited by metal-organic MBE is investigated by photoelectron spectroscopy. Reaction of diethyl-zinc with CuInSe{sub 2} leads to the formation of an intrinsic ZnSe layer and copper depletion of the interface. This is associated with Zn doping of the chalcopyrite surface and a Fermi-level shift toward the conduction band. The implications on the band alignment are discussed. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. Enhanced molecular order in polythiophene films electropolymerized in a mixed electrolyte of anionic surfactants and boron trifluoride diethyl etherate.

    Science.gov (United States)

    Santoso, Handoko T; Singh, Virendra; Kalaitzidou, Kyriaki; Cola, Baratunde A

    2012-03-01

    We synthesized polythiophene (PTh) films on stainless steel electrodes using chronoamperometry in boron trifluoride diethyl etherate (BFEE) electrolyte with anionic surfactants. The presence of the anionic surfactants in BFEE reduced the oxidation potential of thiophene and increased the oxidation current during electropolymerization. The measured in-plane electrical conductivity of PTh films synthesized in the presence of anionic surfactants was up to 300% higher than that of films synthesized under similar conditions without surfactants. The observed increase in conductivity reflects the improved order and packing of polymer chains revealed by X-ray diffraction.

  18. INVESTIGATION ON THE RELATIONSHIP BETWEEN INTRINSIC VISCOSITY AND MOLECULAR WEIGHT OF POLY (VINYL CHLORIDE-DIETHYL MALEATE)

    Institute of Scientific and Technical Information of China (English)

    ZHENG Changren; PAN Hongqing; LIN Shenghe; QIAN Jun; DUAN Qin

    1987-01-01

    A poly (vinylchloride-diethyl maleate) copolymer has been fractionated by repeated precipitation method. All fractions and the unfractionated sample have been characterized by viscometry, dynamic osmometry, Zimm static osmometry, light scattering and gel permeation chromatography. After correction for polydispersity, a [η] ~ M relationship for monodisperse polymer solutions has been obtained:[η] = 1.99 × 10-3M0.87 (ml/g, at 25℃, in cyclohexanone)For the copolymer solution in THF, the second virial coefficient A2 decreases as the molecular weight increases. The relationship is A2 = 2 slope (-M(n) RT)-1/2.

  19. Ionic liquids as efficient phase-transfer catalysts for the solid base-promoted monoalkylation of diethyl malonate

    Institute of Scientific and Technical Information of China (English)

    Hui Sun; Juan Li; Xiao Chen Cai; Dong Jiang; Li Yi Dai

    2007-01-01

    Ionic liquids (ILs) based on 1,3-dialkylimidazolium and teraalkylammonium cations were employed as a series of efficient,environmentally benign phase-transfer catalysts (PTCs) for the base-promoted monoalkylation of diethyl malonate. The influence of various heterogeneous bases on yields was studied. Good yields and high selectivity were obtained. Solvent-free, mild reaction condition, short reaction time, and easy purification were the merits of this method. The catalytic system (IL-base) could also be recycled after the extraction of products with ether.

  20. On-line solid phase extraction-high performance liquid chromatography–isotope dilution–tandem mass spectrometry approach to quantify N,N-diethyl-m-toluamide and oxidative metabolites in urine

    Energy Technology Data Exchange (ETDEWEB)

    Kuklenyik, Peter; Baker, Samuel E.; Bishop, Amanda M.; Morales-A, Pilar; Calafat, Antonia M., E-mail: aic7@cdc.gov

    2013-07-17

    Graphical abstract: -- Highlights: •A fast assay to quantify the concentrations of N,N-Diethyl-m-Toluamide and two urinary metabolites was developed •It uses online SPE, reversed phase HPLC and tandem mass spectrometry •The method is precise and accurate with limits of detection ≤1 ng mL{sup −1} -- Abstract: Human exposure to N,N-diethyl-m-toluamide (DEET) occurs because of the widespread use of DEET as an active ingredient in insect repellents. However, information on the extent of such exposure is rather limited. Therefore, we developed a fast on-line solid phase extraction–high performance liquid chromatography–isotope dilution tandem mass spectrometry (HPLC-MS/MS) method to measure in urine the concentrations of DEET and two of its oxidative metabolites: N,N-diethyl-3-(hydroxymethyl)benzamide and 3-(diethylcarbamoyl)benzoic acid (DCBA). To the best of our knowledge, this is the first HPLC-MS/MS method for the simultaneous quantification of DEET and its select metabolites in human urine. After enzymatic hydrolysis of the conjugated species in 0.1 mL of urine, the target analytes were retained and pre-concentrated on a monolithic column, separated from each other and from other urinary biomolecules on a reversed-phase analytical column, and detected by atmospheric pressure chemical ionization in positive ion mode. The limits of detection ranged from 0.1 ng mL{sup −1} to 1.0 ng mL{sup −1}, depending on the analyte. Accuracy ranged between 90.4 and 104.9%, and precision ranged between 5.5 and 13.1% RSD, depending on the analyte and the concentration. We tested the usefulness of this method by analyzing 75 urine samples collected anonymously in the Southeastern United States in June 2012 from adults with no known exposure to DEET. Thirty eight samples (51%) tested positive for at least one of the analytes. We detected DCBA most frequently and at the highest concentrations. Our results suggest that this method can be used for the analysis of a large

  1. Improving Vegetable Oil Fueled CI Engine Characteristics Through Diethyl Ether Blending

    KAUST Repository

    Vedharaj, S.

    2016-12-01

    In this research, the flow and ignition properties of vegetable oil (VO) are improved by blending it with diethyl ether (DEE). DEE, synthesized from ethanol, has lower viscosity than diesel and VO. When DEE is blended with VO, the resultant DEEVO mixtures have favorable properties for compression ignition (CI) engine operation. As such, DEEVO20 (20% DEE + 80% VO) and DEEVO40 (40% DEE + 60% VO) were initially considered in the current study. The viscosity of VO is 32.4*10−6 m2/s; the viscosity is reduced with the increase of DEE in VO. In this study, our blends were limited to a maximum of 40% DEE in VO. The viscosity of DEEVO40 is 2.1*10−6 m2/s, which is comparable to that of diesel (2.3*10−6 m2/s). The lower boiling point and flash point of DEE improves the fuel spray and evaporation for DEEVO mixtures. In addition to the improvement in physical properties, the ignition quality of DEEVO mixtures is also improved, as DEE is a high cetane fuel (DCN = 139). The ignition characteristics of DEEVO mixtures were studied in an ignition quality tester (IQT). There is an evident reduction in ignition delay time (IDT) for DEEVO mixtures compared to VO. The IDT of VO (4.5 ms), DEEVO20 (3.2 ms) and DEEVO40 (2.7 ms) was measured in IQT. Accordingly, the derived cetane number (DCN) of DEEVO mixtures increased with the increase in proportion of DEE. The reported mixtures were also tested in a single cylinder CI engine. The start of combustion (SOC) was advanced for DEEVO20 and DEEVO40 compared to diesel, which is attributed to the high DCN of DEEVO mixtures. On the other hand, the peak heat release rate decreased for DEEVO mixtures compared to diesel. Gaseous emissions such as nitrogen oxide (NOX), total hydrocarbon (THC) and smoke were reduced for DEEVO mixtures compared to diesel. The physical and ignition properties of VO are improved by the addition of DEE, and thus, the need for the trans-esterification process is averted. Furthermore, this blending strategy is simpler

  2. Diethyl Ether as an Ignition Enhancer for Naphtha Creating a Drop in Fuel for Diesel

    KAUST Repository

    Vallinayagam, R.

    2016-12-01

    Direct use of naphtha in compression ignition (CI) engines is not advisable because its lower cetane number negatively impacts the auto ignition process. However, engine or fuel modifications can be made to operate naphtha in CI engines. Enhancing a fuel’s auto ignition characteristics presents an opportunity to use low cetane fuel, naphtha, in CI engines. In this research, Di-ethyl ether (DEE) derived from ethanol is used as an ignition enhancer for light naphtha. With this fuel modification, a “drop-in” fuel that is interchangeable with existing diesel fuel has been created. The ignition characteristics of DEE blended naphtha were studied in an ignition quality tester (IQT); the measured ignition delay time (IDT) for pure naphtha was 6.9 ms. When DEE was added to naphtha, IDT decreased and D30 (30% DEE + 70% naphtha) showed comparable IDT with US NO.2 diesel. The derived cetane number (DCN) of naphtha, D10 (10% DEE + 90% naphtha), D20% DEE + 80% naphtha) and D30 were measured to be 31, 37, 40 and 49, respectively. The addition of 30% DEE in naphtha achieved a DCN equivalent to US NO.2 diesel. Subsequent experiments in a CI engine exhibited longer ignition delay for naphtha compared to diesel. The peak in-cylinder pressure is higher for naphtha than diesel and other tested fuels. When DEE was added to naphtha, the ignition delay shortened and peak in-cylinder pressure is reduced. A 3.7% increase in peak in-cylinder pressure was observed for naphtha compared to US NO.2 diesel, while D30 showed comparable results with diesel. The pressure rise rate dropped with the addition of DEE to naphtha, thereby reducing the ringing intensity. Naphtha exhibited a peak heat release rate of 280 kJ/m3deg, while D30 showed a comparable peak heat release rate to US NO.2 diesel. The amount of energy released during the premixed combustion phase decreased with the increase of DEE in naphtha. Thus, this study demonstrates the suitability of DEE blended naphtha mixtures as a

  3. cis-Dichlorido(1,3-dimesitylimidazolidin-2-ylidene(2-formylbenzylidene-κ2C,Oruthenium diethyl ether solvate

    Directory of Open Access Journals (Sweden)

    Christian Slugovc

    2010-02-01

    Full Text Available The title compound, [RuCl2(C8H6O(C21H26N2]·C4H10O, contains a catalytically active ruthenium carbene complex of the `second-generation Grubbs/Hoveyda' type with Ru in a square-pyramidal coordination, the apex of which is formed by the benzylidene carbene atom with Ru=C 1.827 (2 Å. The complex shows the uncommon cis, rather than the usual trans, arrangement of the two chloride ligands, with Ru—Cl bond lengths of 2.3548 (6 and 2.3600 (6 Å, and a Cl—Ru—Cl angle of 89.76 (2°. This cis configuration is desirable for certain applications of ring-opening metathesis polymerization (ROMP of strained cyclic olefins. The crystalline solid is a diethyl ether solvate, which is built up from a porous framework of Ru complexes held together by π–π stacking and C—H...Cl and C—H...O interactions. The disordered diethyl ether solvent molecules are contained in two independent infinite channels, which extend parallel to the c axis at x,y = 0,0 and x,y = {1over 2},{1over 2} and have solvent-accessible void volumes of 695 and 464 Å3 per unit cell.

  4. Comparative study of diethyl phthalate degradation by UV/H2O2 and UV/TiO2: kinetics, mechanism, and effects of operational parameters.

    Science.gov (United States)

    Song, Chengjie; Wang, Liping; Ren, Jie; Lv, Bo; Sun, Zhonghao; Yan, Jing; Li, Xinying; Liu, Jingjing

    2016-02-01

    The photodegradation of diethyl phthalate (DEP) by UV/H2O2 and UV/TiO2 is studied. The DEP degradation kinetics and multiple crucial factors effecting the clearance of DEP are investigated, including initial DEP concentration ([DEP]0), initial pH values (pH0), UV light intensity, anions (Cl(-), NO(3-), SO4 (2-), HCO3 (-), and CO3 (2-)), cations (Mg(2+), Ca(2+), Mn(2+), and Fe(3+)), and humic acid (HA). Total organic carbon (TOC) removal is tested by two treatments. And, cytotoxicity evolution of DEP degradation intermediates is detected. The relationship between molar ratio ([H2O2]/[DEP] or [TiO2]/[DEP]) and degradation kinetic constant (K) is also studied. And, the cytotoxicity tests of DEP and its degradation intermediates in UV/H2O2 and UV/TiO2 treatments are researched. The DEP removal efficiency of UV/H2O2 treatment is higher than UV/TiO2 treatment. The DEP degradation fitted a pseudo-first-order kinetic pattern under experimental conditions. The K linearly related with molar ratio in UV/H2O2 treatment while nature exponential relationship is observed in the case of UV/TiO2. However, K fitted corresponding trends better in H2O2 treatment than in TiO2 treatment. The Cl(-) is in favor of the DEP degradation in UV/H2O2 treatment; in contrast, it is disadvantageous to the DEP degradation in UV/TiO2 treatment. Other anions are all disadvantageous to the DEP degradation in two treatments. Fe(3+) promotes the degradation rates significantly. And, all other cations in question inhibit the degradation of DEP. HA hinders DEP degradation in two treatments. The intermediates of DEP degradation in UV/TiO2 treatment are less toxic to biological cell than that in UV/H2O2 treatment.

  5. Synthesis and Physicochemical Characterization of a Diethyl Ester Prodrug of DTPA and Its Investigation as an Oral Decorporation Agent in Rats.

    Science.gov (United States)

    Huckle, James E; Sadgrove, Matthew P; Leed, Marina G D; Yang, Yu-Tsai; Mumper, Russell J; Semelka, Richard C; Jay, Michael

    2016-07-01

    The increasing threats of nuclear terrorism have made the development of medical countermeasures a priority for international security. Injectable formulations of diethylenetriaminepentaacetic acid (DTPA) have been approved by the FDA; however, an oral formulation is more amenable in a mass casualty situation. Here, the diethyl ester of DTPA, named C2E2, is investigated for potential as an oral treatment for internal radionuclide contamination. C2E2 was synthesized and characterized using NMR, MS, and elemental analysis. The physiochemical properties of solubility, lipophilicity, and stability were investigated in order to predict its oral bioavailability. Finally, an animal efficacy study was conducted in Sprague Dawley rats pre-contaminated by intramuscular injection with (241)Am(NO3)3 to establish effectiveness of the therapy via the oral route. Synthesis of C2E2 yielded a crystalline powder with high solubility and improved lipophilicity over DTPA. The ester was stable in both simulated gastric and intestinal fluids over the anticipated time course of absorption. Capsules containing C2E2 were demonstrated to be stable for 12 months under accelerated stability conditions. After a single dose, C2E2 enhanced the elimination of (241)Am in a dose-dependent manner. Significant improvement was seen in both total (241)Am decorporation and reduction of (241)Am liver and skeletal burden. C2E2 was concluded to be effective when orally administered to (241)Am-contaminated rats. It may therefore have potential for medical countermeasure in treating humans contaminated with (241)Am or other transuranic elements. An oral capsule or powder for reconstitution may be suitable formulations for future development based on the physiochemical properties and anticipated dose required for efficacy.

  6. Application of Ce{sub x}Zr{sub 1-x}O{sub 2} catalysts for the synthesis of diethyl carbonate from ethanol and carbon dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Prymak, I.; Kalevaru, V.N.; Kollmorgen, P.; Wohlrab, S. [Leibniz-Institut fuer Katalyse e.V. an der Universitaet Rostock (Germany); Martin, A.

    2013-11-01

    The direct synthesis of diethyl carbonate (DEC) from ethanol and CO{sub 2} is indeed an attractive approach from both academic and commercial points of view. In the present study, we report on the synthesis, characterization and catalytic evaluation of Ce-Zr-O solids with varying Ce/Zr ratios. The catalysts were prepared by citrate complexation method, and characterized by various techniques such as N{sub 2} adsorption (BET-SA), XRD, H{sub 2}-TPR, NH{sub 3}-TPD etc. The catalytic performance of these catalysts was evaluated towards the synthesis of DEC from ethanol and CO{sub 2} under suitable reaction conditions. According to thermodynamic data, the reaction is favorable at low reaction temperatures and high reaction pressures. Thus, the catalytic experiments were carried out in a continuous mode using a plug-flow reactor that was operated up to 200 bar and ca. 200 C. The effect of the reaction temperature (30-180 C) and pressure (80-180 bar) on the yield of DEC was investigated. Among various catalysts tested, Ce-Zr-O catalyst with 80 mol% Ce content has exhibited a relatively better performance compared to all other Ce-Zr-O catalysts. DEC yield increased with increasing reaction temperature up to 140 C. The highest yield of DEC obtained from the best case was 0.7 % at 140 C and at 140 bars. Further increase in temperature to 180 C caused a decrease in the DEC formation due to thermodynamic reasons as mentioned above. The ceria proportion has shown a considerable influence on the BET surface areas and thereby catalytic activity as well. The results revealed that the redox properties as well as acidity characteristics of the solids are strongly influenced by the content of Ce in the catalysts, which in turn showed a clear impact on the catalytic performance. (orig.)

  7. 叠氮二乙基铝的合成及其热分解%Synthesis of Diethyl Aluminum Azide and Its Pyrolysis

    Institute of Scientific and Technical Information of China (English)

    高占先; 冯立春; 张小航; 莫自如

    2001-01-01

    以氯化二乙基铝(DECA)和叠氮化钠为原料合成了叠氮二乙基铝(DEAA),报导了放大实验中遇到的问题和解决的方法,以及DEAA热分解的条件及产物。%Diethyl aluminum azide (DEAA) is synthesized by diethyl aluminum chlorode and sodoum azide. Problems arisen and methods soloved problems are reported on bench-scals research. The products and conditions of DEAA pyrolysis are also reported.

  8. Polymerization of euphorbia oil with Lewis acid in carbon dioxide media

    Science.gov (United States)

    Boron trifluoride diethyl etherate (BF3-OEt2) Lewis acid catalyzed ring-opening polymerization of euphorbia oil (EO), a natural epoxy oil, in liquid carbon dioxide was conducted in an effort to develop useful vegetable oil based polymers. The resulting polymers (RPEO) were characterized by FTIR, 1H-...

  9. ON THE PECULIARITIES OF THE RING CONTRACTION REACTIONS OF HOMODRIMANES VIA ACID MEDIATED EPOXIDE REARRANGEMENT

    Directory of Open Access Journals (Sweden)

    Veaceslav Kulciţki

    2011-06-01

    Full Text Available A selective rearrangement of a epoxy-homodrimanic substrate is described. Using fluorosulfonic acid at low temperature leads by ring contraction to a perhydrindanic structure. On the contrary, using boron trifluoride-diethyl ether at r.t. selectively brings about angular methyl migration.

  10. Reactions of CH-acids with α,β-unsaturated aldehydes in ionic liquids

    DEFF Research Database (Denmark)

    Kryshtal, G. V.; Zhdankina, G. M.; Astakhova, Irina Kira

    2004-01-01

    Metal carbonate-catalyzed reactions of CH-acids (diethyl malonate, ethyl acetoacetate, ethyl cyanoacetate, and ethyl 2-acetyl- and 2-ethoxycarbonyl-5,9- dimethyldeca-4,8-dienoates) with α,β-unsaturated aldehydes (acrolein, crotonaldehyde, citral) were studied in an ionic liquid, 1-butyl-3...

  11. Bioconversion of ferulic acid and 4-vinylguaiacol by a white-rot ...

    African Journals Online (AJOL)

    USER

    2010-03-29

    Mar 29, 2010 ... The fungus is able to convert ferulic acid to 4-vinylguaiacol, which is then metabolized ... of manufacturing vanillin of “natural origin (Li and. Rosazza ... Abbreviations: GC-MS, Gas chromatography and mass ... It was then extracted 3 times with diethyl ether (50 ml per 100 .... Biocatalytic synthesis of vanillin.

  12. Effects of dietary intake of red palm oil on fatty acid composition and ...

    African Journals Online (AJOL)

    AYELESO

    2012-04-24

    Apr 24, 2012 ... were extracted by adding 25 ml of diethyl ether and 25 ml of petroleum ether. The organic phase was dried and the residue was derivatized using 2 ml of 2% sulphuric acid in methanol and 1 ml of toluene at 100°C for 45 min. ... sodium sulphate and transferred into a vial for gas chromatographic analyses.

  13. Conformational analysis of some N,N-diethyl-2-[(4'-substituted) phenylthio] acetamides.

    Science.gov (United States)

    Vinhato, Elisângela; Olivato, Paulo R; Zukerman-Schpector, Julio; Dal Colle, Maurizio

    2013-11-01

    The conformational analysis of some N,N-diethyl-2[(4'-substituted)phenylthio]acetamides bearing the substituents OMe 1, Me 2, H 3, Cl 4, Br 5 and NO26, was performed by νCO IR analysis, along with B3LYP/6-311++G(d,p) and Polarisable Continuum Model (PCM) calculations, as well as NBO analysis for 1, 3, and 6 and X-ray diffraction for 4. The results of the calculations indicated the existence of two stable conformation pairs, i.e. gauche (anti; syn) (most stable) and cis (anti; syn) in the gas phase. The gauche conformers were less polar with respect to the cis ones for 1 and 3, but more polar for 6. The most intense IR carbonyl doublet component observed at the lower frequency can be ascribed to the gauche conformers g(anti; syn) for 3-6 in n-C6H14, which is in agreement with the gauche and cis relative stabilities and frequencies resulting from the PCM calculations. Similarly, the single IR band for 1 and 2 in n-hexane may be attributed to the gauche conformers. The PCM calculations compared well with the IR data for the compounds in solution, showing that there is a progressive increase of the cis/gauche population ratio as the solvent polarity increases. The NBO analysis indicated that the gauche(anti; syn) conformation in the gas phase was stabilized by the relevant LPS4→πC2O1(∗),πC2O1→σC3S4(∗),σC3S4→πC2O1(∗),πC2O1(∗)→σC3S4(∗), and LPO1→σ(∗)C11H28 orbital interactions, which were absent in the cis(anti; syn) conformer. On the contrary, the cis conformer for derivatives 1, 3, and 6 were stabilized by the σC3-S4(∗)→σ(∗)C2N5 orbital interaction (through bond coupling), along with the additional LPO1→σ(∗)S4C10 interaction for 6. Moreover, the electrostatic repulsion between the C(δ+)S(δ-) and C(δ+)O(δ-) dipoles (Repulsive Field Effect) contributed to both the larger destabilization and increase of the νCO frequency of the cis conformer with respect to the gauche conformer. X-ray single crystal analysis indicates that

  14. Simultaneous determination of vanillylmandelic, homovanillic and 5-hydroxyindoleacetic acids in human urine by thin layer chromatography.

    Science.gov (United States)

    Alemany, G; Gamundí, A; Rosselló, C; Rial, R

    1996-01-01

    A TLC method for the simultaneous analysis of vanillylmandelic, homovanillic and 5-hydroxyindole-3-acetic acids in urine is described. The sample is cleaned up through a cyano minicolumn and extracted with diethyl ether. The acids are resolved by high-performance TLC, visualized by Folin Ciocalteau reagent and quantificated by densitometry at 600 nm with beta-(4-hydroxy-3-phenyl) acetic acid as the internal standard.

  15. Correction: Reaction mechanisms in ionic liquids: the kinetics and mechanism of the reaction of O,O-diethyl (2,4-dinitrophenyl) phosphate triester with secondary alicyclic amines.

    Science.gov (United States)

    Pavez, Paulina; Millán, Daniela; Morales, Javiera; Rojas, Mabel; Céspedes, Daniel; Santos, José G

    2016-01-28

    Correction for 'Reaction mechanisms in ionic liquids: the kinetics and mechanism of the reaction of O,O-diethyl (2,4-dinitrophenyl) phosphate triester with secondary alicyclic amines' by Paulina Pavez et al., Org. Biomol. Chem., 2016, DOI: 10.1039/c5ob02128f.

  16. Thiol and Disulfide Derivatives of Ephedra Alkaloids 2 : A Mechanistic Study of Their Effect on the Addition of Diethyl Zinc to Benzaldehyde

    NARCIS (Netherlands)

    Fitzpatrick, Kevin; Hulst, Ron; Kellogg, Richard M.

    1995-01-01

    Thiol and disulfide derivatives of ephedrine have been shown previously to catalyse in high enantiomeric excess (ee) the reaction of diethyl zinc with benzaldehyde. We find that this reaction involves non-linear correlations between the ee of product and catalyst. Osmotic measurements indicate a hig

  17. Grafting of diethyl maleate and maleic anhydride onto styrene-b-(ethylene-co-1-butene)-b-styrene triblock copolymer (SEBS)

    NARCIS (Netherlands)

    Picchioni, F.; Ghetti, S.; Passaglia, E.; Ruggeri, G.

    2000-01-01

    In this paper a study of the bulk functionalization of styrene-b-(ethylene-co-1-butene)-b-styrene triblock copolymer (SEBS) with diethyl maleate (DEM) or maleic anhydride (MAH) and dicumyl peroxide (DCP) as initiator in a Brabender mixer is described. The determination of the functionalization degre

  18. A new method for preparing (2Z, 4Z, 6Z)-diethyl-4,5-oxepinedicarboxylates and some 1H-azepine analogues

    Institute of Scientific and Technical Information of China (English)

    Di Zao Li; Zhong Fei Zheng; Zhi Yun Kang; De Quan Yu

    2009-01-01

    A new method for preparing (2Z, 4Z, 6Z)-4,5-diethyloxepinodicarboxylate by one-step is described. The synthesis of several oxepines and azepines derivatives was carried out by the reaction of substituted furans or pyrroles with diethyl acetylenedicarbox-ylate in boiling toluene. The effect factors for this reaction were discussed and reaction condition was optimized.

  19. The Effect of Time dealumination and Solvent Concentration in Synthesis of Zeolite Catalyst and Catalytic Test for DiEthyl Ether Production Process

    Science.gov (United States)

    Widayat, Widayat; Roesyadi, A.; Rachimoellah, M.

    2009-09-01

    Ethanol is an alternative energy, but its has three distinct disadvantages as a transportation fuel. Its availability is currently limited, and it has a lower volumetric heating value and a lower Reid vapour pressure (RVP) than gasoline. This paper focuses for this disadvantages and to solve this problem can do with converts ethanol to DiEthyl Ether product. This research produced DiEthyl Ether by ethanol dehydration process with zeolite as catalyst. The catalyst synthesis from natural material from District Gunung Kidul, Indonesia. The catalyst produced with dealumination, neutralization, drying and calcination processes. The zeolite catalyst was analysed of Si/Al, X-ray Diffraction and specific surface area. The catalyst product then used for ethanol dehydration to produce DiEthyl Ether. The results shown the biggest surface area is 184,52 m 2 / gram at catalyst production at 10 hours for time dealumination. The crystallite of catalyst product is similar like shown at diffractogram of XRD analysis. The ratio Si/Al biggest is 313.7 that obtaining at catalyst production with 7 hours for time dealumination. The catalytic test use fixed bed reactor with 1 inci diameter and ethanol fermentation borth as feed. The operation condition is 150° C at temperature and atmosphere pressure. The compounds product in liquid phase are diethyl ether, methanol and water.

  20. Infrared Multiple Photon Dissociation Action Spectroscopy and Theoretical Studies of Diethyl Phosphate Complexes: Effects of Protonation and Sodium Cationization on Structure

    NARCIS (Netherlands)

    Fales, B. S.; Fujamade, N. O.; Nei, Y. W.; Oomens, J.; Rodgers, M. T.

    2011-01-01

    The gas-phase structures of deprotonated, protonated, and sodium-cationized complexes of diethyl phosphate (DEP) including [DEP - H](-), [DEP + H](+), [DEP + Na](+), and [DEP - H + 2Na](+) are examined via infrared multiple photon dissociation (IRMPD) action spectroscopy using tunable IR radiation g

  1. Infrared multiple photon dissociation action spectroscopy and theoretical studies of diethyl phosphate complexes: effects of protonation and sodium cationization on structure

    NARCIS (Netherlands)

    Fales, B.S.; Fujamade, N.O.; Nei, Y.W.; Oomens, J.; Rodgers, M.T.

    2011-01-01

    The gas-phase structures of deprotonated, protonated, and sodium-cationized complexes of diethyl phosphate (DEP) including [DEP − H]−, [DEP + H]+, [DEP + Na]+, and [DEP − H + 2Na]+ are examined via infrared multiple photon dissociation (IRMPD) action spectroscopy using tunable IR radiation generated

  2. The First Synthesis and Anti-retroviral Activity of 5',5'-Difluoro-3'-Hydroxy-Apiosyl Nucleoside Cyclomonophosphonic Acid Analogs

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seyeon; Hong, Joon Hee [Chosun University, Gwangju (Korea, Republic of)

    2016-04-15

    The first synthesis of novel 5',5'-difluoro-30-hydroxy apiose nucleoside cyclomonophosphonic acid analogs was performed as potent anti-retroviral agents. Phosphonation was performed by direct displacement of a triflate intermediate with diethyl(lithiodifluoromethyl) phosphonate to give the corresponding(α, α-difluoroalkyl) phosphonate. Condensation successfully proceeded from a glycosyl donor with persilylated bases to yield the nucleoside phosphonate analogs. Deprotection of diethyl phosphonates provided the target nucleoside cyclomonophosphonic acid analogs. The synthesized nucleoside analogs were subjected to anti-viral screening against the human immunodeficiency virus-1 (HIV-1). Cytosine analogs show significant anti-HIV activity.

  3. ELECTROCHEMICAL COPOLYMERIZATION OF 3-(4-FLUOROPHENYL)THIOPHENE AND 3-METHYLTHIOPHENE IN BORON TRIFLUORIDE DIETHYL ETHERATE

    Institute of Scientific and Technical Information of China (English)

    Jing-kun Xu; Zhen-hong Wei; Qiang Xiao; Shou-zhi Pu

    2006-01-01

    The copolymer poly(3-(4-fluorophenyl)thiophene-co-3-methylthiophene) was successfully prepared from mixtures of 3-(4-fluorophenyl)thiophene (FPT) and 3-methylthiophene (MeT) via electrochemical oxidation in boron trifluoride diethyl etherate (BFEE) and its mixed electrolytes with acetonitrile (ACN). The influence of monomer concentration ratios on the copolymerization was investigated by using linear sweep voltammetry and cyclic voltammetry. The structure and morphology of these copolymer films were elucidated by UV-Vis, infrared spectroscopy, elemental analysis, thermal analysis and scanning electron microscopy (SEM), respectively. The results showed that the molar ratio of FPT and MeT units, when copolymer was electrodeposited from feed ratio of FPT:MeT = 1:2, was about 1.08:1. In addition, the introduction of ACN into BFEE has little effect on the properties of as-formed copolymers.

  4. Hydrogen sulfide production during yeast fermentation causes the accumulation of ethanethiol, S-ethyl thioacetate and diethyl disulfide.

    Science.gov (United States)

    Kinzurik, Matias I; Herbst-Johnstone, Mandy; Gardner, Richard C; Fedrizzi, Bruno

    2016-10-15

    Hydrogen sulfide (H2S) is produced by yeast during winemaking and possesses off-flavors reminiscent of rotten eggs. The production of H2S during fermentation has also been associated in the finished wine with the rise of additional volatile sulfur compounds (VSCs) with strong aromas of cooked onions and vegetables. To characterize these more complex VSCs produced from H2S, we performed fermentations in synthetic grape juice. H2S production was manipulated experimentally by feeding increasing concentrations of sulfate to mutant strains that are unable to incorporate H2S efficiently as part of the sulfur assimilation pathway. In finished wines from these mutants, three VSCs - ethanethiol, S-ethyl thioacetate and diethyl disulfide - increased proportionally to H2S. (34)S-labeled sulfate fed to the MET17-deleted strain was incorporated into same three VSCs, demonstrating that they are formed directly from H2S.

  5. Synthesis, structural, optical and thermal studies on 3, 5-diethyl-2, 6-di (4-fluorophenyl)-4-oxopiperidinium chloride

    Science.gov (United States)

    Yuvaraj, V.; NizamMohideen, M.; Arockia doss, M.; Rajarajan, G.; Savithiri, S.; Murugakoothan, P.

    2017-02-01

    A new organic compound 3, 5-diethyl-2, 6-di (4-fluorophenyl)-4-oxopiperidinium chloride (DFOC) was synthesized and its crystal was grown from ethanolic solution adopting the slow evaporation solution growth technique. The structure of the grown crystal was analyzed by single crystal X-ray diffraction study. The compound crystallizes in the orthorhombic system with space group Pnma. 1H and 13C Fourier transform nuclear magnetic resonance spectra of DFOC were recorded to elucidate its molecular structure. UV-vis-NIR spectral study showed that the grown crystal is transparent in the entire visible region with the lower cut-off wavelength of 269 nm. The thermal stability of DFOC was studied by thermogravimetric and differential thermal (TG-DTA) analyses.

  6. Crystal Structure of Diethyl [2,3-Di(Ethoxycarbonyl)-2, 3-di(p-nitrophenyl)l Succinate

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    A new conformational carbon-carbon bond free radical initiator diethyl [2,3- di(ethoxycarbonyl)-2,3-di(p-nitrophenyl)] succinate (EMNPS) was synthesized and identified by elemental analysis, FAB-MS, IR and 1H NMR spectroscopy. The analytical results of single crystal X-ray show the conforma-tion of EMNPS tends to be a stagger gauche form, and torsion angle of the two gauche phenyls is smaller than 60°. There is obvious elongation in central car bon-carbon bond length (0.161 nm). EMNPS can be decomposed into two relatively stable free radicals measured by ESR. By initiating bulk polymeriza-tion of methyl methacrylate (MMA), EMNPS shows the ability of controlling the molecular weight of polymers.

  7. Effects of dimethyl or diethyl carbonate as an additive on volatility and flash point of an aviation fuel.

    Science.gov (United States)

    Li, Dan; Fang, Wenjun; Xing, Yan; Guo, Yongsheng; Lin, Ruisen

    2009-01-30

    Vapor pressures and flash points for several mixtures of an aviation fuel with dimethyl carbonate (DMC) or diethyl carbonate (DEC) have been measured, respectively, over the entire composition range. Correlation between the experimental vapor pressures and the equilibrium temperatures by the Antoine equation is performed for each mixture. The bubble-point lines of pressure versus composition at different temperatures and those of temperature versus composition at different pressures are then obtained from the Antoine correlations. It is found that DMC and DEC are the oxygenated hydrocarbon additives that can adjust effectively the volatility and flash point of the aviation fuel. The correlation of the flash points with the vapor pressure data for the pseudo-binary mixtures of the fuel and DMC or DEC gives satisfactory results.

  8. The in vitro assessment of anti proliferation activity of crude diethyl ether extract of Dendrophthoe species against to myeloma culture cell

    Directory of Open Access Journals (Sweden)

    Mochamad Lazuardi

    2008-03-01

    Full Text Available Herb medicine have an active substances that can dissolved on polar, semi polar and non polar liquid extract. The methanol and ethyl acetate as a polar and semi polar extract liquid were used to study of herb medicine such as Dendrophthoe species. Diethyl ether as a non polar liquid extract was never use to study the Dendrophthoe species. The aim of this study was to investigate the anti proliferation activity of Dendrophthoe species to myeloma culture cells after extracted by non-polar extract solution (diethyl ether. The post test only control group design was used for this research. A thirty six of microtiterplates wells were used for myeloma culture cells in RPMI medium. The wells were devided placing in two groups: treatment groups and controls groups. Each three wells of six treatment subgroups added with 100 µl of 1.1; 5.5; 11; 22; 33 and 44 µg/ml crude diethyl ether extract series. A RPMI solution at similar method and volume were used as control substances. The cells were assessed by inverted microscope in 200x magnified two days after. The cells were quantified analyzed for anti proliferation activity by using 1:1 methylene blue solution. The results showed that started from 11.0 µg/ml of crude diethyl ether extract of Dendrophthoe species have been anti proliferation abilities of myeloma culture cells (p<0.05. In conclusion, actives substances of Dendrophthoe species where dissolved in non polar liquid as diethyl ether has anti proliferation activities to cancer cell in vitro.

  9. Synthesis of Diethyl Pyridin-2-ylphosphonates and Quinolin-2-ylphosphonates by Deoxygenative Phosphorylation of the Corresponding N-Oxides

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sangjin; Kim, Hyunsoo; Yang, Haewon; Yoo, Byungwoo; Yoon, Cheol Min [Korea Univ., Seoul (Korea, Republic of)

    2014-07-15

    The reaction of pyridine N-oxide and quinoline N-oxide activated by ethyl chloroformate with triethyl phosphites at rt gave the corresponding diethyl pyridin-2-ylphosphonate and diethyl quinolin-2-ylphosphonate regio-selectively in good to excellent yield through oxygenative phosphorylation. The reaction condition is mild and efficient compared to the reported methods. All chemicals including commercially available pyridine N-oxides were purchased from specialized suppliers with analytical purity and used without further purification. Non commercially available pyridine N-oxide for the reaction were prepared by known method. IR spectra of products were recorded on a Perkin-Elmer FT-IR 240-c spectrometer using KBr disks. {sup 1}H NMR (300 MHz) and {sup 13}C NMR (75 MHz) spectra were recorded on a Bruker 300 spectrometer in CDCl{sub 3}. High-resolution ESI-MS spectra were obtained on an IT-TOF (Shimadzu, Japan) at Korea Basic Science Institute (KBSI). Column chromatography was performed using Merck silica gel (230-400 mesh). Some known products have physical, spectroscopic, and analytic data identical to those (shown as a CAS registry number) given in the literature. Dialkyl pyridin-2-ylphosphonates widely used as corrosion inhibitors, dispersing and emulsifying agents, antistatics and lubricant additives in various technological fields are known as potent insecticides, fungicides and herbicides. Pyridin-2-ylphosphonates have also been reported to have a promising cytokinin activity, anti-proliferating and antiplatelet activating factor (anti-PAF) activities, and to be used as a chelate ligand to prepare various metal-organic frameworks, such as polymeric material with Zn, Cd and Ag showing luminescence properties, iron complex as a catalyst and copper complex with weak ferromagnetism. Because biological properties of dialkyl pyridin-2-ylphosphonates and physical properties of their complexes depend both on the phosphorus-containing ligand, simple and efficient

  10. Chemical analysis and risk assessment of diethyl phthalate in alcoholic beverages with special regard to unrecorded alcohol.

    Directory of Open Access Journals (Sweden)

    Jenny Leitz

    Full Text Available BACKGROUND: Phthalates are synthetic compounds with a widespread field of applications. For example, they are used as plasticizers in PVC plastics and food packaging, or are added to personal care products. Diethyl phthalate (DEP may be used to denature alcohol, e.g., for cosmetic purposes. Public health concerns of phthalates include carcinogenic, teratogenic, hepatotoxic and endocrine effects. The aim of this study was to develop and validate a method for determining phthalates in alcohol samples and to provide a risk assessment for consumers of such products. METHODOLOGY/PRINCIPAL FINDINGS: A liquid-liquid extraction procedure was optimized by varying the following parameters: type of extraction solvent (cyclohexane, n-hexane, 1,1,2-trichlorotrifluoroethane, the ratio extraction solvent/sample volume (1 ratio 1 to 50 ratio 1 and the number of extraction repetitions (1-10. The best extraction yield (99.9% was achieved with the solvent 1,1,2-trichlorotrifluoroethane, an extraction solvent volume/sample volume ratio of 10 ratio 1 and a double extraction. For quantification, gas chromatography/mass spectrometry with deuterated internal standards was used. The investigated samples were alcoholic beverages and unrecorded alcohol products from different countries (n = 257. Two unrecorded alcohol samples from Lithuania contained diethyl phthalate in concentrations of 608 mg/L and 210 mg/L. CONCLUSIONS/SIGNIFICANCE: The consumption of the phthalate-positive unrecorded alcohols would exceed tolerable daily intakes as derived from animal experiments. Both positive samples were labelled as cosmetic alcohol, but had clearly been offered for human consumption. DEP seems to be unsuitable as a denaturing agent as it has no effect on the organoleptic properties of ethanol. In light of our results that DEP might be consumed by humans in unrecorded alcohols, the prohibition of its use as a denaturing agent should be considered.

  11. PdCl2-loading mesoporous copper oxide as a novel and environmentally friendly catalyst for diethyl carbonate synthesis

    Science.gov (United States)

    Zhang, Pingbo; Zhou, Yan; Fan, Mingming; Jiang, Pingping

    2015-03-01

    PdCl2-loading mesoporous copper oxide (PdCl2/mCuO) catalysts were successfully synthesized via a hard template with copper carbonate basic (Cu2(OH)2CO3), cupric nitrate (Cu(NO3)2·3H2O) and copper citrate (Cu2C6H4O7·2.5H2O) as the copper(II) precursors, respectively. Their catalytic performances were investigated in the synthesis of diethyl carbonate (DEC) by oxidative carbonylation of ethanol with CO and O2. The catalysts were characterized by TGA, XRD, nitrogen adsorption-desorption analysis and SEM with the aim of establishing their composition, morphology and structure. It was observed that the catalysts all showed a good selectivity to diethyl carbonate. However, due to a better mesoporous structure such as a bigger surface area, more uniform particle size and less agglomeration, the PdCl2/mCuO-1 catalyst prepared with Cu2(OH)2CO3 precursor showed a better catalytic activity that the conversion of EtOH was about 4.8% and the STY of DEC was 97.1 mg g-1 h-1. This was because the highly developed mesoporous structure could generate a bigger surface area, which benefited the contact between reactants and active sites, improved the conversion of ethanol, and thus enhanced the catalytic performance. Furthermore, a synthetic procedure diagram about "wet impregnation" method of mesoporous CuO prepared with Cu2(OH)2CO3 precursor was given to illustrate these results intuitively.

  12. The formation of diethyl ether via the reaction of iodoethane with atomic oxygen on the Ag(110) surface

    Science.gov (United States)

    Jones, G. Scott; Barteau, Mark A.; Vohs, John M.

    1999-01-01

    The reactions of iodoethane (ICH 2CH 3) on clean and oxygen-covered Ag(110) surfaces were investigated using temperature-programmed desorption (TPD) and high-resolution electron energy-loss spectroscopy (HREELS). Iodoethane adsorbs dissociatively at 150 K to produce surface ethyl groups on both clean and oxygen-covered Ag(110) surfaces. The ethyl species couple to form butane on both surfaces, with the desorption peak maximum located between 218 and 238 K, depending on the ethyl coverage. In addition to butane, a number of oxidation products including diethyl ether, ethanol, acetaldehyde, surface acetate, ethylene, carbon dioxide and water were formed on the oxygen-dosed Ag(110) surface. Diethyl ether was the major oxygenate produced at all ethyl:oxygen ratios, and the peak temperature for ether evolution varied from 220 to 266 K depending on the relative coverages of these reactants. The total combustion products, CO 2 and H 2O, were primarily formed at low ethyl coverages in the presence of excess oxygen. The formation of ethylene near 240 K probably involves an oxygen-assisted dehydrogenation pathway since ethylene is not formed from ethyl groups on the clean surface. Acetaldehyde and ethanol evolve coincidentally with a peak centered at 270-280 K, and are attributed to the reactions of surface ethoxide species. The surface acetate which decomposes near 620 K is formed from subsequent reactions of acetaldehyde with oxygen atoms. The addition of ethyl to oxygen to form surface ethoxides was verified by HREELS results. The yields of all products exhibited a strong dependence on the relative coverages of ethyl and oxygen.

  13. An Efficient Synthesis of Nitriles from Aldoximes Using Diethyl Phosphorocyanidate under Mild Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Kieseung; An, Hyeonseong; Hwang, Chanyeon [Woosuk Univ.,Wanju (Korea, Republic of)

    2012-10-15

    Nitriles are valuable intermediates in organic synthesis not only because they serve as the appropriate precursors to various functional groups, but also because they are widely used as the key intermediates for pharmaceuticals, agrochemicals and various N-heterocyclic compounds. The cyano group itself is also frequently found in many biologically important molecules. Therefore, a variety of synthetic routes to nitriles from diverse chemical precursors have been developed. Among these routes, nitrile synthesis from aldoximes using an appropriate dehydrating agent has been a general and clean method. For this purpose, numerous reagents such as chlorosulfonyl isocyanate, di-2-pyridyl sulfite, Burgess reagent, [RuCl{sub 2}(p-cymene)]{sub 2}/MS, 4A, BOP, Pd(OAc){sub 2}/PPh{sub 3}, Cu(OAc){sub 2}/ultrasound have been developed. These reagents, however, may have limitations in some respects such as harsh reaction conditions, use of expensive or less readily available reagents, low yields, and lack of generality. Therefore, there is still a need to develop mild and general method for this conversion. Diethyl phosphorocyanidate (DEPC) was initially introduced as an efficient peptide coupling reagent, and has been utilized for useful organic reactions. Previously, we reported that 2-chloro-1-methylpyridinium iodide is an efficient and mild reagent for the dehydration of aldoximes to nitriles under mild conditions. In continuation of our interest in developing mild method for the conversion of aldoximes to nitriles, we herein wish to report the first application of DEPC to the efficient synthesis of nitriles from aldoximes under mild conditions (Scheme 1). In order to obtain the information regarding the optimum reaction conditions, 4-pyridine aldoxime (1a) was reacted with DEPC without base, and in presence of various base in CH{sub 2}Cl{sub 2} at rt for a prolonged reaction time (20 h) (Table 1). CH{sub 2}CI{sub 2} was chosen as reaction medium in this reaction due to the

  14. Vanadocene reactions with hydroxy acids. [Hydroxy acids: acetylsalicylic, gallic, lactic, salicyclic, orotic,. gamma. -hydroxybutyric acids

    Energy Technology Data Exchange (ETDEWEB)

    Latyaeva, V.N.; Lineva, A.N.; Zimina, S.V.; Ehllert, O.G.; Arsen' eva, T.I. (Gor' kovskij Meditsinskij Inst. (USSR))

    1984-03-01

    To prepare a series of vanadium cyclopentadienylcarboxylates soluble in water, the vanadocene reactions with lactic, ..gamma..-oxybutyric-, salicylic,- gallic-, orotic-, and acetylsalicylic acids have been studied. To determine the influence of cyclopentadienyl groups, bound with a vanadium atom, on the physiological activity of the complexes formed, vanadium halides are made to react with lactic acid. Only the vanadocene reaction with orotic acid was conducted in an aqueous medium, other interactions were realized in the diethyl ether, toluene, T, H, P medium. The interaction of vanadocene and vanadium halides with lactic-, salicylic-, acetylsalicylic- and gallic acids was found to lead to the formation of water-soluble vanadium complexes of Cp/sub 2/, VOCOR or CpV (OCOR)/sub 2/ type. The data on the produced compounds yield, their IR spectra, decomposition temperatures, solubility, effective magnetic moments are presented.

  15. Lewis acid catalyzed ring-opening polymerization of natural epoxy oil (Euphorbia oil) in carbon dioxide media

    Science.gov (United States)

    In an attempt to build up useful application of plant oil based polymers, natural epoxy oil (euphorbia oil-EuO) was polymerized in liquid carbon dioxide in the presence of Lewis acid catalyst [Boron trifluoride diethyl etherate (BF3•OEt2)]. The resulting polymers (RPEuO) were characterized by FTIR ...

  16. Volumetric, viscometric and optical study of molecular interactions in binary mixtures of diethyl malonate with ketones at 303.15, 308.15 and 313.15K

    Directory of Open Access Journals (Sweden)

    Rathnam Manapragada V.

    2012-01-01

    Full Text Available Density ρ, viscosity η, and refractive index nD were measured for the binary mixtures of diethyl malonate with ketones (acetophenone, cyclopentanone, cyclohexanone and 3-pentanone at temperatures (303.15, 308.15 and 313.15 K over the entire composition range. Excess volume VE, deviation in viscosity Δη, excess Gibb’s free energy of activation for viscous flow ΔGE and deviation in molar refraction ÄR were determined from the experimental data and computed results were fitted to the Redlich-Kister polynomial equation. The values of VE, Δη, ΔGE, and ΔR were plotted against the mole fraction of diethyl malonate. The observed positive and negative values of excess parameters for all the studied binary mixtures were explained on the basis of intermolecular interactions present in these mixtures. Further different empirical relations were used to correlate the binary mixture viscosities and refractive indices.

  17. Poly[[bis(μ-4,4′-bipyridyl-κ2N:N′bis(thiocyanato-κNmanganese(II] diethyl ether disolvate

    Directory of Open Access Journals (Sweden)

    Mario Wriedt

    2010-07-01

    Full Text Available In the title compound, {[Mn(NCS2(C10H8N22]·2C4H10O}n, the MnII ion is coordinated by four N-bonded 4,4′-bipyridine (bipy ligands and two N-bonded thiocyanate anions in a distorted octahedral coordination geometry. The asymmetric unit consists of one MnII ion and two bipy ligands each located on a twofold rotation axis, as well as one thiocyanate anion and one diethyl ether molecule in general positions. In the crystal structure, the metal centers with terminally bonded thicyanate anions are bridged by the bipy ligands into layers parallel to (001. The diethyl ether solvent molecules occupy the voids of the structure.

  18. Crystal structure of diethyl [(4-nitrophenylamino(2-hydroxyphenylmethyl]phosphonate methanol monosolvate

    Directory of Open Access Journals (Sweden)

    QingMing Wang

    2014-09-01

    Full Text Available In the title compound, C17H21N2O6P·CH3OH, the planes of the 4-nitroaniline and 2-hydroxyphenyl groups form a dihedral angle of 84.04 (8°. The P atom exhibits tetrahedral geometry involving two O-ethyl groups, a Cα atom and a double-bonded O atom. In the crystal, O—H...O, N—H...O and C—H...O hydrogen bonds link the α-aminophosphonic acid and methanol molecules into chains that propagate parallel to the a axis.

  19. Potassium iodide catalyzed reductive dehalogenation of α-halo-ketones using Hantzsch ester diethyl 1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate as reductant

    Institute of Scientific and Technical Information of China (English)

    Hong Sheng Li; Yi Qun Li

    2010-01-01

    In the presence of diethyl 1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate (DHP) and a catalytic amount of potassium iodide,several α-halo ketones were easily reduced to the corresponding ketones in acetone media.The procedure presented here showed several merits such as short reaction time,practical experimental and isolated procedure,and excellent yields of products.

  20. GC/MS ANALYSIS AND ANTIMICROBIAL ACTIVITY OF DIETHYL ETHER FRACTION OF METHANOLIC EXTRACT FROM THE STEM BARK OF ANNONA SENEGALENSIS PERS.

    Directory of Open Access Journals (Sweden)

    E. P. Awa*, S. Ibrahim and D. A. Ameh

    2012-11-01

    Full Text Available The Diethyl ether fraction of the Methanolic extract of Annona senegalensis (Pers stem bark was prepared in yield of (0.16%. Preparative Thin Layer Chromatography analysis of the fraction resulted in the identification of two spots with antimicrobial activity. Subsequent GC/MS analysis of these spots resulted in the identification of ten components (spot one and fourteen components (spot two. The fraction showed significant antimicrobial activity against clinical isolates of E. coli, S. enteriditis and S. dysenteriae.

  1. Numerical investigation on the effect of injection pressure on the internal flow characteristics for diethyl ether, dimethyl ether and diesel fuel injectors using CFD

    Directory of Open Access Journals (Sweden)

    Vijayakumar Thulasi

    2011-01-01

    Full Text Available The spray characteristics of the diesel fuel are greatly affected by the cavitation formed inside the injector due to the high pressure differential across the nozzle. Many researchers across the globe are exploring the potential of using diethyl ether and dimethyl ether as an alternate for diesel fuel to meet the strict emission norms. Due to the variation in the fuel properties the internal flow characteristics in injectors for ether fuels are expected to be different from that of the diesel fuel. In this paper computational technique is used to study and compare the internal flow characteristics of diethyl ether, dimethyl ether and diesel fuel. The two phase flow model considering the fuel as a mixture of liquid and vapor is adopted for the simulation study. The injection pressure is varied from 100 to 400 bar and the flow characteristics of all three fuels are simulated and compared. Results indicate that all three fuels have distinct cavitating patterns owing to different property values. The dimethyl ether is found to be more cavitating than diesel and diethyl ether fuels as expected. The mass of fuel injected are found to be decreasing for the ether fuels when compared with diesel fuel at all injection pressures.

  2. Comparative study of the effects of toluene, benzene, 1,1,1-trichloroethane, diethyl ether, and flurothyl on anxiety and nociception in mice.

    Science.gov (United States)

    Páez-Martínez, Nayeli; Cruz, Silvia Lorenia; López-Rubalcava, Carolina

    2003-11-15

    The main purpose of this study was to compare the effects of solvents from different chemical classes on anxiety and nociception. Independent groups of mice were exposed to air (control group), toluene (1000-4000 ppm), benzene (1000-4000 ppm), 1,1,1-trichloroethane (TCE, 2000-12000 ppm), diethyl ether (10,000-30,000) or flurothyl (200-600 ppm). After a 30-min exposure, animals were tested either in the anxiety paradigm conditioned defensive burying (CDB) test or in the hot plate test. All solvents but flurothyl produced anxiolytic-like actions being the order of potency toluene > benzene > TCE > diethyl ether. When tested in the hot plate paradigm, toluene and TCE increased nociception, benzene and diethyl ether had no effects, and flurothyl decreased nociception Additional groups of mice were conditioned to recognize the aversive stimulus (electrified prod) prior to toluene exposure and then tested in the CDB test. In unconditioned animals, toluene increased the number of shocks that mice received; however, when mice had previous experience in the CDB test, toluene lacked this effect. Taken together, these results show that inhalants have different effects with different potencies both in the CDB and in the hot plate tests. Additionally, data suggest that acute administration of toluene could impair learning.

  3. Acute Toxicity and Ecological Risk Assessment of Benzophenone and N,N-Diethyl-3 Methylbenzamide in Personal Care Products

    Directory of Open Access Journals (Sweden)

    Hong-Qin Sun

    2016-09-01

    Full Text Available Benzophenone (BP and N,N-diethyl-3-methylbenzamide (DEET are two chemicals often used in personal care products (PCPs. There is a lack of systematic ecotoxicological evaluations about the two chemicals to aquatic organisms. In the present study, the acute toxic effects on Chlorella vulgaris, Daphnia Magana, and Brachydanio rerio were tested and the ecotoxicological risks were evaluated. For BP, the 96-h half-maximal effective concentration (EC50 on C. vulgaris was 6.86 mg/L; the 24-h median lethal concentration (LC50 on D. magana was 7.63 mg/L; the 96-h LC50 on B. rerio was 14.73 mg/L. For DEET, those were 270.72 mg/L, 40.74 mg/L, and 109.67 mg/L, respectively. The mixture toxicity of BP and DEET, on C. vulgaris, D. magana, and B. rerio all showed an additive effect. The induced predicted no-effect concentrations (PNECs for BP and DEET by assessment factor (AF method are 0.003 mg/L and 0.407 mg/L, respectively. Both are lower than the concentrations detected from environment at present, verifying that BP and DEET are low-risk chemicals to the environment.

  4. Synthesis and Crystal Structure of Diethyl (4,6-diamino-1,3,5-triazine-2-yl) phosphonate

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The crystal of the title compound diethyl (4,6-diamino-1,3,5-triazine-2-yl) phosphonate, (C14H28N10O6P2, Mr=494.40), has been prepared and determined by X-ray single crystal diffraction. The crystal belongs to the triclinic system, space group P with parameters: a=8.398(1) , b=10.206(1), c=14.538(2), α=75.221(3), β=85.965(3), γ=81.746(3)°, V=1191.6(3)3, S=1.028, Z=2, Dc=1.378Mg/m3, μ=0.233mm-1, F(000)=520, λ(MoKα)=0.71073, T=293(2)K, final R=0.071 and wR=0.1953 for 4177 independent reflections with I≥2σ(I). In the title compound, each molecule is linked to five neighbour molecules by hydrogen bonds forming layers perpendicular to the a axis and molecules in each layer are linked by a two-dimensional network of hydrogen bonds in the bc plane.

  5. Kinetic of the gas-phase reactions of OH radicals and Cl atoms with Diethyl Ethylphosphonate and Triethyl Phosphate

    KAUST Repository

    Laversin, H.

    2015-11-30

    In this paper, the relative-rate technique has been used to obtain rate coefficients for the reaction of two organophosphorus compounds: Triethyl phosphate (TEP) and Diethyl ethylphosphonate (DEEP) with OH radicals and Cl atoms at atmospheric pressure and at different temperatures. The calculated rate constants were fitted to the Arrhenius expression over the temperature range 298 – 352 K. The following expressions (in cm3molecule-1s-1) were obtained for the reactions of OH and CL with DEEP and TEP: kOH+DEEP= (7.84±0.65)x10-14exp((1866±824)/T), kOH+TEP = (6.54±0.42)x10-14exp((1897±626)/T), kCl+DEEP = (5.27± 0.80)x10−11exp(765±140/T) and kCl+TEP = (5.23± 0.80)x10−11exp(736± 110/T). These results show that the reaction of the studied compounds with Cl atoms proceeds more rapidly than that with OH radicals. The related tropospheric lifetimes suggest that once emitted into the atmosphere, TEP and DEEP can be removed within a few hours in areas close to their emission sources. TEP and DEEP are principally removed by OH radicals. However, in coastal areas where the Cl atoms’ concentration is higher, TEP and DEEP removal by reaction with Cl atoms could be a competitive process.

  6. Synthesis and Crystal Structure of Diethyl 5-Acetoxy-3-(4-chlorophenyl)-4,5-dihydroisoxazol-5-yl-5-phosphonate

    Institute of Scientific and Technical Information of China (English)

    SHANG Zhi-Qiang; CHEN Ru-Yu; HUANG You

    2006-01-01

    The crystal structure of the title compound, diethyl 5-acetoxy-3-(4-chlorophenyl)-4,5-dihydroisoxazol-5-yl-5-phosphonate (Ci5H19ClNO6P, Mr = 375.73), has been synthesized by the treatment of nitrile oxides and 1-acetyloxy-vinylphosphonate under very mild conditions in good yields, and determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 16.914(10), b = 10.567(7), c = 21.927(13)(A),β = 110.249(11)°, V= 3677(4)(A)3,Z = 8, Dc = 1.358 g/cm3, F(000) = 1568, μ(MoKa) = 0.324 mm-1, S = 1.011, the final R = 0.0661and wR = 0.1556. The X-ray analytic results showed that the dihedral angle between the phenyl group and the isoxazoline ring is 10.7°.

  7. DFT study on the adsorption of diethyl, ethyl methyl, and dimethyl ethers on the surface of gallium doped graphene

    Science.gov (United States)

    Shokuhi Rad, Ali; Sani, Emad; Binaeian, Ehsan; Peyravi, Majid; Jahanshahi, Mohsen

    2017-04-01

    In this study, we used density functional theory (DFT) to search on the adsorption properties of three important compounds of ether family; diethyl ether (DEE), ethyl methyl ether (EME), and dimethyl ether (DME) on the surface of Gallium doped graphene (GaG). We used three functionals (B3LYP, wb97xd, and MPW1PW91) for optimization and calculation of adsorption energy. After fully optimization, we scrutinized on the charge allocations on the adsorbed ethers as well as GaG (at the area of interaction) based on natural bond orbitals (NBO). Besides, we have calculated the amount of charge transfer upon adsorption of each analyte. We revel that GaG is an ideal adsorbent for chemisorption of all above-mentioned ethers. There is a little difference between the values of adsorption; -123.5, -120, and -118.3 kJ/mol (based on wb97xd) for DEE, EME, and DME, respectively. We found significant changes in the electronic structure of both adsorbent and adsorbate upon adsorption. Moreover, results of charge analyses confirm GaG is a p-type semiconductor.

  8. A Practical Strategy to Discover New Antitumor Compounds by Activating Silent Metabolite Production in Fungi by Diethyl Sulphate Mutagenesis

    Directory of Open Access Journals (Sweden)

    Shi-Ming Fang

    2014-03-01

    Full Text Available Many fungal biosynthetic pathways are silent in standard culture conditions, and activation of the silent pathways may enable access to new metabolites with antitumor activities. The aim of the present study was to develop a practical strategy for microbial chemists to access silent metabolites in fungi. We demonstrated this strategy using a marine-derived fungus Penicillium purpurogenum G59 and a modified diethyl sulphate mutagenesis procedure. Using this strategy, we discovered four new antitumor compounds named penicimutanolone (1, penicimutanin A (2, penicimutanin B (3, and penicimutatin (4. Structures of the new compounds were elucidated by spectroscopic methods, especially extensive 2D NMR analysis. Antitumor activities were assayed by the MTT method using human cancer cell lines. Bioassays and HPLC-photodiode array detector (PDAD-UV and HPLC-electron spray ionization (ESI-MS analyses were used to estimate the activated secondary metabolite production. Compounds 2 and 3 had novel structures, and 1 was a new compound belonging to a class of very rare natural products from which only four members are so far known. Compounds 1–3 inhibited several human cancer cell lines with IC50 values lower than 20 μM, and 4 inhibited the cell lines to some extent. These results demonstrated the effectiveness of this strategy to discover new compounds by activating silent fungal metabolic pathways. These discoveries provide rationale for the increased use of chemical mutagenesis strategies in silent fungal metabolite studies.

  9. Degradation of N,N-diethyl-m-toluamid (DEET) on lead dioxide electrodes in different environmental aqueous matrixes.

    Science.gov (United States)

    Huang, Kuo-Lin; Chen, Te-San; Chen, Pi-Hui; Kuo, Yi-Ming

    2015-01-01

    This study investigates the electrochemical degradation of N,N-diethyl-m-toluamide (DEET) on PbO2 and Bi-PbO2 anodes. The difference in electrode crystalline structure was responsible for the better DEET degradation and TOC removal on PbO2 than on Bi-PbO2. In 1 M Na2SO4, the degradation efficiency and apparent rate constant (kapp) of DEET oxidation on PbO2 increased with the increase in current density or temperature (activation energy=24.4 kJ mol(-1)). The kapp values in DEET-spiked environmental matrixes (municipal wastewater treatment plant secondary effluent (MWTPSE), groundwater (GW), and river water (RW)) were the same (6.05×10(-4) s(-1)), but significantly smaller than that in 1 M Na2SO4 (2.23×10(-3) s(-1)). The TOC removal efficiency was better in MWTPSE than in RW and GW; however, the mineralization current efficiencies in MWTPSE and RW were similar but higher than that in GW. During electrolysis, the aromaticity was lower in GW than in RW.

  10. Effect of diethyl aminoethyl hexanoate on the accumulation of high-value biocompounds produced by two novel isolated microalgae.

    Science.gov (United States)

    Jiang, Liqun; Pei, Haiyan; Hu, Wenrong; Han, Fei; Zhang, Lijie; Hou, Qingjie

    2015-12-01

    The low productivity of microalgae has restricted scale-up application of microalgae-based biodiesel processes. Diethyl aminoethyl hexanoate (DA-6) was investigated to enhance the biomass and metabolite productivity. At a very low concentration (10(-7)M) DA-6 made Chlorella ellipsoidea SDEC-11 and Scenedesmus quadricauda SDEC-13 obtain enlarged cell size, 114mgL(-1)d(-1), 101mgL(-1)d(-1) biomass productivity and 39.13mgL(-1)d(-1), 32.69mgL(-1)d(-1) lipid productivity, respectively. Biomass and lipid productivity of SDEC-11 and SDEC-13 were 100mgL(-1)d(-1) and 30.05mgL(-1)d(-1), 94mgL(-1)d(-1) and 28.43mgL(-1)d(-1), respectively, without DA-6. Twice hormone dose in 10(-6)M DA-6 medium resulted in higher biomass productivity (106mgL(-1)d(-1)) and longer exponential growth of SDEC-13. DA-6 also ensured the property of microalgae biodiesel to meet the EN 14214 standard. The current investigation demonstrated that DA-6 accelerated the microalgae growth and simultaneously improved the quality and quantity of lipid for biodiesel production. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Matrix isolation studies of the interactions of BF3 with water and substituted diethyl ethers. Chemical ionization mass spectrometric determination of the proton affinity of (CF3CH2)2O

    Science.gov (United States)

    Ball, David W.; Zehe, Michael J.

    1993-01-01

    BF3 was co-condensed with H2O, D2O, (C2H5)2O, (CF3CH2)2O, and (C2F5)2O in excess argon at 15 K. Infrared spectra of BF3/water isolated in solid argon provided a more complete analysis of the BF3--H2O complex than previously published. Infrared spectra of the matrices showed a definite Lewis acid-base interaction between BF3 and diethyl ether; a weak but definite interaction with bis (2,2,2-trifluorodiethyl) ether, and no observable interaction with perfluorodiethyl ether. Thus, the ether data indicate a clear trend between strength of interaction with BF3 and the degree of F substitution. To support and explain the emerging relationship between interaction strength and the basicity of the oxygen-containing molecule, the proton affinity of (CF3CH2)2O was measured using chemical ionization mass spectrometry. The implications of the results for lubricant/metal oxide surface interactions are discussed.

  12. 采用二乙氨基二硫代甲酸银光度法测定裂解气中的砷含量%Determination of arsenic content in pyrolysis by using silver diethyl dithiocarbamate spectrophotometric method

    Institute of Scientific and Technical Information of China (English)

    童玲; 高瑞峰

    2012-01-01

    The determination of trace arsenic in prolysis gas by using silver diethyl dithiocarbamate spectrophotometric method was established. This method was applicable to determination of the mass concentration of arsenic in pyrolysis gas in the level of mg/L. The optimal operating conditions of the determination were as follows:the dosage of sulfuric acid was 20 mL, the dosage of the zinc particles in 10-20 mesh was 6 g,the absorbtion wavelength was 530 nm. The relative standard deviation was less than 10% ,and the recovery rate was in the range of 95% -105%.%建立了裂解气中痕量砷(As)的二乙氨基二硫代甲酸银光度测定法.该方法适用于As质量浓度为mg/L级的裂解气的测定.在H2SO4加入量为20 mL,10 ~ 20目的锌粒加入量为6 g,吸光波长为530 nm的优化条件下,As含量测定结果的相对标准偏差小于10%,方法的回收率为95% ~ 105%.

  13. Synthesis, spectroscopic (UV-Vis, FT-IR and NMR), single crystal XRD of 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate: A comprehensive experimental and computational study

    Science.gov (United States)

    Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

    2017-01-01

    A piperidin-4-one containing picrate 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate [3,5-DPPP] was synthesized. The molecular structure of 3,5-DPPP was confirmed by FT-IR, NMR, Uv-Vis, single crystal XRD analysis and DFT and HF methods with 6-31G(d,p) basis set. The XRD data confirm the transfer of protons from picric acid (O2) to piperidin-4-one ring (N1). The 3,5-DPPP compound is stabilized by the presence of intermolecular and intramolecular hydrogen bonds (N-H⋯O, C-H⋯S and C-H⋯O). Density functional theory and HF calculations have been used widely for calculating a wide variety of molecular properties such as optimized structure, FT-IR and Uv-Vis spectra, and provided reliable results which are in agreement with experimental data. The charge density data have been used to understand the properties of molecular systems. Furthermore, several quantum chemical insights have been obtained in the form of the total and partial density of states, the HOMO-LUMO energy gap and electrostatic potential map etc. In addition, the polarizability and first hyperpolarizability were calculated to show the potential applications of 3,5-DPPP in nonlinear optics.

  14. Conversion of furfuryl alcohol into ethyl levulinate using solid acid catalysts.

    Science.gov (United States)

    Lange, Jean-Paul; van de Graaf, Wouter D; Haan, René J

    2009-01-01

    Furfural, a potential coproduct of levulinic acid, can be converted into levulinic acid via hydrogenation to furfuryl alcohol and subsequent ethanolysis to ethyl levulinate. The ethanolysis reaction is known to proceed in the presence of H(2)SO(4). We show here that several strongly acidic resins are comparably effective catalysts for this reaction. Optimal performance is achieved by balancing the number of acid sites with their accessibility in the resin. Acidic zeolites such as H-ZSM-5 also catalyze this reaction, although with a lower activity and a higher co-production of diethyl ether.

  15. Assessment of methods used to determine the safety of the topical insect repellent N,N-diethyl-m-toluamide (DEET).

    Science.gov (United States)

    Chen-Hussey, Vanessa; Behrens, Ron; Logan, James G

    2014-06-03

    N,N-diethyl-m-toluamide (DEET) has been registered for commercial use as an insect repellent for over five decades, and is used widely across the world. Concerns over the safety of DEET first emerged during the 1980s after reports of encephalopathy following DEET exposure, particularly in children. However, the role of DEET in either the illness or deaths was and remains purely speculative. In response to these cases a number of reviews and investigations of DEET safety were carried out. Here we examine the methods used and information available to determine the safety of DEET in humans. Animal testing, observational studies and intervention trials have found no evidence of severe adverse events associated with recommended DEET use. Minor adverse effects noted in animal trials were associated with very large doses and were not replicated between different test species. The safety surveillance from extensive humans use reveals no association with severe adverse events. This review compares the toxicity assessment using three different models to define the risk assessment and safety threshold for DEET use in humans and discusses the clinical consequences of the thresholds derived from the models.The theoretical risks associated with wearing an insect repellent should be weighed against the reduction or prevention of the risk of fatal or debilitating diseases including malaria, dengue, yellow fever and filariasis. With over 48 million European residents travelling to regions where vector borne diseases are a threat in 2009, restricting the concentration of DEET containing repellents to 15% or less, as modelled in the 2010 EU directive, is likely to result in extensive sub-therapeutic activity where repellents are infrequently applied. Future European travellers, as a consequence of inadequate personal protection, could potentially be at increased risk of vector borne diseases. Risk assessments of repellents should take these factors into account when setting safe

  16. Experimental Study of the Isochoric Heat Capacity of Diethyl Ether (DEE) in the Critical and Supercritical Regions

    Science.gov (United States)

    Polikhronidi, N. G.; Abdulagatov, I. M.; Batyrova, R. G.; Stepanov, G. V.; Wu, J. T.; Ustuzhanin, E. E.

    2012-02-01

    Two- and one-phase liquid and vapor isochoric heat capacities ( C V ρ T relationship) of diethyl ether (DEE) in the critical and supercritical regions have been measured with a high-temperature and high-pressure nearly constant-volume adiabatic calorimeter. The measurements were carried out in the temperature range from 347 K to 575 K for 12 liquid and 5 vapor densities from 212.6 kg·m-3 to 534.6 kg·m-3. The expanded uncertainties (coverage factor k = 2, two-standard deviation estimate) for values of the heat capacity were 2% to 3% in the near-critical region, 1.0% to 1.5% for the liquid isochores, and 3% to 4% for the vapor isochores. The uncertainties of density ( ρ) and temperature ( T) measurements were 0.02% and 15 mK, respectively. The values of the internal energy, U( T, V), and second temperature derivative of pressure, (∂2 P/∂ T 2) ρ , were derived using the measured C V data near the critical point. The critical anomaly of the measured C V and derived values of U( T, V) and (∂2 P/∂ T 2) ρ in the critical and supercritical regions were interpreted in terms of the scaling theory of critical phenomena. The asymptotic critical amplitudes {({A_0^+} and {A_0^- )}} of the scaling power laws along the critical isochore for one- and two-phase C V were calculated from the measured values of C V . Experimentally derived values of the critical amplitude ratio for {CV left({A_0^+ /A_0^- = 0.521}right)} are in good agreement with the values predicted by scaling theory. The measured C V data for DEE were analyzed to study the behavior of loci of isothermal and isochoric C V maxima and minima in the critical and supercritical regions.

  17. Acid Brothers: Henry Beecher, Timothy Leary, and the psychedelic of the century.

    Science.gov (United States)

    Moreno, Jonathan D

    2016-01-01

    Henry Knowles Beecher, an icon of human research ethics, and Timothy Francis Leary, a guru of the counterculture, are bound together in history by the synthetic hallucinogen lysergic acid diethylamide (LSD). Both were associated with Harvard University during a critical period in their careers and of drastic social change. To all appearances the first was a paragon of the establishment and a constructive if complex hero, the second a rebel and a criminal, a rogue and a scoundrel. Although there is no evidence they ever met, Beecher's indirect struggle with Leary over control of the 20th century's most celebrated psychedelic was at the very heart of his views about the legitimate, responsible investigator. That struggle also proves to be a revealing bellwether of the increasingly formalized scrutiny of human experiments that was then taking shape.

  18. Synthesis of diethyl succinate catalyzed by functional ionic liquids%功能化离子液体催化合成丁二酸二乙酯

    Institute of Scientific and Technical Information of China (English)

    胡晶晶; 赵地顺; 李静静; 胡甜甜; 翟建华

    2016-01-01

    Four kinds of functional ionic liquids,1-methyl-3-(3-sulfopropyl)imidazolium hydrogen sulfate ([C3 SO3 Hmim]HSO4 ),1-ethyl-3-(3-sulfopropyl)imidazolium hydrogen sulfate ([C3 SO3 Emim]HSO4 ), 1-propyl-3-(3-sulfopropyl)imidazolium hydrogen sulfate ([C3 SO3 Pmim]HSO4 ),1-butyl-3-(3-sulfoprop-yl)imidazolium hydrogen sulfate ([C3 SO3 Bmim]HSO4 ),were designed and synthesized.The properties of samples were characterized by FTIR,1 H NMR and TG.The catalytic activities of the functional ionic liquid were investigated by the esterification of succinic anhydride with ethanol.The results showed that under the optimized conditions n(succinic anhydride)∶n(ethanol)=1∶2.5,catalyst dosage 9%,water carrying agent dosage 35%,reaction temperature 90 ℃ and reaction time 5 h,the yield of diethyl succi-nate was up to 92.28%.The ionic liquids dried in vacuum till remained high activity after reused for 8 times.Moreover,compared to conventional industrial catalysts,ionic liquid catalyst needed less,and had the superiorities of less by-product,mild reaction conditions,high yield and the catalyst could be recy-cled,and has the potential of replacing the traditional sulfuric acid in catalytic esterification reaction.%采用两步法合成了4种不同阳离子的功能化离子液体:1-甲基-3-(3-磺丙基)咪唑硫酸氢盐([C3 SO3 Hmim] HSO4)、1-乙基-3-(3-磺丙基)咪唑硫酸氢盐([C3SO3Emim]HSO4)、1-丙基-3-(3-磺丙基)咪唑硫酸氢盐([C3SO3-Pmim]HSO4)、1-丁基-3-(3-磺丙基)咪唑硫酸氢盐([C3 SO3 Bmim]HSO4)。通过FTIR、1 H NMR和TG分析了离子液体的结构和热稳定性。并将其应用于催化丁二酸酐和乙醇的酯化反应中,考察了4种离子液体的催化活性。结果表明,离子液体[C3SO3Bmim]HSO4的催化效果较好,在n(丁二酸酐)∶n(乙醇)=1∶2.5,催化剂用量9%,环己烷用量35%,反应温度90℃的条件下反应5 h后,丁二酸二乙酯的收率可达92

  19. The in vitro assessment of anti proliferation activity of crude diethyl ether extract of Dendrophthoe species against to myeloma culture cell

    OpenAIRE

    Mochamad Lazuardi

    2008-01-01

    Herb medicine have an active substances that can dissolved on polar, semi polar and non polar liquid extract. The methanol and ethyl acetate as a polar and semi polar extract liquid were used to study of herb medicine such as Dendrophthoe species. Diethyl ether as a non polar liquid extract was never use to study the Dendrophthoe species. The aim of this study was to investigate the anti proliferation activity of Dendrophthoe species to myeloma culture cells after extracted by non-polar extra...

  20. Heat of Mixing and Solution of Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (HMSD1111, LB4315_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (HMSD1111, LB4315_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  1. Heat of Mixing and Solution of 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (HMSD1111, LB4209_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (HMSD1111, LB4209_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  2. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C7H8 Toluene (VMSD1212, LB5158_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume B 'Binary Liquid Systems of Nonelectrolytes II' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C7H8 Toluene (VMSD1212, LB5158_V)' providing data by calculation of molar excess volume from low-pressure density measurements at variable mole fraction and constant temperature.

  3. Volumetric Properties of the Mixture 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (VMSD1111, LB4682_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (VMSD1111, LB4682_V)' providing data from direct low-pressure measurement of mass density at variable mole fraction and constant temperature, in the single-phase region(s).

  4. Volumetric Properties of the Mixture 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (VMSD1212, LB4692_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (VMSD1212, LB4692_V)' providing data by calculation of molar excess volume from low-pressure density measurements at variable mole fraction and constant temperature.

  5. Volumetric Properties of the Mixture Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (VMSD1212, LB5137_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (VMSD1212, LB5137_V)' providing data by calculation of molar excess volume from low-pressure density measurements at variable mole fraction and constant temperature.

  6. Heat of Mixing and Solution of 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (HMSD1111, LB4208_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (HMSD1111, LB4208_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  7. Vapor-Liquid Equilibrium in the Mixture Diethyl carbonate C5H10O3 + C6H14O Hexan-1-ol (EVLM1111, LB5629_E)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume A 'Binary Liquid Systems of Nonelectrolytes I' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Vapor-Liquid Equilibrium in the Mixture Diethyl carbonate C5H10O3 + C6H14O Hexan-1-ol (EVLM1111, LB5629_E)' providing data from direct measurement of pressure at variable mole fraction in liquid phase and constant temperature.

  8. Volumetric Properties of the Mixture 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (VMSD1111, LB4686_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture 2-Ethoxyethanol C4H10O2 + C5H10O3 Diethyl carbonate (VMSD1111, LB4686_V)' providing data from direct low-pressure measurement of mass density at variable mole fraction and constant temperature, in the single-phase region(s).

  9. Volumetric Properties of the Mixture 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (VMSD1212, LB4691_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture 2-Methoxyethanol C3H8O2 + C5H10O3 Diethyl carbonate (VMSD1212, LB4691_V)' providing data by calculation of molar excess volume from low-pressure density measurements at variable mole fraction and constant temperature.

  10. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C7H8 Toluene (VMSD1111, LB5155_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume B 'Binary Liquid Systems of Nonelectrolytes II' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C7H8 Toluene (VMSD1111, LB5155_V)' providing data from direct low-pressure measurement of mass density at variable mole fraction and constant temperature, in the single-phase region(s).

  11. Volumetric Properties of the Mixture Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (VMSD1111, LB5134_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Dimethyl sulfoxide C2H6OS + C5H10O3 Diethyl carbonate (VMSD1111, LB5134_V)' providing data from direct low-pressure measurement of mass density at variable mole fraction and constant temperature, in the single-phase region(s).

  12. XRD and xanes studies of copper complexes using (diethyl 4-amino-1-phenyl-1H-pyrazole-3,5 dicarboxylate) as ligand

    Science.gov (United States)

    Mishra, Ashutosh; Jain, Garima

    2013-06-01

    X-ray diffraction (XRD) and X-ray absorption spectroscopic (XAS) studies have been done on three copper complexes using (diethyl 4-amino-1-phenyl-1H-pyrazole-3,5 dicarboxylate) as ligand. The X-ray diffraction studies of copper complexes have been recorded using Rigaku RINT-2000 X-ray diffractometer equipped with a rotating anode with tube voltage of 40 kV and current of 100 mA. The X-ray absorption spectra of the complexes have been recorded at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore and is called beamline.

  13. (2,4-二甲氧基苯基)烯丙基丙二酸二乙酯异构体的GC/MS研究%Study on Diethyl [3-(2,4-Dimethoxyphenyl) Allyl] Malonate Isomers by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    王敏; 彭奇

    2012-01-01

    A method applying gas chromatography-ion trap mass spectrometry (GC/MS) for the simultaneous analysis of diethyl [3-(2,4-dimethoxyphenyl)allyl]malonate isomers is described. The diethyl [3-(2,4-dimethoxyph-enyl)allyl]malonate mixture of isomers was prepared by the decarboxylative Heck reaction of 2,4-dimethoxybenzoic acid with diethyl 2-al-lylmalonate firstly, and then was analyzed by GC/MS in Electron ionization (El) and Chemical ionization (CD full-scan mode. Two components were isolated by gas chromatography" and identified as isomers from the determination of the molecular ions. Next, the isomers were analyzed by tandem mass spectrometry (MS/MS) mode. Through the analysis of different cleavage fragments of the isomers in MS/MS mode, mass spectrometric fragmentation pathways of the isomers were discussed. The structures of two isomers were determined on the base of different mass characteristic fragmentation pathways. This new meth- od of identifying isomers is a time-saving, economical and effective method, which could provide reference for analysis and identification of this kind of compounds.%为了研究钯催化的2,4-二甲氧基苯甲酸与烯丙基丙二酸二乙酯的脱羧Heck反应的产物结构,建立了(2,4-二甲氧基苯基)烯丙基丙二酸二乙酯同分异构体的分离与鉴定的气相色谱-离子阱质谱方法.首先通过脱羧Heek反应制得(2,4-二甲氧基苯基)烯丙基丙二酸二乙酯异构体混合物,然后利用GC/MS联用技术对混合物进行分析,得到各组分的EI和CI全扫描模式质谱信息.通过对照各组分的分子离子峰确定互为异构体的组分,再对异构体组分采用MS/MS模式获取各自的裂解碎片.通过分析异构体的不同的裂解碎片,讨论质谱裂解方式,从而确定异构体的结构.该方法省时、经济、高效,可为此类化合物的分析与鉴别提供参考.

  14. [Animal experiments with 99mTc-diethyl-HIDA in acute complete bile duct occlusion (author's transl)].

    Science.gov (United States)

    Bähre, M; Biersack, H J; Breuel, H P; Degen, H; Busch, F; Grouls, V; Lindstaedt, H; Thelen, M

    1979-10-01

    In order to establish whether a complete obstructive jaundice can abolish the accumulation of diethyl-HIDA (EHIDA) in the liver parenchyma, the common bile duct was ligated in 14 mongrel dogs. Before as well as at regular intervals after ligature of the common bile duct, a sequence scintigraphy was performed with 2 mCi 99mTc-EHIDA. For evaluation, time-activity curves (Tmax, T1/2), and analogue scintigrams as well as laboratory parameters were used for assessment. Up to seven weeks after ligation of the common bile duct, there was a marked accumulation of EHIDA in the liver parenchyma. The relative liver uptake (liver/background ratio) fell from 8.9 to 2.7, whereas conversely the cholestasis indicators aP and bilirubine rose markedly. Tmax did not show any significant alterations, whereas T1/2 was prolonged from about one week after ligation. Because of the duct ligation, there was no excretion of activity into the intestines. Immediately after ligation of the common bile duct, the gallbladder was shown up as a "hot" area in which the majority of the applied activity appeared from about one hour p.i. Begining with the fifth to the seventh day after ligation, the gallbladder was seen as a "cold" area in the liver paraenchyma. Bilirubine and aP were raised by about 50 times the initial value. With longer lasting cholestasis, the scintigram no longer altered whereas bilirubine and aP rose further. Histological examination after ligation for more than five weeks showed slight alterations as a whole. Gamma-GT and in particular GPT were likewise slightly raised compared to bilirubine and aP. The conclusion was drawn from this that the good accumulation of EHIDA in the liver parenchyma which is to be observed without exception even in cholestasis lasting for several weeks could be explained by a relatively slight hepatocellular damage. Only when there is a consecutive parenchymal damage in extrahepatic jaundice, accumulation of EHIDA in the liver can be abolished.

  15. Extraction of arsenic as the diethyl dithiophosphate complex with supercritical fluid and quantitation by cathodic stripping voltammetry.

    Science.gov (United States)

    Arancibia, Verónica; López, Alex; Zúñiga, M Carolina; Segura, Rodrigo

    2006-02-28

    The separation of arsenic based on in situ chelation with ammonium diethyl dithiophosphate (ADDTP) has been carried out using methanol-modified supercritical CO(2). Aliquots of extract were added to an electroanalytical cell and arsenic was determined by square wave cathodic stripping voltammetry (SWCSV) at a hanging mercury drop electrode (HMDE). Quantitative extractions of As(DDTP)(3) were achieved when the experiments were carried out at a pressure of 2500psi, a temperature of 90 degrees C, 2.0mL of methanol, 20.0min of static extraction and 5.0min of dynamic extraction in the presence of 18mg of ADDTP. Analysis of arsenic was made using 150mgL(-1) of Cu(II) in 1M HCl solution as supporting electrolyte in the presence of ADDTP as ligand. Preconcentration was carried out by deposition at a potential of -0.50V and the intermetallic compound Cu(x)As(y) was reduced at a potential of -0.77 to -0.82V, depending on ligand concentration. The results showed that the presence of ligand plays an important role, increasing the method's sensitivity and preventing the oxidation of As(III). The calibration graph of the As(DDTP)(3) solution was linear from 0.8 to 12.5mugL(-1) of arsenic (LOD 0.5mugL(-1), R=0.9992, t(acc)=60s). The method was validated using carrot pulp spiked with arsenic solution. This method was applied to the determination of arsenic in samples of carrots, beets and irrigation water. Arsenic in beets was: skin 4.10+/-0.18mgkg(-1); pulp 3.83+/-0.19mgkg(-1) and juice 0.71+/-0.09mgL(-1); arsenic in carrots was: skin 2.15+/-0.09mgkg(-1); pulp 0.59+/-0.11mgkg(-1) and juice 0.71+/-0.03mgL(-1). Arsenic in water were: Chiu-Chiu 0.08mgL(-1), Inacaliri 1.12mgL(-1), and Salado river 0.17+/-0.07mgL(-1).

  16. Protective efficacy of menthol propylene glycol carbonate compared to N, N-diethyl-methylbenzamide against mosquito bites in Northern Tanzania.

    Science.gov (United States)

    Kweka, Eliningaya J; Munga, Stephen; Mahande, Aneth M; Msangi, Shandala; Mazigo, Humphrey D; Adrias, Araceli Q; Matias, Jonathan R

    2012-09-05

    The reduction of malaria parasite transmission by preventing human-vector contact is critical in lowering disease transmission and its outcomes. This underscores the need for effective and long lasting arthropod/insect repellents. Despite the reduction in malaria transmission and outcomes in Tanzania, personal protection against mosquito bites is still not well investigated. This study sought to determine the efficacy of menthol propylene glycol carbonate (MR08), Ocimum suave as compared to the gold standard repellent N, N-diethyl-methylbenzamide (DEET), either as a single dose or in combination (blend), both in the laboratory and in the field against Anopheles gambiae s.l and Culex quinquefasciatus. In the laboratory evaluations, repellents were applied on one arm while the other arm of the same individual was treated with a base cream. Each arm was separately exposed in cages with unfed female mosquitoes. Repellents were evaluated either as a single dose or as a blend. Efficacy of each repellent was determined by the number of mosquitoes that landed and fed on treated arms as compared to the control or among them. In the field, evaluations were performed by human landing catches at hourly intervals from 18:00  hr to 01:00  hr. A total of 2,442 mosquitoes were collected during field evaluations, of which 2,376 (97.30%) were An. gambiae s.l while 66 (2.70%) were Cx. quinquefaciatus. MR08 and DEET had comparatively similar protective efficacy ranging from 92% to 100 for both single compound and blends. These findings indicate that MR08 has a similar protective efficacy as DEET for personal protection outside bed nets when used singly and in blends. Because of the personal protection provided by MR08, DEET and blends as topical applicants in laboratory and field situations, these findings suggest that, these repellents could be used efficiently in the community to complement existing tools. Overall, Cx. quinquefasciatus were significantly prevented from blood

  17. Protective efficacy of menthol propylene glycol carbonate compared to N, N-diethyl-methylbenzamide against mosquito bites in Northern Tanzania

    Directory of Open Access Journals (Sweden)

    Kweka Eliningaya J

    2012-09-01

    Full Text Available Abstract Background The reduction of malaria parasite transmission by preventing human-vector contact is critical in lowering disease transmission and its outcomes. This underscores the need for effective and long lasting arthropod/insect repellents. Despite the reduction in malaria transmission and outcomes in Tanzania, personal protection against mosquito bites is still not well investigated. This study sought to determine the efficacy of menthol propylene glycol carbonate (MR08, Ocimum suave as compared to the gold standard repellent N, N-diethyl-methylbenzamide (DEET, either as a single dose or in combination (blend, both in the laboratory and in the field against Anopheles gambiae s.l and Culex quinquefasciatus. Methods In the laboratory evaluations, repellents were applied on one arm while the other arm of the same individual was treated with a base cream. Each arm was separately exposed in cages with unfed female mosquitoes. Repellents were evaluated either as a single dose or as a blend. Efficacy of each repellent was determined by the number of mosquitoes that landed and fed on treated arms as compared to the control or among them. In the field, evaluations were performed by human landing catches at hourly intervals from 18:00 hr to 01:00 hr. Results A total of 2,442 mosquitoes were collected during field evaluations, of which 2,376 (97.30% were An. gambiae s.l while 66 (2.70% were Cx. quinquefaciatus. MR08 and DEET had comparatively similar protective efficacy ranging from 92% to 100 for both single compound and blends. These findings indicate that MR08 has a similar protective efficacy as DEET for personal protection outside bed nets when used singly and in blends. Because of the personal protection provided by MR08, DEET and blends as topical applicants in laboratory and field situations, these findings suggest that, these repellents could be used efficiently in the community to complement existing tools. Overall, Cx

  18. Matrix Isolation FTIR and AB Initio Studies on the Conformations of Dimethyl and Diethyl Carbonate and Their Complexes with Water

    Science.gov (United States)

    Kar, Bishnu Prasad; Ramanathan, N.; Sundararajan, K.; Viswanathan, K. S.

    2011-06-01

    Dimethyl carbonate (DMC) and diethyl carbonate (DEC) have been studied for their conformations using matrix isolation infrared spectroscopy and ab initio computations. In addition to the above studies, the complexes of the two compounds with water have also been studied. The experiments were corroborated with ab initio calculations at the B3LYP/6-31++G** level. The organic carbonates were trapped in argon and nitrogen matrixes using an effusive source maintained at two different temperatures; i.e. room temperature and 170°C. In addition the matrix was also deposited using a supersonic jet source. These experiments were performed to alter the relative population of the various conformations, to aid us in the assignments of the vibrational features. The conformation of DMC corresponding to the global minimum of DMC was found to be a cis-cis conformer where the two methyl groups are found to be at cis position with respect to the carbonyl oxygen. The next higher energy conformer corresponded to a cis-trans structure with a near trans-near trans structure being the highest energy conformer. In our experimental matrix isolation spectra of DMC, we were able to assign features due to the cis-cis and cis-trans conformers. The features of the higher energy cis-trans conformer was confirmed with our experiments using the elevated temperature effusive source and the supersonic source. DEC displays a richer conformational landscape due to the presence of a longer carbon chain. The computational and experimental indicate that the ground state conformer for this compound is one in which carbon attached to oxygen adopts a cis configuration with respect to the carbonyl oxygen, while the terminal carbon adopts an anti conformation. A detailed study of the conformational picture of DEC will be presented. In addition to the above conformational studies, 1:1 hydrogen bonded complexes of DMC and DEC with water were also observed in the matrix, which was corroborated by our

  19. Excess isentropic compressibility and speed of sound of the ternary mixture 2-propanol + diethyl ether + n-hexane and the constituent binary mixtures at 298.15 K

    Indian Academy of Sciences (India)

    Gokhan Sovaroglu; Ertunc Aral

    2006-02-01

    Speed of sound and densities of the ternary mixture 2-propanol + diethyl ether + n-hexane and also the binary mixtures 2-propanol + diethyl ether and 2-propanol + n-hexane have been measured at the entire composition range at 298.15 K. The excess isentropic compressibilities and the excess speed of the sound have been calculated from experimental densities and speed of sound. These excess properties of the binary mixtures were fitted to Redlich-Kister equation, while the Cibulka's equation was used to fit the values related to the values to the ternary system. These excess properties have been used to discuss the presence of significant interactions between the component molecules in the binary mixtures and also the ternary mixtures. Speed of sound of the binary mixtures and the ternary mixture have been compared with calculated values from free length theory (FLT), collision factor theory (CFT), Nomoto's relation (NR), Van Deal's ideal mixing relation (IMR) and Junjie's relation (JR). The results are used to compare the relative merits of these theories and relations in terms of the root mean square deviation relative (RMSDr).

  20. {6,6′-Dimethoxy-2,2′-[naphthalene-2,3-diylbis(nitrilomethylidyne]diphenolato}thiocyanatocobalt(III diethyl ether dichloromethane solvate

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available In the title complex, [Co(C26H20N2O4(NCS]·C4H10O·CH2Cl2, the pentacoordinated CoIII atom exhibits a distorted square-pyramidal geometry with an N,N′,O,O′ tetradentate Schiff base ligand in the basal plane and one thiocyanate ligand at the apical site. The diethyl ether molecule is located in a cavity provided by four O atoms of the ligand with weak C—H...O interactions, generating two short O...O contact distances [2.766 (3 and 2.745 (3 Å] between the diethyl ether molecule and the ligand. The crystal structure is stabilized by the weak C—H...O and C—H...N interactions and π–π interactions between the naphthyl ring system and the benzene ring [centroid–centroid distance = 3.657 (5 Å] and between the two naphthyl ring systems [centroid–centroid distance = 4.305 (2 Å].

  1. Influence of the synthesis parameters on the physico-chemical and catalytic properties of cerium oxide for application in the synthesis of diethyl carbonate

    Energy Technology Data Exchange (ETDEWEB)

    Leino, Ewelina; Kumar, Narendra; Mäki-Arvela, Päivi; Aho, Atte [Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Biskopsgatan 8, 20500 Turku/Åbo (Finland); Kordás, Krisztián [Chemical–Biological Centre, Department of Chemistry, Technical Chemistry, Umeå University, SE-90187 Umeå (Sweden); Laboratory of Microelectronics and Materials Physics, EMPART Research Group of Infotech Oulu, University of Oulu, PL 4500, 90014 Oulu (Finland); Leino, Anne-Riikka [Laboratory of Microelectronics and Materials Physics, EMPART Research Group of Infotech Oulu, University of Oulu, PL 4500, 90014 Oulu (Finland); Shchukarev, Andrey [Chemical–Biological Centre, Department of Chemistry, Technical Chemistry, Umeå University, SE-90187 Umeå (Sweden); Murzin, Dmitry Yu., E-mail: dmurzin@abo.fi [Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Biskopsgatan 8, 20500 Turku/Åbo (Finland); Mikkola, Jyri-Pekka [Laboratory of Industrial Chemistry and Reaction Engineering, Process Chemistry Centre, Åbo Akademi University, Biskopsgatan 8, 20500 Turku/Åbo (Finland); Chemical–Biological Centre, Department of Chemistry, Technical Chemistry, Umeå University, SE-90187 Umeå (Sweden)

    2013-12-16

    Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO{sub 2} properties was discussed. Moreover, the comparison of CeO{sub 2} samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO{sub 2}. Significant variations in physico-chemical properties of CeO{sub 2} by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO{sub 2} catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO{sub 2} using butylene oxide as a dehydrating agent. The dependence of CeO{sub 2} properties on its catalytic activity is evaluated in detail. - Highlights: • Synthesis of cerium (IV) oxide by precipitation method. • Influence of synthesis time, calcination temperature, mode of stirring and solution pH on properties. • Characterization by XRD, SEM, TEM, nitrogen physisorption, XPS, FTIR. • Catalytic performance diethyl carbonate synthesis from ethanol and CO{sub 2}.

  2. DFT investigations of the reaction mechanism of diethyl carbonate synthesis catalyzed by Cu(I)/β or Pd(II)/β zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Yongli [Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Wang, Shengping, E-mail: spwang@tju.edu.cn [Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Huang, Shouying [Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Li, Zhong [Key Laboratory of Coal Science and Technology of Ministry of Education, Taiyuan University of Technology, Taiyuan 030024, Shanxi (China); Ma, Xinbin [Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China)

    2014-07-01

    Density functional theory (DFT) calculations are used to investigate the oxidative carbonylation of ethanol occurring on Cu(I)/β or Pd(II)/β. The thermochemistry and activation energy for all elementary steps involved in the formation of diethyl carbonate are presented. Upon calculation, we identify that the mechanisms for the formation of surface O atom are varying on different catalysts. Ethanol can react with the surface O atom to produce (C{sub 2}H{sub 5}O)(OH)-M/β (M = Cu{sup +}, Pd{sup 2+}) species. And this intermediate can further react with carbon monoxide or ethanol to give monoethyl carbonate or di-ethoxied species ((C{sub 2}H{sub 5}O){sub 2}-M/β). Diethyl carbonate can form via two distinct reaction pathways: (I) ethanol reacts with monoethyl carbonate or (II) carbon monoxide inserts into di-ethoxide species. Upon calculation, we confirmed that both reaction pathways for the formation of DEC are accessible on Cu(I)/β catalyst, whereas only Path II is achievable on Pd(II)/β catalyst.

  3. DFT investigations of the reaction mechanism of diethyl carbonate synthesis catalyzed by Cu(I)/β or Pd(II)/β zeolites

    Science.gov (United States)

    Shen, Yongli; Wang, Shengping; Huang, Shouying; Li, Zhong; Ma, Xinbin

    2014-07-01

    Density functional theory (DFT) calculations are used to investigate the oxidative carbonylation of ethanol occurring on Cu(I)/β or Pd(II)/β. The thermochemistry and activation energy for all elementary steps involved in the formation of diethyl carbonate are presented. Upon calculation, we identify that the mechanisms for the formation of surface O atom are varying on different catalysts. Ethanol can react with the surface O atom to produce (C2H5O)(OH)-M/β (M = Cu+, Pd2+) species. And this intermediate can further react with carbon monoxide or ethanol to give monoethyl carbonate or di-ethoxied species ((C2H5O)2-M/β). Diethyl carbonate can form via two distinct reaction pathways: (I) ethanol reacts with monoethyl carbonate or (II) carbon monoxide inserts into di-ethoxide species. Upon calculation, we confirmed that both reaction pathways for the formation of DEC are accessible on Cu(I)/β catalyst, whereas only Path II is achievable on Pd(II)/β catalyst.

  4. Hydrolysis of Carbonyl Sulfide in Binary Mixture of Diethylene Glycol Diethyl Ether and Water%羰基硫在二乙二醇二乙醚/水二元混合体系中的水解

    Institute of Scientific and Technical Information of China (English)

    李新学; 刘迎新; 魏雄辉

    2005-01-01

    The solubility and hydrolysis of carbonyl sulfide in binary mixture of diethylene glycol diethyl ether and water are studied as a function of composition. The use of an aqueous solution of diethylene glycol diethyl ether enhances the solubility and hydrolysis rate of carbonyl sulfide compared with that in pure water. The composition of the mixture with maximum hydrolysis rate varies with temperature. The thermophysical properties including density, viscosity, and surface tension as a function of composition at 20℃ under atmospheric pressure as well as liquid-liquid equilibrium (LLE) data over the temperature range from 28℃ to 90℃ are also measured for the binary mixture.

  5. (Diethyl ether{1-[2-(1-methyl-1H-imidazol-2-yl-κN3-1,1-diphenylethyl]-(1,2,3,3a,7a-η-indenyl}lithium(I

    Directory of Open Access Journals (Sweden)

    Maxim V. Borzov

    2009-05-01

    Full Text Available In the title compound, [Li(C27H23N2(C4H10O], the Li atom possesses a nearly planar trigonal coordination environment (assuming the cyclopentadienyl ring of the indenyl group occupies one coordination place. The diethyl ether ligand adopts a nearly planar W-type conformation.

  6. Effect of the SK/IK channel modulator 4,5-dichloro-1,3-diethyl-1,3-dihydro-benzoimidazol-2-one (NS4591) on contractile force in rat, pig and human detrusor smooth muscle

    DEFF Research Database (Denmark)

    Nielsen, Jens Steen; Rode, Frederik; Rahbek, Mette

    2011-01-01

    • To investigate the importance of small (SK)- and intermediate (IK)-conductance Ca2(+) -activated K(+) channels on bladder function, by studying the effects of 4,5-dichloro-1,3-diethyl-1,3-dihydro-benzoimidazol-2-one (NS4591), a new modulator of SK/IK channels, on contractions induced...

  7. In Vivo Quantification of Cerebral Translocator Protein Binding in Humans Using 6-Chloro-2-(4′-123I-Iodophenyl)-3-(N,N-Diethyl)-Imidazo[1,2-a]Pyridine-3-Acetamide SPECT

    DEFF Research Database (Denmark)

    Feng, Ling; Svarer, Claus; Thomsen, Gerda;

    2014-01-01

    UNLABELLED: This study provides the first comprehensive quantification of translocator protein (TSPO) binding using SPECT and 6-chloro-2-(4'-(123)I-iodophenyl)-3-(N,N-diethyl)-imidazo[1,2-a]pyridine-3-acetamide ((123)I-CLINDE) in neurologic patients. (123)I-CLINDE is structurally related to well...

  8. (Diethyl ether){1-[2-(1-methyl-1H-imidazol-2-yl-κN)-1,1-diphenyl-ethyl]-(1,2,3,3a,7a-η)-inden-yl}lithium(I).

    Science.gov (United States)

    Sun, Guofeng; Tian, Chong; Nie, Wanli; Borzov, Maxim V

    2009-04-02

    In the title compound, [Li(C(27)H(23)N(2))(C(4)H(10)O)], the Li atom possesses a nearly planar trigonal coordination environment (assuming the cyclo-penta-dienyl ring of the indenyl group occupies one coordination place). The diethyl ether ligand adopts a nearly planar W-type conformation.

  9. Comparative study of different initiation methods in the functionalization of low-density polyethylene with diethyl maleate: Gamma radiation and ultrasound

    Energy Technology Data Exchange (ETDEWEB)

    Albano, C. [Centro de Quimica, Laboratorio de Polimeros, Instituto Venezolano de Investigaciones Cientificas (IVIC), Caracas (Venezuela); Universidad Central de Venezuela, Facultad de Ingenieria, Escuela de Ingenieria Quimica, Caracas (Venezuela)], E-mail: calbano@ivic.ve; Perera, R. [Departamento de Mecanica, Universidad Simon Bolivar, Caracas (Venezuela)], E-mail: rperera@usb.ve; Sanchez, Y.; Karam, A. [Centro de Quimica, Laboratorio de Polimeros, Instituto Venezolano de Investigaciones Cientificas (IVIC), Caracas (Venezuela); Silva, P. [Centro de Fisica, Laboratorio de la Materia Condensada, Instituto Venezolano de Investigaciones Cientificas, Caracas (Venezuela)

    2007-12-15

    This work unfolds a comparative study of the grafting of a low-density polyethylene with diethyl maleate (DEM) using gamma irradiation and ultrasound as means of initiating the grafting reactions. The grafting degree was determined by FTIR using a reported calibration curve. The efficiency of both functionalization methodologies was calculated and the polymers were characterized by differential scanning calorimetry (DSC) and gel permeation chromatography (GPC). The results showed that the grafting degree increases with the radiation dose when the monomer is inserted by gamma radiation. When the ultrasound methodology was used, an additional initiator such as dicumyl peroxide had to be used in order for the grafting to take place. In this last case, changing the time of exposure to the ultrasound source did not induce significant changes in the obtained grafted degree. The use of ultrasonic radiation plus dicumyl peroxide as grafting initiators promoted more insertion than that when gamma radiation was employed.

  10. Distinct molecular structures and hydrogen bond patterns of α,α-diethyl-substituted cyclic imide, lactam, and acetamide derivatives in the crystalline phase

    Science.gov (United States)

    Krivoshein, Arcadius V.; Ordonez, Carlos; Khrustalev, Victor N.; Timofeeva, Tatiana V.

    2016-10-01

    α,α-Dialkyl- and α-alkyl-α-aryl-substituted cyclic imides, lactams, and acetamides show promising anticonvulsant, anxiolytic, and anesthetic activities. While a number of crystal structures of various α-substituted cyclic imides, lactams, and acetamides were reported, no in-depth comparison of crystal structures and solid-state properties of structurally matched compounds have been carried out so far. In this paper, we report molecular structure and intermolecular interactions of three α,α-diethyl-substituted compounds - 3,3-diethylpyrrolidine-2,5-dione, 3,3-diethylpyrrolidin-2-one, and 2,2-diethylacetamide - in the crystalline phase, as studied using single-crystal X-ray diffraction and IR spectroscopy. We found considerable differences in the patterns of H-bonding and packing of the molecules in crystals. These differences correlate with the compounds' melting points and are of significance to physical pharmacy and formulation development of neuroactive drugs.

  11. Bis[μ-1,3-bis(diphenylphosphanylpropane-κ2P:P′]digold(I tetrachloridonickelate(II diethyl ether monosolvate

    Directory of Open Access Journals (Sweden)

    Asako Igashira-Kamiyama

    2013-06-01

    Full Text Available The title compound, [Au2(C27H26P22][NiCl4]·C4H10O, consists of a digold(I complex cation, an [NiCl4]2− complex anion and a diethyl ether solvent molecule. Two 1,3-bis(diphenylphosphanylpropane (dppp ligands bridge two AuI atoms, forming a metallacycle in which each of the AuI atoms is coordinated in a slightly distorted linear environment by two P atoms. In the complex anion, the NiII atom is coordinated by four chloride ligands in a distorted tetrahedral geometry. The complex cation and the complex anion form a cation–anion pair through two Au...Cl contacts of 3.040 (1 and 3.021 (2 Å. One of the phenyl groups of the dppp ligand is disordered over two positions with equal occupancies.

  12. Spectroelectrochemistry of P700 in native photosystem I particles and diethyl ether-treated thylakoid membranes from spinach and Thermosynechococcus elongatus.

    Science.gov (United States)

    Zhang, Yanrong; Nakamura, Akimasa; Kuroiwa, Yoshinori; Kato, Yuki; Watanabe, Tadashi

    2008-04-02

    The redox potentials (E(composite function')) of P700 in intact and diethyl ether-treated thylakoid membranes as well as native photosystem (PS) I particles from spinach and Thermosynechococcus elongatus have been measured by a spectroelectrochemistry with an error range of +/-2-3 mV. Stepwise removal of antenna pigments by ether treatment caused distinct shifts of the E( composite function') value with increasing degree of water saturation in ether; negatively from +471 to +428 mV for spinach, but positively from +423 to +436 mV for T. elongatus. Such a contrasting behavior is discussed by invoking the mode of action of ether on the microenvironments around P700.

  13. Ion-molecule interactions in solutions of lithium perchlorate in propylene carbonate + diethyl carbonate mixtures: an IR and molecular orbital study.

    Science.gov (United States)

    Wang, Jianji; Wu, Yanping; Xuan, Xiaopeng; Wang, Hanqing

    2002-08-01

    FTIR spectra have been recorded and analyzed for solutions of lithium perchlorate in propylene carbonate (PC), diethyl carbonate (DEC), and PC + DEC mixtures. It has been shown that the carbonyl stretch bands for PC and DEC are very sensitive to the interaction between Li+ and the solvent molecules. They split with addition of LiClO4, indicating a strong interaction of Li+ with PC and DEC through the oxygen group of PC and both oxygen and ether oxygen atoms of DEC. In conjunction with molecular orbital calculation, the optimized geometries of solvation are given. In addition, solvent separated ion pairs and contact ion pairs were observed in LiClO4/DEC solutions, and no preferential solvation of Li+ in LiClO4/PC + DEC solutions were detected.

  14. Ternary (liquid + liquid) equilibria of (diethyl carbonate + ethanol or 1-propanol + water) systems at 303.15 K under atmospheric pressure

    Science.gov (United States)

    Ginting, Rizqy Romadhona; Mustain, Asalil; Gunardi, Ignatius; Wibawa, Gede

    2017-01-01

    Ternary (liquid + liquid) equilibria data of diethyl carbonate (DEC) + ethanol or 1-propanol + water systems were accurately determined at 303.15 K using jacketed equilibrium cell under atmospheric pressure. The reliability of experimental tie-line data were checked by using Bachman-Brown correlation giving an r-squared value of 0.9933 and 0.9996, respectively. Both systems studied in this work exhibit Treybal's Type I ternary phase behavior. The experimental tie-line data were correlated well using the Non-Random Two Liquid (NRTL) and Universal Quasi-Chemical (UNIQUAC) activity coefficient models giving root-mean-square deviation (RMSD) of 0.95 and 1.18% for DEC + ethanol + water system.,While DEC + 1-propanol + water system gives RMSD value of 0.30 and 0.37%, respectively. The effect of carbon chain length of alcohol to the phase boundary of both systems was observed and discussed in detail.

  15. Simultaneous determination of curcumin diethyl disuccinate and its active metabolite curcumin in rat plasma by LC-MS/MS: Application of esterase inhibitors in the stabilization of an ester-containing prodrug.

    Science.gov (United States)

    Ratnatilaka Na Bhuket, Pahweenvaj; Niwattisaiwong, Nuansri; Limpikirati, Patanachai; Khemawoot, Phisit; Towiwat, Pasarapa; Ongpipattanakul, Boonsri; Rojsitthisak, Pornchai

    2016-10-15

    Four esterase inhibitors, ethylenediamine tetraacetic acid disodium (Na2EDTA), sodium fluoride (NaF), bis(4-nitrophenyl) phosphate (BNPP) and phenylmethanesulfonyl fluoride (PMSF), were evaluated for their inhibitory effects on enzymatic hydrolysis of labile phenolate esters in curcumin diethyl disuccinate (CDD), a prodrug of curcumin (CUR), in rat plasma. BNPP and PMSF at 10mM exhibited stabilization by preventing degradation of CDD. BNPP at a final concentration of 10mM was subsequently selected to prevent ex vivo metabolism of CDD throughout LC-MS/MS analysis of CDD and CUR in rat plasma. A simple protein precipitation technique using acetonitrile as a precipitating agent was used to extract CDD, CUR and dimethylcurcumin (DMC), an internal standard, from rat plasma. Chromatographic separation was performed on a Halo C8 column (4.6×50mm, 2.7μm) using an isocratic mobile phase containing acetonitrile-0.2% formic acid in water (73:27v/v) with a flow rate of 0.4mLmin(-1). An AB SCIEX QTRAP(®) 6500 mass spectrometer was operated using a positive ion electrospray mode for ionization and detection of analytes and internal standard. Calibration curves for CDD and CUR were established using 50μL of rat plasma over the concentration range of 1-500ngmL(-1). The developed method was fully validated according to US Food and Drug Administration (FDA) guidelines for selectivity, sensitivity, linearity, accuracy, precision, dilution integrity, recovery, matrix effect, and stability. The validated method was applied to evaluate the pharmacokinetics of CDD and CUR in rats after a single intravenous dose of 40mgkg(-1). The method using BNPP as an esterase inhibitor was successful in determining the remaining CDD in rat plasma. The pharmacokinetic results indicate that CDD in rats is converted instantaneously to CUR after intravenous administration and a higher CUR plasma concentration at 5min is achieved in comparison with direct intravenous injection of CUR. Copyright © 2016

  16. Influence of boric acid on electrospray ionization efficiency.

    Science.gov (United States)

    Rebane, Riin; Herodes, Koit

    2012-01-01

    Liquid chromatography electrospray ionization mass-spectrometry (LC-ESI-MS) was used to analyze 9-fluorenylmethylmethoxycarbonyl chloride (Fmoc-Cl) and diethyl ethoxymethylenemalonate (Deemm) derivatives of three amino acids and five other compounds. Influence of boric acid on their ionization was investigated and dramatic impact on the signal was observed. The strongest signal suppression (6% of signal remains) was observed for the Deemm derivative of beta-Alanine (with ammonium acetate in eluent). With only formic acid as the eluent pH modifier, signal enhancement was observed, being largest for Fmoc-Cl derivative of Phenylalanine, 267%. Investigation of the influence of boric acid shows that it is a possible signal enhancer for LC-ESI-MS analysis.

  17. (E)-4-[(4-Diethyl­amino-2-hy­droxy­benzyl­idene)amino]­benzoic acid

    Science.gov (United States)

    Kargar, Hadi; Sharafi, Zahra; Kia, Reza; Tahir, Muhammad Nawaz

    2012-01-01

    In the title compound, C18H20N2O3, a potential bidentate N,O-donor Schiff base ligand, the benzene rings are inclined at an angle of 12.25 (19)°. The mol­ecule has an E conformation about the C=N bond. One of the ethyl groups is disordered over two positions, with a refined site-occupancy ratio of 0.55 (1):0.45 (1). An intra­molecular O—H⋯N hydrogen bond makes an S(6) ring motif. In the crystal, pairs of O—H⋯O hydrogen bonds link mol­ecules, forming inversion dimers with R 2 2(8) ring motifs. PMID:22589907

  18. Impact of gluconic fermentation of strawberry using acetic acid bacteria on amino acids and biogenic amines profile.

    Science.gov (United States)

    Ordóñez, J L; Sainz, F; Callejón, R M; Troncoso, A M; Torija, M J; García-Parrilla, M C

    2015-07-01

    This paper studies the amino acid profile of beverages obtained through the fermentation of strawberry purée by a surface culture using three strains belonging to different acetic acid bacteria species (one of Gluconobacter japonicus, one of Gluconobacter oxydans and one of Acetobacter malorum). An HPLC-UV method involving diethyl ethoxymethylenemalonate (DEEMM) was adapted and validated. From the entire set of 21 amino acids, multiple linear regressions showed that glutamine, alanine, arginine, tryptophan, GABA and proline were significantly related to the fermentation process. Furthermore, linear discriminant analysis classified 100% of the samples correctly in accordance with the microorganism involved. G. japonicus consumed glucose most quickly and achieved the greatest decrease in amino acid concentration. None of the 8 biogenic amines were detected in the final products, which could serve as a safety guarantee for these strawberry gluconic fermentation beverages, in this regard.

  19. Synthesis of 2- (3-Hydroxy- 1-adamantyl) -2-glyoxylic Acid%2-(3-羟基-1-金刚烷基)-2-乙醛酸的合成

    Institute of Scientific and Technical Information of China (English)

    李靖柯; 周鸿睿; 彭俊; 冯悦; 胡湘南

    2012-01-01

    金刚烷经相继甲酸化、酰氯化后与丙二酸二乙酯乙氧基镁反应,得到1-金刚烷甲酰基丙二酸二乙酯,再经水解脱羧、高锰酸钾氧化得到沙克列汀中间体2-(3-羟基-1-金刚烷基)-2-乙醛酸,总收率约28%.%2-(3-Hydroxy-l-adamantyl)-2-glyoxyiic acid, the intermediate of saxagliptin, was synthesized from adamantane via successive reactions with formic acid, thiotiyl chloride and diethyl ethoxymagnesium malonate to give diethyl 1-adamantaneformyl malonate. which was subjected to hydrolysis and decarboxylation by mixed acid and then oxidation by potassium permanganate. The overall yield was about 28%.

  20. A comparative study of anaerobic fixed film baffled reactor and up-flow anaerobic fixed film fixed bed reactor for biological removal of diethyl phthalate from wastewater: a performance, kinetic, biogas, and metabolic pathway study.

    Science.gov (United States)

    Yousefzadeh, Samira; Ahmadi, Ehsan; Gholami, Mitra; Ghaffari, Hamid Reza; Azari, Ali; Ansari, Mohsen; Miri, Mohammad; Sharafi, Kiomars; Rezaei, Soheila

    2017-01-01

    Phthalic acid esters, including diethyl phthalate (DEP), which are considered as top-priority and hazardous pollutants, have received significant attention over the last decades. It is vital for industries to select the best treatment technology, especially when the DEP concentration in wastewater is high. Meanwhile, anaerobic biofilm-based reactors are considered as a promising option. Therefore, in the present study, for the biological removal of DEP from synthetic wastewater, two different anaerobic biofilm-based reactors, including anaerobic fixed film baffled reactor (AnFFBR) and up-flow anaerobic fixed film fixed bed reactor (UAnFFFBR), were compared from kinetic and performance standpoints. As in the previous studies, only the kinetic coefficients have been calculated and the relationship between kinetic coefficients and their interpretation has not been evaluated, the other aim of the present study was to fill this research gap. In optimum conditions, 90.31 and 86.91% of COD as well as 91.11 and 88.72% of DEP removal were achieved for the AnFFBR and UAnFFFBR, respectively. According to kinetic coefficients (except biomass yield), the AnFFBR had better performance as it provided a more favorable condition for microbial growth. The Grau model was selected as the best mathematical model for designing and predicting the bioreactors' performance due to its high coefficients of determination (0.97 < R(2)). With regard to the insignificant variations of the calculated Grau kinetic coefficients (KG) when the organic loading rate (with constant HRT) increased, it can be concluded that both of the bioreactors can tolerate high organic loading rate and their performance is not affected by the applied DEP concentrations. Both the bioreactors were capable of treating low-to-high strength DEP wastewater; however, according to the experimental results and obtained kinetic coefficients, the AnFFBR indicated higher performance. Although the AnFFBR can be considered as a

  1. 甲基丙烯酰氧乙基二乙基磷酰胺的合成及乳化%Synthesis and Emulsification of Methacryloyl Chloride Ethyl Diethyl Phosphoric Amide

    Institute of Scientific and Technical Information of China (English)

    王昭飞; 关晋平; 陈国强; 曹雪琴

    2011-01-01

    以三氯化磷、无水乙醇、四氯化碳、单乙醇胺、甲基丙烯酰氯为原料,合成出一种磷氮系纺织品阻燃剂--甲基丙烯酰氧乙基二乙基磷酰胺,其结构经过HNMR、CNMR、PNMR和IR表征.结果表明,以三乙胺为缚酸剂,二氯甲烷为溶剂,将9.05 g甲基丙烯酰氯(0.1 mo1)于0℃滴入装有17.2 g氯膦酸二乙酯(0.1 mo1)和6.1 g乙醇胺(0.1 mol)的三颈瓶中,滴完,升至室温反应12 h,所得粗产物在135℃/13.3 Pa减压蒸馏,得到淡黄色黏稠液体,产率为69%.考察了产物的乳化条件并测试了其乳液的粒径及稳定性,表明在HLB=9时乳液的粒径最小,乳液的平均粒径为123.5 nm,Zeta电位为+30.193 mV.%A flame retardant containing nitrogen-phosphor for textiles was synthesized from phosphorus trichloride, absolute ethylalcohol, carbon tetrachloride, monoethanol amine, methacryloyl chloride.The structure was characterized by method of 1HNMR,13CNMR,31PNMR and IR.The results show that 17.2 g diethyl chlorophosphate (0.1 mol), 6.1 g ethanolamine ( 0.1 mol ) and 9.05 g methacryloyl chloride(0.1 mol) finished dropping at 0 ℃ , then reacted for 12 h at room temperature, with triethylamine as acid-binding agent and dichloromethane as solution, and the yield coefficient was 69% under vacuum distillation of 135 ℃/13.3 Pa.The different conditions of emulsion were researched.The test of the grain diameter of latex emulsion and its stability shows that the minimum diameter of emulsion forms in HLB =9,and the average of diameter is 123.5 nm,the Zeta is +30.193 mV.

  2. 2-亚磷酸二乙酯基杂环烯酮缩胺类化合物的合成%Synthesis of 2-Diethyl Phosphate Heterocyclic Ketene Aminals

    Institute of Scientific and Technical Information of China (English)

    余富朝; 严胜骄; 贺能琴; 林军

    2011-01-01

    用廉价易得原料Mn(OAc)2-KMnO4体系代替昂贵的Mn(OAc)3催化二甲缩硫醚(1)与亚磷酸二乙酯反应获得结构新颖的2-亚磷酸二乙酯基缩硫醚化合物2a~2d.然后,化合物2a~2d与二胺类化合物3反应以较高产率合成了一系列2-亚磷酸二乙酯基杂环烯酮缩胺(4).%Mercaptals (1), with low-cost and readily available Mn(Oac)2-KMnO4 system instead of the expensive Mn(Oac)3 as catalyst, reacted with diethyl phosphite to give novel 2-diethyl phosphate mercaptals 2a~2d. Sequentially, compounds 2a~2d reacted with diamines 3 to afford a series of 2-diethyl phosphate heterocyclic ketene amines (4) with good yields.

  3. Is there a risk associated with the insect repellent DEET (N,N-diethyl-m-toluamide) commonly found in aquatic environments?

    Science.gov (United States)

    Costanzo, S.D.; Watkinson, A.J.; Murby, E.J.; Kolpin, D.W.; Sandstrom, M.W.

    2007-01-01

    DEET (N,N-diethyl-m-toluamide) is the active ingredient of most commercial insect repellents. This compound has commonly been detected in aquatic water samples from around the world indicating that DEET is both mobile and persistent, despite earlier assumptions that DEET was unlikely to enter aquatic ecosystems. DEET's registration category does not require an ecological risk assessment, thus information on the ecological toxicity of DEET is sparse. This paper reviews the presence of DEET in aqueous samples from around the world (e.g. drinking water, streams, open seawater, groundwater and treated effluent) with reported DEET concentrations ranging from 40–3000 ng L− 1. In addition, new DEET data collected from 36 sites in coastal waterways from eastern Australia (detections ranging from 8 to 1500 ng L− 1) are examined. A summary of new and existing toxicity data are discussed with an emphasis on preparing a preliminary risk assessment for DEET in the aquatic environment. Collated information on DEET in the aquatic environment suggests risk to aquatic biota at observed environmental concentrations is minimal. However, the information available was not sufficient to conduct a full risk assessment due to data deficiencies in source characterisation, transport mechanisms, fate, and ecotoxicity studies. These risks warrant further investigation due to the high frequency that this organic contaminant is detected in aquatic environments around the world.

  4. The insect repellent N,N-diethyl-m-toluamide (DEET) induces angiogenesis via allosteric modulation of the M3 muscarinic receptor in endothelial cells.

    Science.gov (United States)

    Legeay, Samuel; Clere, Nicolas; Hilairet, Grégory; Do, Quoc-Tuan; Bernard, Philippe; Quignard, Jean-François; Apaire-Marchais, Véronique; Lapied, Bruno; Faure, Sébastien

    2016-06-27

    The insect repellent N,N-diethyl-m-toluamide (DEET) has been reported to inhibit AChE (acetylcholinesterase) and to possess potential carcinogenic properties with excessive vascularization. In the present paper, we demonstrate that DEET specifically stimulates endothelial cells that promote angiogenesis which increases tumor growth. DEET activates cellular processes that lead to angiogenesis including proliferation, migration and adhesion. This is associated with an enhancement of NO production and VEGF expression in endothelial cells. M3 silencing or the use of a pharmacological M3 inhibitor abrogates all of these effects which reveals that DEET-induced angiogenesis is M3 sensitive. The experiments involving calcium signals in both endothelial and HEK cells overexpressing M3 receptors, as well as binding and docking studies demonstrate that DEET acts as an allosteric modulator of the M3 receptor. In addition, DEET inhibited AChE which increased acetylcholine bioavailability and binding to M3 receptors and also strengthened proangiogenic effects by an allosteric modulation.

  5. The insect repellent DEET (N,N-diethyl-3-methylbenzamide) increases the synthesis of glutathione S-transferase in cultured mosquito cells.

    Science.gov (United States)

    Hellestad, Vanessa J; Witthuhn, Bruce A; Fallon, Ann M

    2011-04-01

    DEET (N,N-diethyl-3-methylbenzamide) is the active ingredient used in many commonly used insect repellents, but its mode of action remains poorly understood. Efforts to identify properties that could lead to the development of more effective active ingredients have distinguished among DEET's repellent, deterrent, and insecticidal activities. We used an Aedes albopictus mosquito cell line to evaluate DEET's toxicological properties in the absence of sensory input mediated by the olfactory system. When cells were treated with DEET and labeled with [(35)S]methionine/cysteine, a single 25-kDa protein was induced, relative to other proteins, on SDS-polyacrylamide gels. The 25-kDa band from DEET-treated cells was enriched in peptides corresponding to glutathione S-transferase D10 and/or theta in the Aedes aegypti genome. Consistent with the increased expression of the labeled protein, DEET-treated cells had increased glutathione S-transferase activity, and the radiolabeled band bound to Sepharose 4B containing reduced glutathione. By analyzing partial tryptic digests, we established that DEET induces the homolog of A. aegypti glutathione S-transferase, class theta, corresponding to protein XP_001658009.1 in the NCBI database. This specific effect of DEET at the subcellular level suggests that DEET induces physiological responses that extend beyond recognition by the peripheral olfactory system.

  6. Reaction mechanisms in ionic liquids: the kinetics and mechanism of the reaction of O,O-diethyl (2,4-dinitrophenyl) phosphate triester with secondary alicyclic amines.

    Science.gov (United States)

    Pavez, Paulina; Millán, Daniela; Morales, Javiera; Rojas, Mabel; Céspedes, Daniel; Santos, José G

    2016-01-28

    The reactions of O,O-diethyl 2,4-dinitrophenyl phosphate triester (1) with secondary alicyclic (SA) amines in the ionic liquids [Bmim]BF4 and [Bmim]DCA were subjected to a kinetic study. Eyring plots were obtained for the title reactions in the above ionic liquids (ILs) and also in aqueous ethanol (44 wt% ethanol). Two different reaction pathways were observed in [Bmim]BF4: nucleophilic attack at the phosphoryl center, SN2(P), and at the C-1 aromatic carbon, SN(Ar), where the product distribution remained constant and independent of the amine nature. In contrast, in [Bmim]DCA only the SN2(P) pathway was found. From the kinetic analysis of the SN2(P) pathway in both ILs, curved upwards plots of kobsdvs. 1-formylpiperazine concentration were obtained. Based on the kinetic behavior, a change in the mechanism of the SN2(P) pathway is proposed for the aminolysis of 1, from a concerted process in aqueous ethanol to a stepwise mechanism, through a zwitterionic pentacoordinate intermediate, when [Bmim]BF4 and [Bmim]DCA are used as the solvents of the reaction.

  7. Identification of Diethyl 2,5-Dioxahexane Dicarboxylate and Polyethylene Carbonate as Decomposition Products of Ethylene Carbonate Based Electrolytes by Fourier Transform Infrared Spectroscopy

    KAUST Repository

    Shi, Feifei

    2014-07-10

    The formation of passive films on electrodes due to electrolyte decomposition significantly affects the reversibility of Li-ion batteries (LIBs); however, understanding of the electrolyte decomposition process is still lacking. The decomposition products of ethylene carbonate (EC)-based electrolytes on Sn and Ni electrodes are investigated in this study by Fourier transform infrared (FTIR) spectroscopy. The reference compounds, diethyl 2,5-dioxahexane dicarboxylate (DEDOHC) and polyethylene carbonate (poly-EC), were synthesized, and their chemical structures were characterized by FTIR spectroscopy and nuclear magnetic resonance (NMR). Assignment of the vibration frequencies of these compounds was assisted by quantum chemical (Hartree-Fock) calculations. The effect of Li-ion solvation on the FTIR spectra was studied by introducing the synthesized reference compounds into the electrolyte. EC decomposition products formed on Sn and Ni electrodes were identified as DEDOHC and poly-EC by matching the features of surface species formed on the electrodes with reference spectra. The results of this study demonstrate the importance of accounting for the solvation effect in FTIR analysis of the decomposition products forming on LIB electrodes. © 2014 American Chemical Society.

  8. Spectrophotometric determination of platinum(IV) in alloys, complexes, environmental, and pharmaceutical samples using 4-[N,N-(diethyl)amino] benzaldehyde thiosemicarbazone.

    Science.gov (United States)

    Naik, P Parameshwara; Karthikeyan, J; Shetty, A Nityananda

    2010-12-01

    4-[N,N-(Diethyl)amino] benzaldehyde thiosemicarbazone (DEABT) is proposed as an analytical reagent for the spectrophotometric determination of platinum(IV). The DEABT forms 1:2 yellow complex with Pt(IV), which is sparingly soluble in water and completely soluble in water-ethanol-DMF medium. The Pt(IV)-DEABT complex shows maximum absorbance at 405 nm. Beer's law is valid up to 7.80 μg cm(-3), and optimum concentration range for the determination of platinum(IV) is 0.48-7.02 μg cm(-3). The molar absorptivity and Sandell's sensitivity of the method are found to be 1.755 × 10(4) dm(3) mol(-1) cm(-1) and 0.0012 μg cm(-2), respectively. The relative error and coefficient of variation (n=6) for the method does not exceed ± 0.43% and 0.35%, respectively. Since the method tolerates a number of metal ions commonly associated with platinum, it can be employed for the determination of platinum in environmental samples, pharmaceutical samples, alloys, catalysts, and complexes. The method is rapid as the Pt(IV)-DEABT complex is soluble in water-ethanol-DMF medium and not requiring any time consuming extraction method for the complex.

  9. Metal assisted approach to develop molecularly imprinted mesoporous material exhibiting pockets for the fast uptake of diethyl phthalate as copper complex.

    Science.gov (United States)

    Kaur, Prabhjot; Narula, Priyanka; Kaur, Varinder; Singh, Raghubir; Kansal, Sushil Kumar

    2014-01-01

    A new molecularly imprinted mesoporous material (MIM) containing specific pockets for the extraction of diethyl phthalate (DEP) as copper complex has been prepared for the first time. The mesoporous material was developed by utilizing copper-phthalate complex (Cu-DEP) as the template molecule, 3-aminopropyltriethoxysilane (APS) as a functional monomer and tetraethoxyorthosilicate (TEOS) as the silica source for polymer network formation. The mesoporous material showed fast uptake kinetics, and equilibrium was obtained within 30 min due to the introduction of copper, which provides an additional site for interaction with the functional monomer. Synthesized polymer was well characterized using UV-Vis spectrophotometry, IR spectroscopy, TGA studies, and TEM. To achieve efficient extraction of the template molecule, various factors including sorption kinetics, quantity of MIM, time required for equilibrium set-up, sorption isotherm and reuse of MIM were optimized. The extracted DEP samples were analyzed quantitatively at 310 nm using an HPLC-DA system. The prepared material is robust and can be reused. In addition, it was found to be selective for DEP as compared to other phthalates.

  10. An Uncommon Plant Growth Regulator, Diethyl Aminoethyl Hexanoate, Is Highly Effective in Tissue Cultures of the Important Medicinal Plant Purple Coneflower (Echinacea purpurea L.

    Directory of Open Access Journals (Sweden)

    Xiao-Lu Chen

    2013-01-01

    Full Text Available We investigated the effects of various concentrations of diethyl aminoethyl hexanoate (DA-6 on the regeneration and growth of adventitious buds in in vitro purple coneflower cultures. Among the 3 types of explants tested, leaf explants required higher concentrations of DA-6 than petiole and root explants in order to obtain high regeneration rates, while root explants required the lowest concentration of DA-6. Additionally, explants with higher ploidy levels were more sensitive to the addition of DA-6, while explants with lower ploidy levels required higher concentrations of DA-6 to achieve its maximal regeneration rate. Interestingly, the application of a concentration that was conducive to the regeneration of explants with lower ploidy levels was inhibitory to the regeneration of explants with higher ploidy levels. Moreover, during the growth of regenerated buds, DA-6 application significantly improved plant height and weight, root weight, root thickness, root number, primary root length, total root length, and root/top ratio. Differences in the responses of explants to supplementation with DA-6 were also observed among explants with different ploidy levels, with buds having lower ploidy levels responding to lower concentrations of DA-6. Taken together, the results of the present experiments showed that proper application of DA-6 could increase in vitro culture efficiency in purple coneflower.

  11. Methotrexate diethyl ester-loaded lipid-core nanocapsules in aqueous solution increased antineoplastic effects in resistant breast cancer cell line

    Science.gov (United States)

    Yurgel, Virginia C; Oliveira, Catiuscia P; Begnini, Karine R; Schultze, Eduarda; Thurow, Helena S; Leon, Priscila MM; Dellagostin, Odir A; Campos, Vinicius F; Beck, Ruy CR; Guterres, Silvia S; Collares, Tiago; Pohlmann, Adriana R; Seixas, Fabiana K

    2014-01-01

    Breast cancer is the most frequent cancer affecting women. Methotrexate (MTX) is an antimetabolic drug that remains important in the treatment of breast cancer. Its efficacy is compromised by resistance in cancer cells that occurs through a variety of mechanisms. This study evaluated apoptotic cell death and cell cycle arrest induced by an MTX derivative (MTX diethyl ester [MTX(OEt)2]) and MTX(OEt)2-loaded lipid-core nanocapsules in two MTX-resistant breast adenocarcinoma cell lines, MCF-7 and MDA-MB-231. The formulations prepared presented adequate granulometric profile. The treatment responses were evaluated through flow cytometry. Relying on the mechanism of resistance, we observed different responses between cell lines. For MCF-7 cells, MTX(OEt)2 solution and MTX(OEt)2-loaded lipid-core nanocapsules presented significantly higher apoptotic rates than untreated cells and cells incubated with unloaded lipid-core nanocapsules. For MDA-MB-231 cells, MTX(OEt)2-loaded lipid-core nanocapsules were significantly more efficient in inducing apoptosis than the solution of the free drug. S-phase cell cycle arrest was induced only by MTX(OEt)2 solution. The drug nanoencapsulation improved apoptosis induction for the cell line that presents MTX resistance by lack of transport receptors. PMID:24741306

  12. Chemical modification of contractile 3-nm-diameter filaments in Vorticella spasmoneme by diethyl-pyrocarbonate and its reversible renaturation by hydroxylamine.

    Science.gov (United States)

    Fang, Jie; Zhang, Bei; Asai, Hiroshi

    2003-10-31

    A peritrich ciliate possesses a zooid and a long stalk consisting of a bundle of 3-nm-diameter filaments. Glycerinated stalks can contract in the presence of free Ca(2+) and re-extend in the absence of free Ca(2+). In the present study, we demonstrated that histidine residue(s) played a critical role in spasmoneme contraction by using glycerinated stalk of Vorticella. Concentration-dependent inhibition of spasmoneme contraction was observed in the presence of reversible histidine-modifying reagent named diethyl-pyrocarbonate (DEPC). In addition, the contractility degree of DEPC-modified spasmoneme could be partially restored by hydroxylamine treatment. The 244nm absorption of modified spasmoneme protein(s) increased with rising DEPC concentration and decreased following the addition of hydroxylamine treatment. Adding Ca(2+) before DEPC modification could prevent the spasmoneme contraction from inhibition of DEPC. Those results suggested that histidine residues were actively involved in spasmoneme contraction. Ca(2+)-binding ability of spasmin was not inhibited by DEPC modification, which suggested that the essential histidine residues were not on the calcium-binding site of spasmin.

  13. Ozone/graphene oxide catalytic oxidation: a novel method to degrade emerging organic contaminant N, N-diethyl-m-toluamide (DEET)

    Science.gov (United States)

    Liu, Jia-Nan; Chen, Zhuo; Wu, Qian-Yuan; Li, Ang; Hu, Hong-Ying; Yang, Cheng

    2016-08-01

    N, N-diethyl-m-toluamide (DEET) is one of the important emerging contaminants that are being increasingly detected in reclaimed water as well as in drinking water sources. However, DEET is refractory to conventional biological treatment and pure ozone which is absent of hydroxyl radical. Current researches on the efficient removal of DEET are still quite limited. This study utilizes a novel method, namely ozone/graphene oxide (O3/GO), to investigate the effects on DEET removal in aqueous systems, especially in reclaimed water. The results indicate that the DEET degradation rate was significantly accelerated through the combined effect of GO and ozonation which can yield abundant hydroxyl radical, compared to pure ozone condition. According to hydroxyl radical scavenging experiments, hydroxyl radical was found to play a dominant role in synergistic removal of DEET. These findings can offer sound suggestions for future research on the removal of emerging organic contaminants. The information could also be beneficial to reclaimed water safety and sustainable management.

  14. Validation of an aggregate exposure model for substances in consumer products: a case study of diethyl phthalate in personal care products.

    Science.gov (United States)

    Delmaar, Christiaan; Bokkers, Bas; ter Burg, Wouter; Schuur, Gerlienke

    2015-05-01

    As personal care products (PCPs) are used in close contact with a person, they are a major source of consumer exposure to chemical substances contained in these products. The estimation of realistic consumer exposure to substances in PCPs is currently hampered by the lack of appropriate data and methods. To estimate aggregate exposure of consumers to substances contained in PCPs, a person-oriented consumer exposure model has been developed (the Probabilistic Aggregate Consumer Exposure Model, PACEM). The model simulates daily exposure in a population based on product use data collected from a survey among the Dutch population. The model is validated by comparing diethyl phthalate (DEP) dose estimates to dose estimates based on biomonitoring data. It was found that the model's estimates compared well with the estimates based on biomonitoring data. This suggests that the person-oriented PACEM model is a practical tool for assessing realistic aggregate exposures to substances in PCPs. In the future, PACEM will be extended with use pattern data on other product groups. This will allow for assessing aggregate exposure to substances in consumer products across different product groups.

  15. An uncommon plant growth regulator, diethyl aminoethyl hexanoate, is highly effective in tissue cultures of the important medicinal plant purple coneflower (Echinacea purpurea L.).

    Science.gov (United States)

    Chen, Xiao-Lu; Zhang, Jun-Jie; Chen, Rong; Li, Qing-Ling; Yang, Yue-Sheng; Wu, Hong

    2013-01-01

    We investigated the effects of various concentrations of diethyl aminoethyl hexanoate (DA-6) on the regeneration and growth of adventitious buds in in vitro purple coneflower cultures. Among the 3 types of explants tested, leaf explants required higher concentrations of DA-6 than petiole and root explants in order to obtain high regeneration rates, while root explants required the lowest concentration of DA-6. Additionally, explants with higher ploidy levels were more sensitive to the addition of DA-6, while explants with lower ploidy levels required higher concentrations of DA-6 to achieve its maximal regeneration rate. Interestingly, the application of a concentration that was conducive to the regeneration of explants with lower ploidy levels was inhibitory to the regeneration of explants with higher ploidy levels. Moreover, during the growth of regenerated buds, DA-6 application significantly improved plant height and weight, root weight, root thickness, root number, primary root length, total root length, and root/top ratio. Differences in the responses of explants to supplementation with DA-6 were also observed among explants with different ploidy levels, with buds having lower ploidy levels responding to lower concentrations of DA-6. Taken together, the results of the present experiments showed that proper application of DA-6 could increase in vitro culture efficiency in purple coneflower.

  16. One-Pot Three-Component Synthesis of Novel Diethyl((2-oxo-1,2-dihydroquinolin-3-yl(arylaminomethylphosphonate as Potential Anticancer Agents

    Directory of Open Access Journals (Sweden)

    Yi-Lin Fang

    2016-04-01

    Full Text Available With the aim of discovering new anticancer agents, we have designed and synthesized novel α-aminophosphonate derivatives containing a 2-oxoquinoline structure using a convenient one-pot three-component method. The newly synthesized compounds were evaluated for antitumor activities against the A549 (human lung adenocarcinoma cell, HeLa (human cervical carcinoma cell, MCF-7 (human breast cancer cell, and U2OS (human osteosarcoma cell cancer cell lines in vitro, employing a standard 3-(4,5-dimethyl-2-thiazolyl-2,5-diphenyl-2-H-tetrazolium bromide (MTT assay. The results of pharmacological screening indicated that many compounds exhibited moderate to high levels of antitumor activities against the tested cancer cell lines and that most compounds showed more potent inhibitory activities comparable to 5-fluorouracil (5-FU which was used as a positive control. The mechanism of representative compound 4u (diethyl((2-oxo-1,2-dihydroquinolin-3-yl(phenyl-aminomethylphosphonate indicated that the compound mainly arrested HeLa cells in S and G2 stages and was accompanied by apoptosis in HeLa cells. This action was confirmed by acridine orange/ethidium bromide staining, Hoechst 33342 staining, and flow cytometry.

  17. 丙二酸二乙酯的生产工艺改进%Malonic Diethyl Production Process ImProvement

    Institute of Scientific and Technical Information of China (English)

    张东卫; 杨国忠; 王虹

    2015-01-01

    Diethyl malonate is an important organic synthetic intermediate and has important use in medicine,spices,dye and other industrial. The traditional production process to produce cyanide containing waste water and high salt wastewater cannot be processed. Now most of new process are not in need to achieve industrial development theories or experimental stage. By improving of now traditional technology,adding alkali solution process,more environmental protection,avoid the cyanide containing wastewater,highcomplex salt waste liquid produced,are very good for industrialization.%丙二酸二乙酯是重要的有机合成中间体,在医药、香料、染料等工业有重要用途。传统的生产工艺含氰废水和高复盐废液无法处理。现在新的工艺,大多处于理论或小试阶段还不能达到工业发展的需要。通过对现在传统工艺改进,加入碱解工艺,更加环保,避免了含氰废水、高复盐废液的产生,非常有利于工业化的进行。

  18. Synthesis of Diethyl Carbonate from Carbon Dioxide, Propylene Oxide and Ethanol over KNO3-CeO2 and KBr-KNO3-CeO2 Catalysts

    Directory of Open Access Journals (Sweden)

    Yanlou Wang

    2016-03-01

    Full Text Available One-pot syntheses of diethyl carbonate (DEC from CO2, propylene oxide and ethanol were carried out using different solid catalysts. The supercritical CO2 extraction method was used to separate the liquid products and reactants from the catalysts after reaction. The KNO3-CeO2 and KBr-KNO3-CeO2 were found to be active for the reaction after calcinations. The catalyst was also reusable. The thermodynamic properties of the reaction were also evaluated. The effects of various conditions, such as reaction time, amount of catalysts, molar ratio of the reactants, the composition and calcination temperature of the catalysts on the conversion and yields, were investigated, and the yield of DEC was about 13.0% with a selectivity of 38.5% over KBr-KNO3-CeO2. The yield of DEC was improved about 10-fold by using KBr-KNO3-CeO2 catalyst compared to CeO2.

  19. Corrosion Inhibition of 316L Steel Using Sodium Diethyl Dithiocarbamate in Simulated Crude Oil Solution%二乙基二硫代氨基甲酸钠在原油模拟液中对316L钢的缓蚀作用

    Institute of Scientific and Technical Information of China (English)

    任晓光; 杨杰

    2012-01-01

    The corrosion inhibition behaviors of 316L steel using the sodium diethyl dithiocarbamate(SDDTC) compound in simulated crude oil solution were studied in the absence and presence of zinc sulfate or sodium chromate with different combinations.Experiment results showed that in the environments of high acidity and high concentrations of chloride ions the SDDTC compound could well inhibit the corrosion of 316L steel.The good synergic effects on the corrosion inhibition of 316L steel by additions of either zinc sulfate or sodium chromate into SDDTC compound were indicated in this study,which is of great significance and importance in practical applications.%配制原油模拟液,研究了二乙基二硫代氨基甲酸钠(SDDTC)于模拟液中单独使用以及分别与硫酸锌,铬酸钠的复配对316L钢的缓蚀效果.实验表明:在高酸高氯环境下,SDDTC能够很好地抑制316L钢的腐蚀;而且SDDTC与硫酸锌、铬酸钠之复配缓蚀剂具有很好的协同增效作用.这一相关研究具有重要的实际应用意义.

  20. Comparison of three buffer solutions for amino acid derivatization and following analysis by liquid chromatography electrospray mass spectrometry.

    Science.gov (United States)

    Rebane, Riin; Herodes, Koit

    2012-07-06

    For reversed phase separation amino acids are usually derivatized. Several derivatization reactions are carried out at basic pH. In the present work, influence of three basic buffer solutions on liquid chromatography electrospray ionization mass-spectrometric (LC-ESI-MS) analysis of amino acid derivatives was studied. Borate buffer--the most common derivatization buffer--was found to influence ESI ionization up to 23 min retention time. For 9-fluorenylmethylmethoxycarbonyl chloride (Fmoc-Cl derivatization) carbonate buffer should be preferred as it provides higher responses. Hexafluoroisopropanol (HFIP) buffer improves chromatographic peak shapes and responses for diethyl ethoxymethylenemalonate (DEEMM) derivatives.

  1. Choleretic effect of structural analogs of valproic acid in the rat.

    Science.gov (United States)

    Watkins, J B; Klaassen, C D

    1983-03-01

    A comparison of structure-choleretic activity relationship has been made for several branched- and straight-chain carboxylic acids including valproic acid. Cumulative bile flow was 13.8, 23.8, 29.4 and 14.9 ml/4hr/kg body weight for dimethyl-, diethyl-, dipropyl- (valproic acid), and dibutyl-acetic acid, respectively, after iv administration of approximately equimolar doses (1100 mumoles/kg). Except for dibutylacetic acid, maximal bile flow increased from control rates of 50-60 to 120-140 microliters/min/kg. Administration of higher doses of 2,2-dimethylbutanoic acid and 2-ethylbutanoic acid did not increase maximal bile flow above 125-140 microliters/min/kg but did prolong the duration of choleresis. Maximal and cumulative bile flows increased with length of carboxylic acid chain for 2,2-dimethyl substituted acids (2,2-dimethylacetic acid to 2,2-dimethylbutanoic acid). If the two methyl groups were on C-3 (3-methylbutanoic acid), no change in bile flow was observed. Straight-chain acids from C-5 to C-11 and pent-4-enoic acid did not alter bile flow. Thus, the effectiveness of several branched-chain carboxylic acids as choleretics parallel their ability as anticonvulsants. In contrast, the straight-chain acids which cause central nervous system depression have no choleretic activity.

  2. Pharmacokinetics and Concentration-Effect Relationship of Oral LSD in Humans.

    Science.gov (United States)

    Dolder, Patrick C; Schmid, Yasmin; Haschke, Manuel; Rentsch, Katharina M; Liechti, Matthias E

    2015-06-24

    The pharmacokinetics of oral lysergic acid diethylamide are unknown despite its common recreational use and renewed interest in its use in psychiatric research and practice. We characterized the pharmacokinetic profile, pharmacokinetic-pharmacodynamic relationship, and urine recovery of lysergic acid diethylamide and its main metabolite after administration of a single oral dose of lysergic acid diethylamide (200 μg) in 8 male and 8 female healthy subjects. Plasma lysergic acid diethylamide concentrations were quantifiable (>0.1 ng/mL) in all the subjects up to 12 hours after administration. Maximal concentrations of lysergic acid diethylamide (mean±SD: 4.5±1.4 ng/mL) were reached (median, range) 1.5 (0.5-4) hours after administration. Concentrations then decreased following first-order kinetics with a half-life of 3.6±0.9 hours up to 12 hours and slower elimination thereafter with a terminal half-life of 8.9±5.9 hours. One percent of the orally administered lysergic acid diethylamide was eliminated in urine as lysergic acid diethylamide, and 13% was eliminated as 2-oxo-3-hydroxy-lysergic acid diethylamide within 24 hours. No sex differences were observed in the pharmacokinetic profiles of lysergic acid diethylamide. The acute subjective and sympathomimetic responses to lysergic acid diethylamide lasted up to 12 hours and were closely associated with the concentrations in plasma over time and exhibited no acute tolerance. These first data on the pharmacokinetics and concentration-effect relationship of oral lysergic acid diethylamide are relevant for further clinical studies and serve as a reference for the assessment of intoxication with lysergic acid diethylamide. © The Author 2015. Published by Oxford University Press on behalf of CINP.

  3. Rapid Synthesis of Flavor Compound 4-Ethyloctanoic Acid under Microwave Irradiation

    Science.gov (United States)

    Liu, Yu-Ping; Yin, De-Cai; Chen, Hai-Tao; Sun, Bao-Guo

    2010-01-01

    Rapid synthesis of 4-ethyloctanoic acid by means of microwave irradiation is described. Diethyl malonate reacted with 2-ethyl-1-bromohexane in the presence of sodium ethoxide to give diethyl (2-ethylhexyl)malonate (1b). 1b was saponified in the solution of ethanol and potassium hydroxide and then acidified to form (2-ethylhexyl)propanedioic acid (1c), and 1c was heated and decarboxylized to give 4-ethyloctanoic acid (1d). The influence of reaction temperature and reaction time on the yield of 1b and the effect of reaction time on the yield of 1c and 1d were investigated in order to optimize the synthetic conditions. The relative optimal conditions for the synthesis of 1b were a mole ratio of sodium to diethyl malonate to 2-ethylhexyl bromide of 0.1:0.11:0.11, a reaction temperature of 80–85 °C, and a reaction time of 2–2.5 h. The yield of 1b was about 79%. 1b was saponified for 30 min and then acidified to form 1c, and the yield of 1c was 96%. 1c was heated for 16 min at 180°C to give 1d, and the yield of 1d was about 90%. The overall yield of 1d is 70% under microwave irradiation. The reaction time was reduced greatly. In order to compare the result of microwave irradiation with that of an oil bath, the reactions were also performed in an oil bath. The structures of intermediates, product and by-product were confirmed by HRMS, 1H NMR, 13C-NMR and IR. PMID:21152328

  4. 乙醇在浓硫酸催化下,温度不同产物不同之因探析%Analysis of Reasons for Different Products of Alcohol at Different Temperatures with Concentrated Sulfuric Acid as Catalyst

    Institute of Scientific and Technical Information of China (English)

    侯月芳

    2014-01-01

    乙醇在浓硫酸催化下脱水反应,生成乙醚与乙烯的主要因素是温度。文章分析了不同温度下的产物。%The main factor for alcohol to produce diethyl ether and ethylene in the dehydration re-action with concentrated sulfuric acid as catalyst is the temperature .The paper analyzes the products at different temperatures .

  5. Degradation of diethyl phthalate in treated effluents from an MBR via advanced oxidation processes: effects of nitrate on oxidation and a pilot-scale AOP operation.

    Science.gov (United States)

    Park, J H; Park, C G; Lee, J W; Ko, K B

    2010-01-01

    The major objective of this study was to delineate the oxidation of diethyl phthalate (DEP) in water, using bench-scale UV/H2O2 and O3/H2O2 processes, and to determine the effects of nitrate (NO(3-)-N, 5 mg L(-1)) on this oxidation. The oxidation of DEP was also investigated through a pilot-scale advanced oxidation process (AOP), into which a portion of the effluent from a pilot-scale membrane bioreactor (MBR) plant was pumped. The bench-scale operation showed that DEP could be oxidized via solely UV oxidation or O3 oxidation. The adverse effect of nitrate on the DEP oxidation was remarkable in the UV/H2O2 process, and the nitrate clearly reduced its oxidation. The adverse effect of nitrate on O3 oxidation was also observed. It was noted, however, that the nitrate clearly enhanced the DEP oxidation in the O3/H2O2 process. A series of pilot-scale AOP operations indicated that the addition of H2O2 enhanced DEP oxidation in both the UV/H2O2 and O3/H2O2 processes. No noticeable adverse effect of nitrate was observed in the NO(3-)-N concentration of about 6.0 mg L(-1), which was naturally contained in the treatment stream. About 52% and 61% of the DEP were oxidized by each of these two oxidation processes in this pilot-scale operation. Both the UV/H2O2 and O3/H2O2 processes appeared to be desirable alternatives for DEP oxidation in treatment effluent streams.

  6. Fe/S doped granular activated carbon as a highly active heterogeneous persulfate catalyst toward the degradation of Orange G and diethyl phthalate.

    Science.gov (United States)

    Pu, Mengjie; Ma, Yongwen; Wan, Jinquan; Wang, Yan; Huang, Mingzhi; Chen, Yangmei

    2014-03-15

    Fe/S doped granular activated carbon (Fe/SGAC) was synthesized with ferric nitrate, Na2S2O3 and (NH4)2S2O8 via an impregnation-precipitation, reduction-oxidation combining with aqueous-phase synthesis method treatment. Surface density of functional groups, surface area changes as well as the chemical state inside Fe/SGAC catalyst were studied by Boehm titration, N2 adsorption and X-ray photoelectron spectroscopy (XPS). The reactivity of the catalysts was tested by degrading Orange G (OG) and diethyl phthalate (DEP). The Fe/SGAC catalysts could significantly enhance the removal rate of OG as compared to persulfate alone and PS/GAC. And the catalytic capacity was also enhanced by S doping. But the degradation of DEP under the similar condition was inhibited by adsorption process because of the different hydrophobicities of OG and DEP molecule. Fe2O3/FeOOH (Fe(3+)) (represents ferrihydrite) together with FeO/Fe3O4 (Fe(2+)) and Fe2O3-satellite, which provide the new active site for persulfate catalyst was found to be the major components of iron element in Fe/SGAC catalyst; the existence of FeS2(S(-)) for sulfur element verified the assumption that the doped S element promoted the electron transfer between the persulfate species and iron oxide at the interface. COD removal experiment further confirmed that mostly contaminant removal was owed to the Fe/SGAC catalytic persulfate oxidation process.

  7. Impact on prevalence of intestinal helminth infection in school children administered with seven annual rounds of diethyl carbamazine (DEC with albendazole

    Directory of Open Access Journals (Sweden)

    I P Sunish

    2015-01-01

    Full Text Available Background & objectives: One third of the world′s population is infected with one or more of the most common soil-transmitted helminths (STH. Albendazole (ALB is being administered with diethyl carbamazine (DEC in filariasis endemic areas to eliminate lymphatic filariasis (LF and helminth infections. In this study, the cumulative impact of seven annual rounds of mass drug administrations (MDA of DEC and ALB on STH infection in school children in selected villages in southern India was determined. Methods: During 2001-2010, seven MDAs were implemented by the Tamil Nadu s0 tate h0 ealth d0 epartment, India. LF and STH infections were monitored in school children from 18 villages of the two treatment arms (viz, DEC alone and DEC+ALB. Kato-Katz cellophane quantitative thick smear technique was employed to estimate STH infections at three weeks, six months and one year post MDA. Results: Prior to treatment, an overall STH prevalence was 60 per cent. After each MDA, infection markedly reduced at three weeks post-treatment in both the arms. The prevalence increased at six months period, which was maintained up to one year. After seven rounds of MDA, the infection reduced from 60.44 to 12.48 per cent in DEC+ALB arm; while the reduction was negligible in DEC alone arm (58.77 to 52.70%. Interpretation & conclusions: Seven rounds of MDA with DEC+ALB reduced the infection load significantly, and further sustained low level of infection for 10 years. However, complete parasite elimination could not be achieved. To curtail STH infection in the community, MDA should be regularized and environmental sanitation measures need to be improved by effective community-based campaigns.

  8. Incongruent nuclear and mitochondrial genetic structure of new world screwworm fly populations due to positive selection of mutations associated with dimethyl- and diethyl-organophosphates resistance.

    Science.gov (United States)

    Bergamo, Luana Walravens; Fresia, Pablo; Azeredo-Espin, Ana Maria L

    2015-01-01

    Livestock production is an important economic activity in Brazil, which has been suffering significant losses due to the impact of parasites. The New World screwworm (NWS) fly, Cochliomyia hominivorax, is an ectoparasite and one of the most important myiasis-causing flies endemic to the Americas. The geographic distribution of NWS has been reduced after the implementation of the Sterile Insect Technique (SIT), being eradicated in North America and part of Central America. In South America, C. hominivorax is controlled by chemical insecticides, although indiscriminate use can cause selection of resistant individuals. Previous studies have associated the Gly137Asp and Trp251Leu mutations in the active site of carboxylesterase E3 to resistance of diethyl and dimethyl-organophosphates insecticides, respectively. Here, we have sequenced a fragment of the carboxylesterase E3 gene (ChαE7), comprising part of intron iII, exon eIII, intron iIII and part of exon eIV, and three mitochondrial gene sequences (CR, COI and COII), of NWS flies from 21 locations in South America. These markers were used for population structure analyses and the ChαE7 gene was also investigated to gain insight into the selective pressures that have shaped its evolution. Analysis of molecular variance (AMOVA) and pairwise FST analysis indicated an increased genetic structure between locations in the ChαE7 compared to the concatenated mitochondrial genes. Discriminant analysis of principal components (DAPC) and spatial analysis of molecular variance (SAMOVA) indicated different degrees of genetic structure for all markers, in agreement with the AMOVA results, but with low correlation to geographic data. The NWS fly is considered a panmitic species based on mitochondrial data, while it is structured into three groups considering the ChαE7 gene. A negative association between the two mutations related to organophosphate resistance and Fay & Wu's H significant negative values for the exons, suggest

  9. A margin of exposure approach to assessment of non-cancerous risk of diethyl phthalate based on human exposure from bottled water consumption.

    Science.gov (United States)

    Zare Jeddi, Maryam; Rastkari, Noushin; Ahmadkhaniha, Reza; Yunesian, Masud; Nabizadeh, Ramin; Daryabeygi, Reza

    2015-12-01

    Phthalates may be present in food due to their widespread presence as environmental contaminants or due to migration from food contact materials. Exposure to phthalates is considered to be potentially harmful to human health as well. Therefore, determining the main source of exposure is an important issue. So, the purpose of this study was (1) to measure the release of diethyl phthalate (DEP) in bottled water consumed in common storage conditions specially low temperature and freezing conditions; (2) to evaluate the intake of DEP from polyethylene terephthalate (PET) bottled water and health risk assessment; and (3) to assess the contribution of the bottled water to the DEP intake against the tolerable daily intake (TDI) values. DEP migration was investigated in six brands of PET-bottled water under different storage conditions room temperature, refrigerator temperature, freezing conditions (40 °C ,0 °C and -18 °C) and outdoor] at various time intervals by magnetic solid extraction (MSPE) using gas chromatography-mass spectroscopy (GC-MS). Eventually, a health risk assessment was conducted and the margin of exposure (MOE) was calculated. The results indicate that contact time with packaging and storage temperatures caused DEP to be released into water from PET bottles. But, when comprising the DEP concentration with initial level, the results demonstrated that the release of phthalates were not substantial in all storage conditions especially at low temperatures (bottled water was much lower than the reference value. However, the lowest MOE was estimated for high water consumers (preschooler > children > lactating women > teenagers > adults > pregnant women), but in all target groups, the MOE was much higher than 1000, thus, low risk is implied. Consequently, PET-bottled water is not a major source of human exposure to DEP and from this perspective is safe for consumption.

  10. Kinetic and thermodynamic study of the reduction of 1,1-diphenylethylene by a thermally frustrated diethyl ether-BCF Lewis pair

    Energy Technology Data Exchange (ETDEWEB)

    Whittemore, Sean M.; Autrey, Thomas

    2015-02-01

    The reaction enthalpy and rate of reduction of 1,1-diphenylethylene (DPE) by the Frustrated Lewis pair formed between tris-pentafluorophenylborane (BCF) and diethyl ether (Et₂O) in dichloromethane have been determined by mixing calorimetry. At 50 °C and 13.6 atm hydrogen a 0.08 M solution of DPE is reduced to 1,1-diphenylethane in the presence of 1 equivalent BCF and 0.8 equivalents Et₂O in 40 minutes. NMR spectroscopy showed >99% conversion to the reduced product. The rate of conversion of the olefin to the alkane as monitored by the time dependent heat flow showed a linear dependence on the free Et₂O and BCF concentration. Integration of the heat flux provides a measure of the reaction enthalpy of ΔH ca. -116±4 kJ/mol for the reaction Ph₂C=CH₂+H2→Ph₂CHCH₃. The equilibrium constant for dative adduct formation, Et₂O+BCF↔Et₂O—BCF, was determined as a function of temperature by ¹⁹F NMR spectroscopy and provided an experimental measure of the enthalpy, ΔH = -54.6±3.3 kJ/mol⁻¹ and entropy, ΔS=-154±13 Jmol⁻¹ K⁻¹, for dative bond formation in DCM. Extrapolation of the van’t Hoff plot to 50 ºC provides Keq that is used to estimate the concentration of free BCF and Et₂O available to activate hydrogen. This work was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Biosciences. Pacific Northwest National Laboratory (PNNL) is a multiprogram national laboratory operated for DOE by Battelle.

  11. Understanding the azeotropic diethyl carbonate-water mixture by structural and energetic characterization of DEC(H2O)(n) heteroclusters.

    Science.gov (United States)

    Ripoll, Juan D; Mejía, Sol M; Mills, Matthew J L; Villa, Aída L

    2015-04-01

    Diethyl carbonate (DEC) is an oxygenated fuel additive. During its synthesis through a promising green process, a DEC-water azeotrope is formed, which decreases DEC production efficiency in the gas phase. Molecular information about this system is scarce but could be of benefit in understanding (and potentially improving) the synthetic process. Therefore, we report a detailed computational study of the conformers of DEC, and their microsolvation with up to four water molecules, with the goal of understanding the observed 1:3 DEC:H2O molar ratio. The most stable DEC conformers (with mutual energy differences < 1.5 kcal mol(-1)) contribute to the energetic and structural properties of the complexes. An exhaustive stochastic exploration of each potential energy surface of DEC-(H2O)n, (where n = 1, 2, 3, 4) heteroclusters discovered 3, 8, 7, and 4 heterodimers, heterotrimers, heterotetramers, and heteropentamers, respectively, at the MP2/6-311++G(d,p) level of theory. DEC conformers and energies of the most stable structures at each heterocluster size were refined using CCSD(T)/6-311++G(d,p). Energy decomposition, electron density topology, and cooperative effects analyses were carried out to determine the relationship between the geometrical features of the heteroclusters and the non-covalent interaction types responsible for their stabilization. Our findings show that electrostatic and exchange energies are responsible for heterocluster stabilization, and also suggest a mutual weakening among hydrogen bonds when more than three water molecules are present. All described results are complementary and suggest a structural and energetic explanation at the molecular level for the experimental molar ratio of 1:3 (DEC:H2O) for the DEC-water azeotrope.

  12. 三氟化硼乙醚配合物电化学合成导电高分子研究进展%Recent Advances in the Electrochemical Polymerization of Inherently Conducting Polymers from Boron Trifluoride Diethyl Etherate and its Mixed Electrolytes

    Institute of Scientific and Technical Information of China (English)

    聂广明; 徐景坤; 张书圣

    2005-01-01

      In the past quarter century, inherently conducting polymers have attracted great attention due to their important academic interest and industrial applications. Electrochemical polymerization has been proved to be one of the most useful approaches for conducting polymer synthesis with several advantages. Boron trifluoride diethyl etherate (BFEE) solution is a middle strong Lewis acid together with good ionic conductivity and good electrocatalytic properties. When BFEE is used as the solvent, no supporting electrolyte is needed. The complexation of aromatic monomers such as thiophene and its derivatives, benzene, pyrrole, furan, fused ring aromatic compounds, with BFEE can significantly lower the anodic oxidation potentials of the monomers, which is beneficial to the preparation of high quality conducting polymers. For this sake, many efforts have been focused on the electrochemical polymerization during the past decade in pure BFEE and its mixed electrolytes with strong acids such as trifluoroacetic acid or concentrated sulfuric acid, diethyl ether, alcohol or acetonitrile. Up to now, a series of high quality inherently conducting polymers have been produced from these media. In this paper, the electrochemical polymerization of high quality conducting polymers prepared from BFEE and its mixed electrolytes were briefly introduced.%  在过去的20多年中,导电高分子因具有重要的学术意义和应用价值受到了广泛关注。电化学方法是制备导电高分子的重要方法。三氟化硼乙醚是一种中等强度的Lewis酸,并具有良好的离子电导率和电催化性能,它可以同时作为溶剂和支持电解质,与噻吩及其衍生物、苯、吡咯、呋喃、稠环芳香化合物等单体相互作用,降低了单体的氧化电位,有利于高性能导电高分子的合成。利用电化学方法在纯三氟化硼乙醚中合成了一系列高性能导电高分子,还开展了在三氟化硼乙醚分别与三

  13. 77 FR 60144 - Importer of Controlled Substances; Notice of Registration; United States Pharmacopeial Convention

    Science.gov (United States)

    2012-10-02

    ..., 77 FR 40911, United States Pharmacopeial Convention, 12601 Twinbrook Parkway, Rockville, Maryland... Methaqualone (2565) I Lysergic acid diethylamide (7315) I Marihuana (7360) I Tetrahydrocannabinols (7370) I...

  14. 78 FR 54913 - Importer of Controlled Substances; Notice of Registration; United States Pharmacopeial Convention

    Science.gov (United States)

    2013-09-06

    ... FR 32457, United States Pharmacopeial Convention, 12601 Twinbrook Parkway, Rockville, Maryland 20852... Methaqualone (2565) I Lysergic acid diethylamide (7315) I Marihuana (7360) I Tetrahydrocannabinols (7370) I...

  15. FSH and LH Secretion from in-vitro Cultured Buffalo Anterior Pituitary Cells Following Treatment with Diethyl-Stilbestrol and Medroxy-Progesterone and Their Effects on Ovarian Activity and Hematological Variables of Female Rabbits

    Directory of Open Access Journals (Sweden)

    Kaleem Iqbal1, Nafees Akhtar1*, Nazir Ahmad1 and Sajjad-ur-Rahman2

    2016-11-01

    Full Text Available Aims of this study were: to investigate whether FSH and LH secretion from in-vitro cultured buffalo adenohypophyseal cells can be increased by supplementing culture media with diethyl-stilbestrol and medroxy-progesterone, respectively; to monitor bioactivity of these in-vitro produced gonadotropins and to see if these gonadotropins have any adverse effects on hematology and internal body organs of female rabbits. Pituitary glands collected from 36 adult buffaloes slaughtered at a local abattoir were used. The anterior pituitary cells were cultured in-vitro using medium RPMI-1640 (code R6504-Sigma enriched with 10% fetal calf serum and GnRH and treated with 0.5 or 1.0 mg/100 ml diethyl-stilbestrol, and 2.5 or 5.0 mg/ml medroxy-progesterone, or left as untreated control. The results showed that FSH and LH concentrations from cultures treated with low or high dose of respective steroids were higher (P<0.05 than those for controls. Treatment of pre-pubertal female rabbits with in-vitro extracted FSH increased serum FSH and LH concentrations, ovarian size and number of developing follicles (GFs on the ovaries compared to controls (P<0.01. However, rabbits treated with in-vitro produced extract of LH showed increased serum FSH and LH, while there was no effect on ovarian size and number of GFs. Moreover, treatment of rabbits with both gonadotropins had no effects on body weight, hematological variables and internal body organs. In conclusion, diethyl-stilbestrol and medroxy-progesterone enhanced the secretion of FSH and LH, respectively, from cultured pituitary cells. Moreover, in-vitro produced FSH increased ovarian size, serum FSH and LH and stimulated ovarian activity, while in-vitro produced LH neither increased ovarian size nor stimulated ovarian activity.

  16. CO气相偶联合成草酸二乙酯反应热力学分析%Thermodynamic analysis of process for CO coupling to diethyl oxalate

    Institute of Scientific and Technical Information of China (English)

    李扬; 胡玉容; 王科

    2011-01-01

    采用Joback基团贡献法推导了亚硝酸乙酯的摩尔定压热容与温度的关系式,并估算了亚硝酸乙酯和碳酸二乙酯的标准摩尔生成吉布斯自由能.综合物性手册中各化合物的热力学函数,计算了CO偶联合成草酸二乙酯反应中主反应和副反应的反应热、反应吉布斯自由能和平衡常数,并对此进行了分析,发现较低的反应温度有利于草酸二乙酯的生成,且主反应自发进行的程度远高于副反应.%The relationship between molar constant heat capacity and temperature of ethyl nitrite was induced by Joback group contribution method, and the standard molar formation Gibbs free energy of ethyl nitrite and diethyl carbonate was also estimated by this method respectively. Reaction enthalpy change, reaction Gibbs free energy change and equilibrium constant of relevant reactions occurred in the process for CO coupling to diethyl oxalate were calculated and analyzed together with basic chemical thermodynamic data obtained from chemistry and engineer handbooks. The result shows that the lower temperature is advantageous to the formation of diethyl oxalate, and the reaction degree of the main reaction is much higher than that of the side reaction.

  17. Spectrophotometric method for the determination of sorbic acid in various food samples with iron(III) and 2-thiobarbituric acid as reagents.

    Science.gov (United States)

    Lau, O W; Luk, S F; Lam, R K

    1989-02-01

    A simple, rapid and accurate spectrophotometric method has been developed for the determination of sorbic acid in various food samples based on the oxidation of sorbic acid by iron(III) at 100 degrees C to malonaldehyde, which then reacts with 2-thiobarbituric acid to form a reddish brown product. The optimum experimental conditions for colour development have been assessed. Absorbance measurements were made at 529 nm in the presence of 0.4% m/V citric acid. The calibration graph was linear for 0-6 micrograms ml-1 of sorbic acid with a slope of 0.131 A micrograms-1 ml. The recoveries of sorbic acid at concentrations of 164-557 micrograms ml-1 ranged from 96 to 103%. The relative standard deviations of ten replicate determinations of sorbic acid in a synthetic cream soda sample spiked with 573 micrograms ml-1 of sorbic acid and in an onion juice sample containing 82 micrograms ml-1 of sorbic acid were 1.6 and 1.9%, respectively. Interferences from several common food additives can be minimised by extracting sorbic acid with diethyl ether and then back-extracting the acid with sodium hydrogen carbonate. The method has been applied successfully to the determination of sorbic acid in a wide range of food samples including beverages, cake, cake mate, garlic bread sprinkle, onion juice, oyster flavoured sauce and grenadine syrup.

  18. Determination of salicylic acid by HPLC in plasma and saliva from children with juvenile chronic arthritis.

    Science.gov (United States)

    Legaz, M E; Acitores, E; Valverde, F

    1992-12-01

    A high performance liquid chromatography (HPLC) method has been developed for measuring salicylic acid in the plasma and saliva of children with juvenile chronic arthritis (JCA). Samples were extracted with diethyl ether and, after drying, redissolved in methanol to be chromatographed. Quantitation of salicylic acid was performed by reverse phase HPLC on a spherisorb ODS-2 column, using methanol: water: acetic acid as mobile phase. Phenolic was monitored by absorbance at 237 nm. Linearity between the amount of mass injected and the response in the detector was determined. This method was applied to compare concentrations of salivary and plasma salicylic acid. The method also permitted the quantitation of salivary salicylate as a non-invasive, indirect method for monitoring the concentration of plasma salicylate in patients with JCA.

  19. Heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C6H14O2 3-Oxaheptan-1-ol (HMSD1111, LB4210_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C6H14O2 3-Oxaheptan-1-ol (HMSD1111, LB4210_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  20. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C8H18O3 3,6,9-Trioxaundecane (VMSD1211, LB4034_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C8H18O3 3,6,9-Trioxaundecane (VMSD1211, LB4034_V)' providing data from direct low-pressure dilatometric measurement of molar excess volume at variable mole fraction and constant temperature.

  1. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1511, LB4522_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1511, LB4522_V)' providing data from direct measurement of low-pressure thermodynamic speed of sound at variable mole fraction and constant temperature, in the single-phase region(s).

  2. Heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C6H14O3 3,6-Dioxaoctan-1-ol (HMSD1111, LB4212_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C6H14O3 3,6-Dioxaoctan-1-ol (HMSD1111, LB4212_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  3. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1212, LB4520_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1212, LB4520_V)' providing data by calculation of molar excess volume from low-pressure density measurements at variable mole fraction and constant temperature.

  4. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C8H18O3 3,6,9-Trioxaundecane (VMSD1112, LB4038_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C8H18O3 3,6,9-Trioxaundecane (VMSD1112, LB4038_V)' providing data by calculation of mass density in the single-phase region(s) from low-pressure dilatometric measurements of the molar excess volume at variable mole fraction and constant temperature.

  5. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C10H22O5 2,5,8,11,14-Pentaoxapentadecane (VMSD1211, LB4863_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C10H22O5 2,5,8,11,14-Pentaoxapentadecane (VMSD1211, LB4863_V)' providing data from direct low-pressure dilatometric measurement of molar excess volume at variable mole fraction and constant temperature.

  6. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1111, LB4521_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C6H12O3 2,4,6-Trimethyl-1,3,5-trioxane (VMSD1111, LB4521_V)' providing data from direct low-pressure measurement of mass density at variable mole fraction and constant temperature, in the single-phase region(s).

  7. Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C10H22O5 2,5,8,11,14-Pentaoxapentadecane (VMSD1112, LB4866_V)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Volumetric Properties of the Mixture Diethyl carbonate C5H10O3 + C10H22O5 2,5,8,11,14-Pentaoxapentadecane (VMSD1112, LB4866_V)' providing data by calculation of mass density in the single-phase region(s) from low-pressure dilatometric measurements of the molar excess volume at variable mole fraction and constant temperature.

  8. Heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C8H18O3 3,6-Dioxadecan-1-ol (HMSD1111, LB4213_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C8H18O3 3,6-Dioxadecan-1-ol (HMSD1111, LB4213_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  9. Heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C5H12O3 3,6-Dioxaheptan-1-ol (HMSD1111, LB4211_H)

    Science.gov (United States)

    Cibulka, I.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume C 'Binary Liquid Systems of Nonelectrolytes III' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'heat of Mixing and Solution of Diethyl carbonate C5H10O3 + C5H12O3 3,6-Dioxaheptan-1-ol (HMSD1111, LB4211_H)' providing data from direct low-pressure calorimetric measurement of molar excess enthalpy at variable mole fraction and constant temperature.

  10. Efficacy of the repellent N,N-diethyl-3-methyl-benzamide (DEET) against tabanid flies on horses evaluated in a field test in Switzerland.

    Science.gov (United States)

    Herholz, C; Kopp, C; Wenger, M; Mathis, A; Wägeli, S; Roth, N

    2016-05-15

    Female tabanid flies (Diptera: Tabanidae) can be a serious nuisance for horses because of their painful bites during blood feeding. They also play a primary role in mechanical transmission of a lentivirus causing Equine Infectious Anemia (EIA), a virus that has spread within Europe in recent years. According to the European law for products intended for use as a repellent on horses (recreational and sport horses), a field test is mandatory to demonstrate sufficient repellency of such a substance against the specific target fly species, but currently no agreed protocols are available for testing of potential repellents. The aim of the present study was to establish a protocol for a field test to investigate the efficacy of N,N-diethyl-3-methyl-benzamide (DEET, Brum®, Huebeli-Stud Horse Care AG) in a 15-17% oil-water emulsion against tabanid flies on horses up to four hours. Between July and August 2015, four horses on three farms each were tested on two consecutive days in a cross-over design. The four horses on Farm A were used in the pre-test as well as in the main test. Two and a half hours after repellent application the horses were lunged until sweating. Tabanid fly infestations were both photographed and directly counted during five minutes 3 and 4h after repellent application on the right side of the horses in the area from the head to the flank, belly and first third of the foreleg. Without repellent application, up to 29 tabanid flies were counted on a horse, whereas the maximum for the repellent treated horses was four. In 50% of the horses treated with DEET there were no Tabanids observed (efficacy 100%), and in all horses the tabanid fly counts were lower than in the control horses with one exemption at 4h. The efficacy of the DEET repellent was at least 80% and 71% respectively, three or four hours after application (with a confidence level of 89%). A fly trap (Horse Pal) revealed the presence of the tabanid species Tabanus brominus and Haematopota

  11. Methotrexate diethyl ester-loaded lipid-core nanocapsules in aqueous solution increased antineoplastic effects in resistant breast cancer cell line

    Directory of Open Access Journals (Sweden)

    Yurgel VC

    2014-03-01

    Full Text Available Virginia C Yurgel,1,* Catiuscia P Oliveira,2,* Karine R Begnini,1 Eduarda Schultze,1 Helena S Thurow,1 Priscila MM Leon,1 Odir A Dellagostin,1 Vinicius F Campos,1 Ruy CR Beck,2 Silvia S Guterres,2 Tiago Collares,1 Adriana R Pohlmann,2–4 Fabiana K Seixas11Programa de Pós-Graduação em Biotecnologia (PPGB, Grupo de Pesquisa em Oncologia Celular e Molecular, Laboratório de Genômica Funcional, Biotecnologia/Centro de Desenvolvimento Tecnológico, Universidade Federal de Pelotas, Pelotas, Rio Grande do Sul, Brazil; 2Programa de Pós-Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul, Brazil; 3Departamento de Química Orgânica, Instituto de Química, Universidade Federal do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul, Brazil; 4Centro de Nanociência e Nanotecnologia, CNANO-UFRGS, Universidade Federal do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul, Brazil*These authors contributed equally to this workAbstract: Breast cancer is the most frequent cancer affecting women. Methotrexate (MTX is an antimetabolic drug that remains important in the treatment of breast cancer. Its efficacy is compromised by resistance in cancer cells that occurs through a variety of mechanisms. This study evaluated apoptotic cell death and cell cycle arrest induced by an MTX derivative (MTX diethyl ester [MTX(OEt2] and MTX(OEt2-loaded lipid-core nanocapsules in two MTX-resistant breast adenocarcinoma cell lines, MCF-7 and MDA-MB-231. The formulations prepared presented adequate granulometric profile. The treatment responses were evaluated through flow cytometry. Relying on the mechanism of resistance, we observed different responses between cell lines. For MCF-7 cells, MTX(OEt2 solution and MTX(OEt2-loaded lipid-core nanocapsules presented significantly higher apoptotic rates than untreated cells and cells incubated with unloaded lipid-core nanocapsules. For MDA-MB-231

  12. Diethyl hexyl phthalate-induced changes in insulin signaling molecules and the protective role of antioxidant vitamins in gastrocnemius muscle of adult male rat

    Energy Technology Data Exchange (ETDEWEB)

    Srinivasan, Chinnapaiyan; Khan, Adam Ismail; Balaji, Venkataraman; Selvaraj, Jayaraman; Balasubramanian, Karundevi, E-mail: kbala82@rediffmail.com

    2011-12-15

    Diethyl hexyl phthalate (DEHP) is an endocrine disruptor, it influences various organ systems in human beings and experimental animals. DEHP reduced the serum testosterone and increased the blood glucose, estradiol, T{sub 3} and T{sub 4} in rats. However, the effect of DEHP on insulin signaling and glucose oxidation in skeletal muscle is not known. Adult male albino rats were divided into four groups: Group I: Control; Groups II and III: DEHP treated (dissolved in olive oil at a dose of 10 and 100 mg/kg body weight, respectively, once daily through gastric intubation for 30 days); and Group IV: DEHP (100 mg/kg body weight) plus vitamins E (50 mg/kg body weight) and C (100 mg/kg body weight) dissolved in olive oil and distilled water, respectively, once daily through gastric intubation for 30 days. On completion of treatment, animals were euthanized and perfused (whole body); gastrocnemius muscle was dissected out and subjected to assessment of various parameters. DEHP treatment increased the H{sub 2}O{sub 2}, hydroxyl radical levels and lipid peroxidation which disrupt the membrane integrity and insulin receptor. DEHP impaired the insulin signal transduction, glucose uptake and oxidation through decreased expression of plasma membrane GLUT4, which may partly be responsible for the elevation of fasting blood glucose level. The present study suggests that DEHP exposure affects glucose oxidation in skeletal muscle and is mediated through enhanced lipid peroxidation, impaired insulin signaling and GLUT4 expression in plasma membrane. Antioxidant vitamins (C and E) have a protective role against the adverse effect of DEHP. -- Highlights: Black-Right-Pointing-Pointer DEHP treatment significantly decreased serum insulin and testosterone levels. Black-Right-Pointing-Pointer Increased ROS and decreased glucose uptake were observed in DEHP treated animals. Black-Right-Pointing-Pointer Impaired insulin signaling in gastrocnemius muscle was observed in DEHP treatment. Black

  13. Observation and Simulation of Transient Anion Oligomers (LiClO4)n(-) (n = 1-4) in Diethyl Carbonate LiClO4 Solutions.

    Science.gov (United States)

    Wang, Furong; Pernot, Pascal; Archirel, Pierre; Schmidhammer, Uli; Ortiz, Daniel; Le Caër, Sophie; Mostafavi, Mehran

    2017-08-10

    NMR measurements show that diethyl carbonate (DEC, a solvent with a low dielectric constant) solutions of LiClO4 contain (LiClO4)n oligomers. The reduction of these species by solvated and presolvated electrons is followed by picosecond pulse radiolysis measurements. The data analysis shows that several anions absorbing in the near-infrared (NIR) and visible range are formed after the 7 ps electron pulse. In contrast with tetrahydrofuran (THF) solutions of LiClO4, the anionic monomer (LiClO4)(-) is not observed in DEC solutions. This is due to the fact that DEC is a nonpolar solvent favoring the clustering of monomers in the nonirradiated solution, as shown by NMR results, and also due to the instability of the anionic monomer. The absorption spectra of the anionic dimer (LiClO4)2(-), trimer (LiClO4)3(-), and tetramer (LiClO4)4(-) are clearly observed in NIR and visible ranges. Compared to the results obtained for the same system in THF and in agreement with simulated absorption spectra, the experimental results show that the absorption bands are shifted to the blue end of the spectrum when n increases. The kinetics recorded for the molar LiClO4 solution indicates that the solute is only in the form of oligomers (LiClO4)n with a large n value and that the reduced species absorb weakly in the visible region. Lastly, and contrary to what is known for well-separated ions in polar solvents, it is shown that the (LiClO4)n(-) anions are not stable with respect to self-reduction, leading to the decomposition of perchlorate anions. In this reaction, the perchlorate anion ClO4(-) is reduced by the Li atom into a chlorate anion ClO3(-). This is proved by the presence of ClO3(-) and chlorinated species detected by mass spectrometry measurements in irradiated DEC solutions containing LiClO4.

  14. Isolation and identification of mosquito (Aedes aegypti ) biting deterrent fatty acids from male inflorescences of breadfruit (Artocarpus altilis (Parkinson) Fosberg).

    Science.gov (United States)

    Jones, A Maxwell P; Klun, Jerome A; Cantrell, Charles L; Ragone, Diane; Chauhan, Kamlesh R; Brown, Paula N; Murch, Susan J

    2012-04-18

    Dried male inflorescences of breadfruit ( Artocarpus altilis , Moraceae) are burned in communities throughout Oceania to repel flying insects, including mosquitoes. This study was conducted to identify chemicals responsible for mosquito deterrence. Various crude extracts were evaluated, and the most active, the hydrodistillate, was used for bioassay-guided fractionation. The hydrodistillate and all fractions displayed significant deterrent activity. Exploratory GC-MS analysis revealed more than 100 distinctive peaks, and more than 30 compounds were putatively identified, including a mixture of terpenes, aldehydes, fatty acids, and aromatics. A systematic bioassay-directed study using adult Aedes aegypti females identified capric, undecanoic, and lauric acid as primary deterrent constituents. A synthetic mixture of fatty acids present in the most active fraction and individual fatty acids were all significantly more active than N,N-diethyl-m-toluamide (DEET). These results provide support for this traditional practice and indicate the potential of male breadfruit flowers and fatty acids as mosquito repellents.

  15. Radiosynthesis of a novel potential adenosine A{sub 3} receptor ligand, 5-ethyl 2,4-diethyl-3-((2-[{sup 18}F]fluoroethyl)sulfanylcarbonyl)-6-phenylpyridine-5-carboxylate ([{sup 18}F]FE rate at SUPPY:2)

    Energy Technology Data Exchange (ETDEWEB)

    Haeusler, D. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Tech. and Biopharmaceutics, Univ. of Vienna (Austria); Mitterhauser, M. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Tech. and Biopharmaceutics, Univ. of Vienna (Austria); Hospital Pharmacy of the General Hospital of Vienna (Austria); Mien, L.K. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Tech. and Biopharmaceutics, Univ. of Vienna (Austria); Dept. of Psychiatry and Psychotherapy, Medical Univ. of Vienna (Austria); Shanab, K.; Spreitzer, H. [Dept. of Drug and Natural Product Synthesis, Univ. of Vienna (Austria); Lanzenberger, R.R [Dept. of Psychiatry and Psychotherapy, Medical Univ. of Vienna (Austria); Schirmer, E. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Drug and Natural Product Synthesis, Univ. of Vienna (Austria); Ungersboeck, J.; Wadsak, W. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Inorganic Chemistry, Univ. of Vienna (Austria); Nics, L. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Nutritional Sciences, Univ. of Vienna (Austria); Viernstein, H. [Dept. of Pharmaceutical Tech. and Biopharmaceutics, Univ. of Vienna (Austria); Dudezak, R.; Kletter, K. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria)

    2009-07-01

    Since, to date very limited information on the distribution and function of the adenosine A{sub 3} receptor is available, the development of suitable radioligands is needed. Recently, we introduced [{sup 18}F]FE rate at SUPPY (5-(2-[{sup 18}F]fluoroethyl) 2,4-diethyl-3-(ethylsulfanylcarbonyl)-6-phenylpyridine-5-carboxylate) as the first PET-ligand for the A3R. Regarding the metabolic profile - this class of dialkylpyridines comprises two ester functions within one molecule, one carboxylic and one thiocarboxylic - one could expect carboxylesterases significantly contributing to cleavage and degradation. Therefore, our aim was the development of [{sup 18}F]FE rate at SUPPY:2 (5-ethyl 2,4-diethyl-3-((2-[{sup 18}F]fluoroethyl)sulfanylcarbonyl)-6-phenylpyridine-5-carboxylate), the functional isomer containing the label at the thiocarboxylic moiety. For satisfactory yields in high scale radiosyntheses, a reaction temperature of 75 C has to be applied for at least 20 min using 20 mg/mL of precursor. So far, 6 complete high-scale radiosyntheses were performed. Starting from an average of 51.2 {+-} 21.8 GBq (mean{+-}SD) [{sup 18}F]fluoride, 5.8 {+-} 4.1 GBq of formulated [{sup 18}F]FE rate at SUPPY:2 (12.0{+-}5.4%, based on [{sup 18}F]fluoride, not corrected for decay) were prepared in 75 {+-} 8 min. (orig.)

  16. Reactive Distillation for Esterification of Bio-based Organic Acids

    Energy Technology Data Exchange (ETDEWEB)

    Fields, Nathan; Miller, Dennis J.; Asthana, Navinchandra S.; Kolah, Aspi K.; Vu, Dung; Lira, Carl T.

    2008-09-23

    The following is the final report of the three year research program to convert organic acids to their ethyl esters using reactive distillation. This report details the complete technical activities of research completed at Michigan State University for the period of October 1, 2003 to September 30, 2006, covering both reactive distillation research and development and the underlying thermodynamic and kinetic data required for successful and rigorous design of reactive distillation esterification processes. Specifically, this project has led to the development of economical, technically viable processes for ethyl lactate, triethyl citrate and diethyl succinate production, and on a larger scale has added to the overall body of knowledge on applying fermentation based organic acids as platform chemicals in the emerging biorefinery. Organic acid esters constitute an attractive class of biorenewable chemicals that are made from corn or other renewable biomass carbohydrate feedstocks and replace analogous petroleum-based compounds, thus lessening U.S. dependence on foreign petroleum and enhancing overall biorefinery viability through production of value-added chemicals in parallel with biofuels production. Further, many of these ester products are candidates for fuel (particularly biodiesel) components, and thus will serve dual roles as both industrial chemicals and fuel enhancers in the emerging bioeconomy. The technical report from MSU is organized around the ethyl esters of four important biorenewables-based acids: lactic acid, citric acid, succinic acid, and propionic acid. Literature background on esterification and reactive distillation has been provided in Section One. Work on lactic acid is covered in Sections Two through Five, citric acid esterification in Sections Six and Seven, succinic acid in Section Eight, and propionic acid in Section Nine. Section Ten covers modeling of ester and organic acid vapor pressure properties using the SPEAD (Step Potential

  17. Occurrence and Determination of Haloacetic Acids in Metro Manila Drinking Water

    Directory of Open Access Journals (Sweden)

    Irene B. Rodriguez

    2009-12-01

    Full Text Available Haloacetic acids are found in chlorinated water with high organic matter content. An analytical method based on a US EPA method for measuring these compounds in water is described. The optimized method used diethyl ether as extraction solvent with sulphuric acid-methanol as esterification agent and subsequent detection by gas chromatography-electron capture detection. Evaluation of this method showed that it was linear in the concentration range of 10 to 150 µg L-1 and the method detection limits were from 17 to 57 µg L-1. Although the method demonstrated low recoveries (16 to 43%, it is useful in the quantitative determination of monochloroacetic acid as well as the qualitative determination of other haloacetic acids in water. Drinking water samples taken from different areas in Metro Manila serviced by the local treatment plants were analysed using the method. Monochloroacetic acid, monobromoacetic acid, and bromochloroacetic acid were detected in these samples. Monochloroacetic acid was quantified and found in concentrations ranging from 19 to 157 µg L-1. In most of the water samples, the concentration of monochloroacetic acid exceeded the US EPA maximum allowable total concentration of 60 µg L-1 for the five haloacetic acids (monochloro-, dichloro-, trichloro-, monobromo-, and dibromoacetic acids in drinking water. This initial study established the occurrence of potentially harmful haloacetic acids in the local drinking water supplies.

  18. 2,4-二甲基吡咯-3,5-二羧酸二乙酯的合成--推荐一个大学有机化学实验%Synthesis of Diethyl 2,4-dimethyl-pyrrole-3,5-dicarboxylate:Recommending a University Organic Chemistry Experiment

    Institute of Scientific and Technical Information of China (English)

    汪剑波; 宗乾收; 沈锦锦; 毕成; 吴晨俊

    2016-01-01

    Using Knorr pyrrole synthesis, diethyl 2,4-dimethyl-pyrrole-3,5-dicarboxylate was synthesized via one-pot method with ethyl acetoacetate and sodium nitrite as starting materials in the presence of acetic acid and zinc powder. The experiment involves the experimental operation and analyses including temperature control, reflux, recrystal ization, melting point, IR and NMR spectroscopies. The advantages of the experiment are simple raw materials and high product yield. The experiment is helpful for cultivating and improving the synthesis ability of students, as wel as in-depth understanding of heterocyclic synthesis and spectral analysis.%采用Knorr吡咯合成法,以乙酰乙酸乙酯和亚硝酸钠为原料,在醋酸和锌粉作用下采用“一锅法”得到2,4-二甲基吡咯-3,5-二羧酸二乙酯。本实验涉及到控温、回流、重结晶、熔点测定、红外光谱及核磁共振等实验操作和分析检测方法。该实验原料简单易得、产物收率高,结合波谱解析方法,可以培养和提高学生合成实验的能力,加强学生对杂环合成和波谱解析的理解与分析。

  19. Elemental and spectroscopic characterization of fractions of an acidic extract of oil sands process water.

    Science.gov (United States)

    Jones, D; Scarlett, A G; West, C E; Frank, R A; Gieleciak, R; Hager, D; Pureveen, J; Tegelaar, E; Rowland, S J

    2013-11-01

    'Naphthenic acids' (NAs) in petroleum produced water and oil sands process water (OSPW), have been implicated in toxicological effects. However, many are not well characterized. A method for fractionation of NAs of an OSPW was used herein and a multi-method characterization of the fractions conducted. The unfractionated OSPW acidic extract was characterized by elemental analysis, electrospray ionization-Orbitrap-mass spectrometry (ESI-MS), and an esterified extract by Fourier Transform infrared (FTIR) and ultraviolet-visible (UV) absorption spectroscopy and by comprehensive multidimensional gas chromatography-MS (GCxGC-MS). Methyl esters were fractionated by argentation solid phase extraction (Ag(+) SPE) and fractions eluting with: hexane; diethyl ether: hexane and diethyl ether, examined. Each was weighed, examined by elemental analysis, FTIR, UV, GC-MS and GCxGC-MS (both nominal and high resolution MS). The ether fraction, containing sulfur, was also examined by GCxGC-sulfur chemiluminescence detection (GCxGC-SCD). The major ions detected by ESI-MS in the OSPW extract were assigned to alicyclic and aromatic 'O2' acids; sulfur was also present. Components recovered by Ag(+) SPE were also methyl esters of alicyclic and aromatic acids; these contained little sulfur or nitrogen. FTIR spectra showed that hydroxy acids and sulfoxides were absent or minor. UV spectra, along with the C/H ratio, further confirmed the aromaticity of the hexane:ether eluate. The more minor ether eluate contained further aromatics and 1.5% sulfur. FTIR spectra indicated free carboxylic acids, in addition to esters. Four major sulfur compounds were detected by GCxGC-SCD. GCxGC-high resolution MS indicated these were methyl esters of C18 S-containing, diaromatics with ≥C3 carboxylic acid side chains. Copyright © 2013 Crown Copyright and Elsevier Ltd. Published by Elsevier Ltd.. All rights reserved.

  20. Alteration of mice L-tryptophan metabolism by the organophosphorous acid triester diazinon.

    Science.gov (United States)

    Seifert, J; Pewnim, T

    1992-12-01

    Diazinon [O,O-diethyl O-(2-isopropyl-6-methyl-4- pyrimidinyl)phosphorothioate] altered the formation of several L-tryptophan metabolites associated with the L-kynurenine pathway in mice. Liver kynurenine formamidase was inhibited almost completely by diazinon (10 mg/kg). The enzyme inhibition resulted in reduced L-kynurenine biosynthesis in livers with a concomitant accumulation of N-formyl-L-kynurenine. In contrast to the liver, plasma L-kynurenine increased up to 5-fold in diazinon-treated mice. Consequently, the urinary excretion of xanthurenic acid and kynurenic acid was raised 5- to 15-fold. The revelation of this novel mechanism of diazinon action is an important piece of information needed for a better understanding of the noncholinergic toxicity of organophosphorous acid triesters and methylcarbamates.

  1. Acidic deposition ("acid rain")

    Science.gov (United States)

    Schreiber, R. Kent; LaRoe, Edward T.; Farris, Gaye S.; Puckett, Catherine E.; Doran, Peter D.; Mac, Michael J.

    1995-01-01

    Acidic deposition, or "acid rain," describes any form of precipitation, including rain, snow, and fog, with a pH of 5.5 or below (Note: pH values below 7 are acidic; vinegar has a pH of 3). It often results when the acidity of normal precipitation is increased by sulfates and nitrates that are emitted into the atmosphere from burning fossil fuels. This form of airborne contamination is considered harmful, both directly and indirectly, to a host of plant and animal species.Although acid rain can fall virtually anywhere, ecological damages in environmentally sensitive areas downwind of industrial and urban emissions are a major concern. This includes areas that have a reduced capacity to neutralize acid inputs because of low alkalinity soils and areas that contain species with a low tolerance to acid conditions. To determine the distribution of acidic deposition and evaluate its biological effects, research and monitoring are being conducted by the federal government with support from states, universities, and private industry.            The national extent of the acid rain problem has been estimated by sampling water from 3,000 lakes and 500 streams (Irving 1991), representing more than 28,000 lakes and 56,000 stream reaches with a total of 200,000 km (125,000 mi). Some particularly sensitive areas, such as the Adirondack Mountain region, have been more intensively sampled and the biota examined in detail for effects from acidity.         To identify trends in aquatic ecosystems, present and historical survey data on water chemistry and associated biota are compared. In lakes, the chemical and biological history and pH trends may be inferred or reconstructed in some cases by examining assemblages of fossil diatoms and aquatic invertebrates in the sediment layers. In terrestrial ecosystems, vegetation damage is surveyed and effects of acidic deposition to plants and animals are determined from laboratory and field exposure experiments. Natural

  2. Catalytic Ethanol Dehydration over Different Acid-activated Montmorillonite Clays.

    Science.gov (United States)

    Krutpijit, Chadaporn; Jongsomjit, Bunjerd

    2016-01-01

    In the present study, the catalytic dehydration of ethanol to obtain ethylene over montmorillonite clays (MMT) with mineral acid activation including H2SO4 (SA-MMT), HCl (HA-MMT) and HNO3 (NA-MMT) was investigated at temperature range of 200 to 400°C. It revealed that HA-MMT exhibited the highest catalytic activity. Ethanol conversion and ethylene selectivity were found to increase with increased reaction temperature. At 400°C, the HA-MMT yielded 82% of ethanol conversion having 78% of ethylene yield. At lower temperature (i.e. 200 to 300°C), diethyl ether (DEE) was a major product. The highest activity obtained from HA-MMT can be attributed to an increase of weak acid sites and acid density by the activation of MMT with HCl. It can be also proven by various characterization techniques that in most case, the main structure of MMT did not alter by acid activation (excepted for NA-MMT). Upon the stability test for 72 h during the reaction, the MMT and HA-MMT showed only slight deactivation due to carbon deposition. Hence, the acid activation of MMT by HCl is promising to enhance the catalytic dehydration of ethanol.

  3. Solvent-free synthesis and oxidative aromatization of diethyl-2,6-dimethyl-4-(1-phenyl-3-aryl-1H-pyrazol-4-yl-1,4-dihydropyridine-3,5-dicarboxylates using hypervalent iodine (III reagents

    Directory of Open Access Journals (Sweden)

    Parvin Kumar

    2014-03-01

    Full Text Available In this article, an efficient, environmentally benign, solvent-free synthesis of diethyl-2,6-dimethyl-4-(1-phenyl-3-aryl-1H-pyrazol-4-yl-1,4-dihydropyridine-3,5-dicarboxylates and their simple oxidative aromatization in presence of selected hypervalent iodine (III reagents under solvent-free condition at room temperature is demonstrated. All reactions were carried out by grinding the reactant pyrazole substituted Hantzch-1,4-dihydropyridines and hypervalent iodine (III reagent in a mortar with pestle. [Hydroxy(tosyloxyiodo]benzene act as an more efficient oxidizing reagent in comparison to phenyliodine bistrifluoroacetate and iodobenzene diacetate in terms of reaction time and yields. The advantages of present protocol are the environment friendly, short reaction time, mild reaction conditions, and high yields of the products.

  4. Development of a MAb-based immunoassay for the simultaneous determination of O,O-diethyl and O,O-dimethyl organophosphorus pesticides in vegetable and fruit samples pretreated with QuEChERS.

    Science.gov (United States)

    Zhao, Fengchun; Hu, Chunyan; Wang, Huimin; Zhao, Longyu; Yang, Zhengyou

    2015-12-01

    To develop a broad-specificity immunoassay for organophosphorus pesticides (OPs), a broad-specificity monoclonal antibody (MAb) for OPs against a generic hapten, O,O-diethyl O-(3-carboxyphenyl) phosphorothioate with the carboxy group in the meta position of the benzene ring, was produced. Eight haptens were prepared and covalently attached to ovalbumin (OVA) for use as coating antigens, and the optimum coating antigen was selected. Then, a sensitive and broadly class selective competitive indirect enzyme-linked immunosorbent assay (ciELISA) based on the MAb and the optimum coating antigen (hapten H-OVA, possessing an O,O-dimethyl generic structure and linked through a linear spacer arm) was developed and optimized. The MAb developed in this study showed quite different cross-reactivity and selectivity compared to previously produced anti-OPs broad-specificity MAbs. Specifically, the MAb showed high and uniform sensitivity to seven O,O-diethyl OPs and six O,O-dimethyl OPs. With the optimum ciELISA, the IC50 values of the 13 OPs were determined as 23.1∼151.2 ng mL(-1). The average IC50 and coefficient of variation (CV) for the IC50 values of the 13 OPs were 74.6 ng mL(-1) and 33.9%, respectively. For the recovery study, a QuEChERS approach based on dispersive solid-phase extraction (d-SPE) was implemented to decrease the matrix effects of vegetable and fruit samples. The recoveries of six representative OPs from the spiked samples ranged from 89.4 to 135.5%; the CV ranged from 3.5 to 15.7%. The ciELISA was also applied to real samples, followed by confirmation with gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. The results demonstrated that the ciELISA is suitable for monitoring OP contamination in vegetable and fruit samples.

  5. Nano-composite polymer gel electrolytes containing ortho-nitro benzoic acid: role of dielectric constant of solvent and fumed silica

    Science.gov (United States)

    Kumar, R.

    2015-03-01

    In this paper, nano-composite polymer gel electrolytes containing polymethylmethacrylate, dimethylacetamide, diethyl carbonate, fumed silica and ortho-nitro benzoic acid have been synthesized. Electrical conductivity, viscosity, pH and thermal behavior of these electrolytes have been studied. The effect of acid, polymer, fumed silica concentration on conductivity, pH and viscosity has been discussed. The effect of dielectric constant of solvent on conductivity behavior of composite polymer gel electrolytes has also been studied. Two maxima in conductivity behavior have been observed with fumed silica concentration for composite polymer gel electrolytes, which have been explained on the basis of double percolation threshold model. Maximum conductivity of 3.20 × 10-4 and 2.46 × 10-6 S/cm at room temperature has been observed for nano-composite polymer gel electrolytes containing 10 wt% polymethylmethacrylate in 1 M solution of o-nitro benzoic acid in dimethylacetamide and diethyl carbonate respectively. The intensity of first maximum observed in conductivity at low concentration of fumed silica has been found to decrease with the decrease in acid concentration for composite polymer gel electrolytes, while the intensity of second maximum at higher fumed silica concentration remains unaffected. The conductivity of composite gels does not show much change in the temperature range of 20-100 °C and also remains constant with time, making them suitable for use as electrolytes in various devices like fuel cells, proton batteries, electrochromic window applications etc.

  6. 碳酸二乙酯吸收CO 2的性能评价%Performance Evaluation of CO2Capture with Diethyl Carbonate

    Institute of Scientific and Technical Information of China (English)

    汤志刚; 李红伟; 贺志敏; 崔敬杰; 郭栋; 赵志军

    2016-01-01

    全球CO 2减排的要求日益严峻,碳捕集成本较高,迫切需要开发高效率、低成本的捕集技术。碳酸二乙酯(DEC)是一种新型高效的CO2吸收溶剂,今采用恒定溶剂法测定282.79~302.69 K下CO2在DEC中的溶解度,并采用Prausnitz-Shair法、分子连接性指数(MCI)和PR状态方程法对其进行了预测;通过与碳酸二甲酯(DMC)的相平衡数据对比,发现相同温度下,DEC的亨利系数小于DMC。采用连续吸收-解吸实验对DEC吸收CO 2效果进行综合评价,通过研究液气比、吸收温度、解吸温度(采用加热解吸)和N 2流量(采用气提解吸)对CO 2吸收率的影响,探索出最佳操作条件;并与DMC的实验结果进行对比,发现采用N 2气提解吸,DEC系统成本明显低于DMC。加热解吸能耗高,气提解吸溶剂损失大,因而探索了一种通过压缩、冷凝进行解吸的新流程,经模拟计算,发现其流程简单,系统成本比加热解吸少,但比气提解吸多;与DMC结果进行对比,发现DEC优于DMC。结果表明,DEC是一种比较有潜力的CO 2吸收溶剂。%CO2 emission reduction is now urgently required as global warming intensifies. However, the high cost of capturing CO2seriously restricts its development. Therefore, it is urgent to develop a high-effective carbon capture technology. Diethyl carbonate (DEC) is a novel CO2absorbent. CO2 solubility in DEC was experimentally determined by the constant volume method at the range of 282.79~302.69 K, at same time which was predicted by Prausnitz-Shair method, Molecular Connectivity Index and Peng-Robinson (PR) equation of state. It is showed that the Henry constants of DEC are smaller than those of DMC at the same temperature by comparison of their phase equilibrium data. The continuous absorption and desorption experimental apparatus and process simulation were applied to study on the performance of DEC capturing CO2. The effects of the liquid

  7. Structural Elucidation of Z- and E- Isomers of 5-Alkyl-4-ethoxycarbonyl-5-(4`-chlorophenyl-3-oxa-4-pentenoic Acids

    Directory of Open Access Journals (Sweden)

    H. M. F. Madkour

    2000-05-01

    Full Text Available Z- and E-isomers of 5-alkyl-4-ethoxycarbonyl-5-(4`-chlorophenyl-3-oxa-4-pentenoic acids were prepared via the condensation of p-chloroacetophenone and/or pchloropropiophenone with diethyl-2,2`-oxydiacetate in the presence of sodium hydride as a basic catalyst. The Z-isomers of 2a and 2b were found to be predominant. The behaviour of the corresponding anhydrides towards the action of hydrazine, phenylhydrazine, primary aromatic amines, hydrocarbons and ethanolysis has also been investigated. The structures and configurations of the products have been elucidated by chemical and spectroscopic means.

  8. Apoptotic activity of the marine diatom Cocconeis scutellum and eicosapentaenoic acid in BT20 cells.

    Science.gov (United States)

    Nappo, Michela; Berkov, Strahil; Massucco, Carlotta; Di Maria, Valentina; Bastida, Jaume; Codina, Carles; Avila, Conxita; Messina, Patrizia; Zupo, Valerio; Zupo, Simona

    2012-04-01

    The marine diatoms Cocconeis scutellum Ehrenberg (Bacillariophyceae) are known to trigger apoptosis in the androgenic gland of the Mediterranean crustacean Hippolyte inermis Leach (Decapoda), affecting the shrimp's sex reversal. The aim of this study was to evaluate a possible apoptotic effect of extracts and fractions from these microalgae also on human tissues. The chemical profile of C. scutellum was determined by gas chromatography-mass spectrometry (GC-MS) and, afterwards, organic extracts and fractions from the diatoms were used to treat to breast cancer BT20 cells. Double labeling with annexin V-FITC and isotonic propidium iodide (PI) along with flow cytometry analysis enabled the evaluate of cell apoptosis and viability, whereas hypotonic PI staining was used to analyze the cell cycle in BT20 lines. The involvement of specific caspases was studied by Western blotting. Results demonstrated that the diethyl ether extract and, in particular, fraction 3, the richest fraction in eicosapentaenoic acid (EPA) from the diethyl ether extract, selectively induced apoptosis (up to 89.2% at 1 μg/well of fraction 3) and decreased viability in BT20 cells. The apoptotic effect was displayed in a concentration and time-dependent manner, by activating caspases-8 and 3, and arresting the progression of the cell cycle from S to G2-M phase. EPA alone showed similar apoptotic effects in BT20 cells. The study demonstrates the apoptotic activity of C. scutellum diatoms on breast cancer cells and suggests their potential use as a source of apoptotic compounds.

  9. Improved synthesis of glycine, taurine and sulfate conjugated bile acids as reference compounds and internal standards for ESI-MS/MS urinary profiling of inborn errors of bile acid synthesis.

    Science.gov (United States)

    Donazzolo, Elena; Gucciardi, Antonina; Mazzier, Daniela; Peggion, Cristina; Pirillo, Paola; Naturale, Mauro; Moretto, Alessandro; Giordano, Giuseppe

    2017-04-01

    Bile acid synthesis defects are rare genetic disorders characterized by a failure to produce normal bile acids (BAs), and by an accumulation of unusual and intermediary cholanoids. Measurements of cholanoids in urine samples by mass spectrometry are a gold standard for the diagnosis of these diseases. In this work improved methods for the chemical synthesis of 30 BAs conjugated with glycine, taurine and sulfate were developed. Diethyl phosphorocyanidate (DEPC) and diphenyl phosphoryl azide (DPPA) were used as coupling reagents for glycine and taurine conjugation. Sulfated BAs were obtained by sulfur trioxide-triethylamine complex (SO3-TEA) as sulfating agent and thereafter conjugated with glycine and taurine. All products were characterized by NMR, IR spectroscopy and high resolution mass spectrometry (HRMS). The use of these compounds as internal standards allows an improved accuracy of both identification and quantification of urinary bile acids. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Stereodivergent Mannich reaction of bis(trimethylsilyl)ketene acetals with N-tert-butanesulfinyl imines by Lewis acid or Lewis base activation, a one-pot protocol to obtain chiral β-amino acids.

    Science.gov (United States)

    Cantú-Reyes, Margarita; Alvarado-Beltrán, Isabel; Ballinas-Indilí, Ricardo; Álvarez-Toledano, Cecilio; Hernández-Rodríguez, Marcos

    2017-09-20

    We report a one-pot synthesis of chiral β(2,2,3)-amino acids by the Mannich addition of bistrimethylsilyl ketene acetals to N-tert-butanesulfinyl imines followed by the removal of the chiral auxiliary. The synthesis and isolation of pure β-amino acid hydrochlorides were conducted under mild conditions, without strong bases and this method is operationally simple. The stereoselective reaction was promoted by two different activation methods that lead to different stereoisomers: (1) Lewis Acid (LA) catalysis with boron trifluoride diethyl etherate and (2) Lewis Base (LB) catalysis with tetrabutylammonium difluorotriphenylsilicate. The reaction presented good diastereoselectivity with LB activation and moderate to good dr with LA catalysis. The exceptions in both protocols were imines with electron donating groups in the aromatic ring.

  11. Synthesis of 3a,12a-dihydroxy-23a,23b-dihomo-5b-cholan-24-oic acid

    Directory of Open Access Journals (Sweden)

    SLAVKO KEVRESAN

    2004-05-01

    Full Text Available A novel multi-step synthesis of 3a,12a-dihydroxy-23a,23b-dihomo-5b-cholan-24-oic acid (23a,23b-dihomodeoxycholic acid (5 has been achieved from methyl 3a,12a-dihydroxy-5b-cholanoate (1. Reduction of compound 1 with LiAlH4 in dry ether gave the corresponding alcohol 2 in 83 % yield. Selective esterification of compound 2 with tosyl chloride in dry piridine at 0–5 ºC for 12 h afforded the 3a,12a-dihydroxy-5b-24-cholanyl tosylate (3 in 64 % yield. The reaction of the tosyl derivative 3 with sodium diethyl malonate gave compound 4 which was first subjected to hydrolysis under basic conditions, followed by decarboxylation under acidic conditions to afford 3a,12a-dihydroxy-5b-23a,23b-dihomocholan-24-oic acid in 84 % yield.

  12. Isolation and estimation of the 'aromatic' naphthenic acid content of an oil sands process-affected water extract.

    Science.gov (United States)

    Jones, David; West, Charles E; Scarlett, Alan G; Frank, Richard A; Rowland, Steven J

    2012-07-20

    The naphthenic acids of oil sands process-affected water (OSPW) are said to be important toxicants. The major acids are stated to have alicyclic structures and recently, numerous of these have been identified, but some evidence suggests 'aromatic' acids are also present. The proportions of such acids have not been reported because they exist in so-called supercomplex mixtures with the alicyclic species. Their contribution to the toxicity of OSPW, if any, is therefore unknown. Here we report the use of multidimensional comprehensive gas chromatography-mass spectrometry (GC×GC-MS) with polar first dimension and non-polar second dimension GC columns and argentation solid phase extraction, to separate methyl esters of the acids of an OSPW supercomplex, into distinct fractions. A major fraction (ca 70%) was shown to contain acids (methyl esters) previously identified as alicyclic species. Authentic adamantane acid methyl esters were shown to chromatograph in this fraction. This fraction was isolated by argentation solid phase extraction (SPE) by elution with hexane. GC-MS and GC×GC-MS confirmed this to be the major fraction in the original supercomplex containing alicyclic acids (methyl esters). A second fraction shown to contain monoaromatic acids (methyl esters) by GC×GC-MS was unexpectedly abundant (ca 30% relative to the acyclic acids). The naphtheno-aromatic dehydroabietic acid was confirmed by co-injection with an authentic compound and several acids previously tentatively identified as naphtheno-monoaromatics were present. This fraction was isolated by argentation SPE by elution with more polar 5% diethyl ether in hexane. GC-MS and GC×GC-MS confirmed that the fraction represented a significant proportion of the original supercomplex. A further fraction, eluting from the argentation SPE column with more 5% diethyl ether in hexane in the same retention volume as authentic methyl naphthoate, contained, in addition to some of the second fraction, a third, much

  13. O-H...O versus O-H...S hydrogen bonding. 3. IR-UV double resonance study of hydrogen bonded complexes of p-cresol with diethyl ether and its sulfur analog.

    Science.gov (United States)

    Biswal, Himansu S; Wategaonkar, Sanjay

    2010-05-20

    In this work the hydrogen bonded complexes of diethyl ether (DEE) and diethyl sulfide (DES) with p-cresol (p-CR) were investigated. Only one conformer of the p-CR.DEE complex and three conformers of the p-CR.DES complex were found to be present under the supersonic jet expansion conditions. The conformational assignments were done with the help of IR-UV double resonance studies and ab initio calculations. The red shifts in the OH stretching frequency for the O-H...O and O-H...S hydrogen bonded complexes were quite close to each other. In fact, one of the p-CR.DES conformers showed a slightly larger red shift in the OH stretch than that in the p-CR.DEE conformer, which suggests that in this case sulfur is not a weak hydrogen bond acceptor as noted previously in case of the p-CR.H(2)O and p-CR.H(2)S complexes (Biswal et al. J. Phys. Chem. A 2009, 113, 5633). The natural bond orbital analysis also shows that the extent of overlap between sulfur lone pair orbitals (LP) and OH antibonding orbital (sigma*(OH)) was comparable to the oxygen (LP) and sigma*(OH) overlap, consistent with the similar magnitudes of the red shifts of OH stretch in the DES and DEE complexes. The computed binding energy of the p-CR.DES complex, however, was about 80% of the p-CR.DEE complex. The electron densities at the bond critical points indicated that the O-H...S interaction was weaker than the O-H...O interaction in this particular system also. The important finding of this study was that the IR red shifts in the H-bond donor X-H stretching frequency were not quite consistent with the computed binding energies and the atoms-in-molecules analysis contrary to the general understanding. Energy decomposition analysis suggests that O-H...S hydrogen bonding interaction is dispersive in nature and the dispersion contribution decreases with the increase in the length of the alkyl chain of the "S" hydrogen bond acceptor.

  14. Carbonyl{3,3′-di-tert-butyl-5,5′-dimethoxy-2,2′-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yloxy]biphenyl-κ2P,P′}hydrido(triphenylphosphane-κPrhodium(I diethyl ether trisolvate

    Directory of Open Access Journals (Sweden)

    Detlef Selent

    2013-01-01

    Full Text Available In the title compound, [RhH(C74H68O8P2(C18H15P(CO]·3C4H10O, the CHP3 coordination set at the RhI ion is arranged in a distorted trigonal–bipyramidal geometry with the P atoms adopting equatorial coordination sites and the C atom of the carbonyl ligand as well as the H atom adopting the axial sites. The asymmetric unit contains two very similar molecules of the rhodium complex, two half-occupied diethyl ether molecules and further diethyl ether solvent molecules which could not be modelled successfully. Therefore contributions of the latter were removed from the diffraction data using the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  15. 液相氧化羰基化合成碳酸二乙酯的新型催化体系CuCl/1,10-菲罗啉/N-甲基咪唑%A Novel Catalyst CuCl/1,10-Phenanthroline/N-Methylimidazole for the Oxidative Carbonylation of Ethanol to Diethyl Carbonate

    Institute of Scientific and Technical Information of China (English)

    莫婉玲; 李光兴; 朱永强; 熊辉; 梅付名

    2003-01-01

    @@ Diethyl carbonate (DEC) is one of the important green chemicals widely used for organic synthesis because of its various functional groups. DEC is a better octane blending fuel, and has more oxygen in the molecule than methyl tert-butyl ether (MTBE), 40.6% versus 18.2%, which reduces emissions from gasoline and diesel engine. For these reasons many studies on the production of DEC have been extensively carried out.

  16. Synthesis of 2-Carbethoxy-3-(2-thienyl)propanoic acid%(2-噻吩基甲基)丙二酸单甲酯的合成

    Institute of Scientific and Technical Information of China (English)

    曾海霞; 赵煜松

    2012-01-01

    2-Carbethoxy-3-(2-thienyl)propanoic acid is a key intermediate of Eprosartan.It was prepared with 2-thiophene- aldehyde, diethyl malonate as the main materials, through the addition, elimination and hydrolysis reaction.%(2-噻吩基甲基)丙二酸单甲酯为合成依普罗沙坦的关键中间体,以2-噻吩甲醛、丙二酸二乙酯为主要原料,通过加成、消除、水解反应制备而得。

  17. Poly(lactic acid/thermoplastic starch sheets: effect of adipate esters on the morphological, mechanical and barrier properties

    Directory of Open Access Journals (Sweden)

    Marianne Ayumi Shirai

    2016-02-01

    Full Text Available Abstract Blends of poly(lactic acid (PLA and thermoplastic starch (TPS plasticized with adipate esters (diisodecyl adipate and diethyl adipate having different molecular weight were used to produce sheets. The calendering-extrusion process at a pilot scale was used, and the mechanical, barrier, and morphological characterization of the obtained materials were performed. The increase in the TPS content affected the mechanical properties of the sheets by increasing the elongation and decreasing the rigidity. TPS conferred a more hydrophilic character to the sheets, as observed from the water vapor permeability results. The sheets plasticized with diisodecyl adipate (DIA, having a higher molecular weight, had better mechanical and barrier properties than diethyl adipate (DEA plasticized sheets, indicating that DIA was more effective as plasticizer. Micrographs obtained by confocal laser microscopy and scanning electron microscopy showed different morphologies when different proportions of PLA and TPS were used (dispersed or co-continuous structures, which were strongly associated with the mechanical and barrier properties.

  18. Bis[μ-1,3-bis­(di­phenyl­phosphan­yl)propane-κ2 P:P′]digold(I) tetra­chloridonickelate(II) diethyl ether monosolvate

    Science.gov (United States)

    Igashira-Kamiyama, Asako; Itai, Takuma; Arai, Yuka; Konno, Takumi

    2013-01-01

    The title compound, [Au2(C27H26P2)2][NiCl4]·C4H10O, consists of a digold(I) complex cation, an [NiCl4]2− complex anion and a diethyl ether solvent mol­ecule. Two 1,3-bis­(di­phenyl­phosphan­yl)propane (dppp) ligands bridge two AuI atoms, forming a metallacycle in which each of the AuI atoms is coordinated in a slightly distorted linear environment by two P atoms. In the complex anion, the NiII atom is coordinated by four chloride ligands in a distorted tetra­hedral geometry. The complex cation and the complex anion form a cation–anion pair through two Au⋯Cl contacts of 3.040 (1) and 3.021 (2) Å. One of the phenyl groups of the dppp ligand is disordered over two positions with equal occupancies. PMID:23794999

  19. Low dose genotoxicity of 4-bromo-n,n-diethyl-5,5- dimethyl-2,5-dihydro-1,2-oxaphosphol-2-amine 2-oxide in mice bone marrow cells and Allium cepa L. root tip cells

    Directory of Open Access Journals (Sweden)

    Kalcheva Vanya

    2009-01-01

    Full Text Available The chemistry of organophosphorus compounds is a subject of increasing interest and different new compounds have been synthesized. There are data that some known organophosphates are mutagens. Oxaphosphole derivatives possess biological activity and might influence proliferating cells. Bioassays are currently used in ecotoxicology to investigate the effects and mechanisms of action of new chemicals. To provide a broad coverage of the mutagenic potential of a chemical, information on different experimental test-systems is required. Genotoxicity assays are usually performed at high doses, but humans are exposed to most environmental chemicals at low doses. The objective of this study was to determine the genotoxicity of low doses (2.82x10-6 µg/kg and 2.82x10-9 µg/kg, corresponding to concentrations 10-12M and 10-15M of 4-bromo-N,N-diethyl- 5,5-dimethyl-2,5-dihydro-1,2-oxaphosphol-2-amine 2-oxide (Br-oxph in ICR mice bone marrow cells and Allium cepa L. root tip cells. Treatment with Br-oxph for 3 h produced alterations in the mitotic index in Allium cepa cells and induced chromosome aberrations in both test systems. These effects remained 48 h after the treatment. The data from the study showed the existence of cytotoxic and genotoxic effects of Br-oxph at tested doses.

  20. Synthesis and electroluminescent properties of blue fluorescent materials based on 9,9-diethyl-N,N-diphenyl-9 H-fluoren-2-amine substituted anthracene derivatives for organic light-emitting diodes

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Seul Bee; Kim, Chanwoo; Park, Soo Na; Kim, Young Seok [Department of Chemistry, Sungkyunkwan University, Suwon, 440-746 (Korea, Republic of); Lee, Ho Won [Department of Information Display, Hongik University, Seoul, 121-791 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@hongik.ac.kr [Department of Information Display, Hongik University, Seoul, 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon, 440-746 (Korea, Republic of)

    2015-11-30

    Four 9,9-diethyl-N,N-diphenyl-9 H-fluoren-2-amine substituted anthracene derivatives have been designed and synthesized by Suzuki cross coupling reactions. To explore the electroluminescent properties of these blue materials, multilayer blue organic light-emitting diodes were fabricated in the following device structure: indium tin oxide (180 nm)/N,N’-diphenyl-N,N’-(1-napthyl)-(1,1′-phenyl)-4,4′-diamine (50 nm)/blue emitting materials (1–4) (30 nm)/bathophenanthroline (30 nm)/lithium quinolate (2 nm)/Al (100 nm). All devices appeared excellent deep-blue emissions. Among them, a device exhibited a maximum luminance of 5686 cd/m{sup 2}, the luminous, power and external quantum efficiencies of 5.11 cd/A, 3.79 lm/W, and 4.06% with the Commission International de L'Eclairage coordinates of (0.15, 0.15) at 500 cd/m{sup 2}, respectively. - Highlights: • We synthesized blue fluorescent materials based on anthracene derivatives. • The EL efficiencies of these materials depend on the quantum yields in solid states. • These materials have great potential for applications as blue emitter in OLEDs.

  1. 草酸二乙酯加氢制乙二醇产品精馏试验研究%Preparation of ethylene glycol with hydrogenation of diethyl oxalate by vacuum distillation

    Institute of Scientific and Technical Information of China (English)

    范鑫; 王科; 袁小金; 许红云; 李扬; 胡玉容

    2011-01-01

    The fraction of ethylene glycol is enriched from crude glycol by vacuum batch distillation. The crude glycol is prepared by the hydrogenation of diethyl oxalate. The experiment show that this separation method is feasible and ethylene glycol with purity of more than 99. 8% is obtained. Furthermore the effects of tower top pressure,reflux ratio on product purity are analyzed. The optimal operating condition is determined in the experimental condition.%通过减压间歇精馏对草酸二乙酯加氢制乙二醇产品进行精制.试验表明该方法切实可行,获得了纯度≥99.8%的乙二醇产品;同时探讨了塔顶压强、回流比变化对产品纯度的影响,获得了试验条件下的最佳操作条件,为工业化提纯草酸二乙酯加氢制乙二醇产品提供了有益信息.

  2. Radiosynthesis of the adenosine A{sub 3} receptor ligand 5-(2-[{sup 18}F]fluoroethyl) 2,4-diethyl-3-(ethylsulfanylcarbonyl)-6-phenylpyridine-5-carboxylate ([{sup 18}F]FE rate at SUPPY)

    Energy Technology Data Exchange (ETDEWEB)

    Wadsak, W. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Inorganic Chemistry, Univ. of Vienna (Austria); Mien, L.K. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Technology and Biopharmaceutics, Univ. of Vienna (Austria); Dept. of Psychiatry and Psychotherapy, Medical Univ. of Vienna (Austria); Shanab, K.; Spreitzer, H. [Dept. of Psychiatry and Psychotherapy, Medical Univ. of Vienna (Austria); Weber, K.; Schmidt, B.; Haeusler, D. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Technology and Biopharmaceutics, Univ. of Vienna (Austria); Sindelar, K.M.; Ettlinger, D.E.; Dudczak, R.; Kletter, K. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Keppler, B.K.; Viernstein, H. [Dept. of Inorganic Chemistry, Univ. of Vienna (Austria); Mitterhauser, M. [Dept. of Nuclear Medicine, Medical Univ. of Vienna (Austria); Dept. of Pharmaceutical Technology and Biopharmaceutics, Univ. of Vienna (Austria); Hospital Pharmacy of the General Hospital of Vienna (Austria)

    2008-07-01

    Since to date very limited information on the distribution and function of the adenosine A{sub 3} receptor is available, the development of a suitable radioligand is needed. Such a selective radioligand can then be used for quantitative autoradiography, preclinical studies in animals and subsequent human PET applications. Recently, a promising candidate compound, 5-(2-fluoroethyl) 2,4-diethyl-3-(ethylsulfanylcarbonyl)-6-phenylpyridine-5-carboxylate (FE rate at SUPPY), has been presented. The successful preparation of a suitable labelling precursor and the evaluation and optimization of the radiosynthesis of [{sup 18}F]FE rate at SUPPY is presented herewith. For satisfactory yields, a reaction temperature of 75 C has to be applied for at least 20 min using 8-10 mg of precursor. Until now, 15 complete high-scale radiosyntheses were performed. Starting from an average of 51 {+-} 12 GBq (average {+-}SD; range: 30-67 GBq) [{sup 18}F]fluoride, 9.4 {+-} 3.6 GBq of formulated [{sup 18}F]FE rate at SUPPY (32.3 {+-} 12.4%, based on [{sup 18}F]fluoride, corrected for decay) were prepared in < 105 min. (orig.)

  3. Bis(μ-2-tert-butylphenylimido-1:2κ2N:Nchlorido-2κCl-(diethyl ether-1κO(2η5-pentamethylcyclopentadienyllithiumtantalum(V

    Directory of Open Access Journals (Sweden)

    Jacqueline M. Cole

    2011-06-01

    Full Text Available In the title compound, [LiTa(C10H15(C10H13N2Cl(C4H10O], the TaV atom is coordinated by a η5-pentamethylcyclopentadienyl (Cp* ligand, a chloride ion and two N-bonded 2-tert-butylphenylimide dianions. With respect to the two N atoms, the chloride ion and the centroid of the Cp* ring, the tantalum coordination geometry is approximately tetrahedral. The lithium cation is bonded to both the 2-tert-butylphenylimide dianions and also a diethyl ether molecule, in an approximate trigonal planar arrangement. The Ta...Li separation is 2.681 (15 Å. In the crystal, a weak C—H...Cl interaction links the molecules. When compared to the 2,6-diisopropylphenylimide analogue (`the Wigley derivative' of the title compound, the two structures are conformationally matched with an overall r.m.s. difference of 0.461Å.

  4. Apparent shortening of the Csp(3)-Csp(3)bond analysed via a variable-temperature X-ray diffraction study in racemic 1,1'-binaphthalene-2,2'-diyl diethyl bis(carbonate).

    Science.gov (United States)

    Nayak, Susanta K; Chandrasekhar, S; Guru Row, T N

    2009-05-01

    Crystal structure determination at room temperature [292 (2) K] of racemic 1,1'-binaphthalene-2,2'-diyl diethyl bis(carbonate), C(26)H(22)O(6), showed that one of the terminal carbon-carbon bond lengths is very short [Csp(3)-Csp(3) = 1.327 (6) A]. The reason for such a short bond length has been analysed by collecting data sets on the same crystal at 393, 150 and 90 K. The values of the corrected bond lengths clearly suggest that the shortening is mainly due to positional disorder at two sites, with minor perturbations arising as a result of thermal vibrations. The positional disorder has been resolved in the analysis of the 90 K data following the changes in the unit-cell parameters for the data sets at 150 and 90 K, which appear to be an artifact of a near centre of symmetry relationship between the two independent molecules in the space group P1 at these temperatures. Indeed, the unit cell at low temperature (150 and 90 K) is a supercell of the room-temperature unit cell.

  5. Synthesis of New Fluorine Substituted Heterocyclic Nitrogen Systems Derived from p-Aminosalicylic Acid as Antimycobacterial Agents

    Directory of Open Access Journals (Sweden)

    Mohammed Saleh I. T. Makki

    2013-01-01

    Full Text Available Some new fluorine substituted heterocyclic nitrogen systems 2–17 have been synthesized from ring closure reactions of substituted p-amino salicylic acids (PAS. The Schiffs base of PAS was cyclized with chloroacetyl chloride and mercaptoacetic acid to give azetidinone 2, thiazolidinone 3, and spiro-fluoroindolothiazoline-dione 10. However, PAS when reacted directly with 4-fluorobenzoyl chloride and 5-oxazolinone yielded derivatives 4, 5, and 7. Aminomethylation of PAS using formaldehyde and piperidine or piperazine formed N-alkyl and N,N′-dialkyl derivatives (11 and 12 respectively upon fluorinated benzoylation gave compounds 13 and 14. Similarly, treatment of PAS with thiosemicarbazide 15 and subsequent cyclization with diethyl oxalate yielded the fluorinated heterocycle 17. The structures of the fluorinated heterocyclic systems have been established on the basis of elemental analysis, 1H NMR, 13C NMR, and MS spectral data. Some of the targets exhibited a high inhibition towards Mycobacterium strain with favorable log P values.

  6. Valproic Acid

    Science.gov (United States)

    ... acid is in a class of medications called anticonvulsants. It works by increasing the amount of a ... older (about 1 in 500 people) who took anticonvulsants such as valproic acid to treat various conditions ...

  7. Amino acids

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/002222.htm Amino acids To use the sharing features on this page, please enable JavaScript. Amino acids are organic compounds that combine to form proteins . ...

  8. Obeticholic Acid

    Science.gov (United States)

    Obeticholic acid is used alone or in combination with ursodiol (Actigall, Urso) to treat primary biliary cholangitis (PBC; a ... were not treated successfully with ursodiol alone. Obeticholic acid is in a class of medications called farnesoid ...

  9. Ascorbic Acid

    Science.gov (United States)

    Ascorbic acid is used to prevent and treat scurvy, a disease caused by a lack of vitamin C in ... Ascorbic acid comes in extended-release (long-acting) capsules and tablets, lozenges, syrup, chewable tablets, and liquid drops to ...

  10. Mefenamic Acid

    Science.gov (United States)

    Mefenamic acid is used to relieve mild to moderate pain, including menstrual pain (pain that happens before or during a menstrual period). Mefenamic acid is in a class of medications called NSAIDs. ...

  11. Acid mucopolysaccharides

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003368.htm Acid mucopolysaccharides To use the sharing features on this page, please enable JavaScript. Acid mucopolysaccharides is a test that measures the amount ...

  12. Ethacrynic Acid

    Science.gov (United States)

    Ethacrynic acid, a 'water pill,' is used to treat swelling and fluid retention caused by various medical problems. It ... Ethacrynic acid comes as a tablet to take by mouth. It is usually taken once or twice a day ...

  13. Aminocaproic Acid

    Science.gov (United States)

    Aminocaproic acid is used to control bleeding that occurs when blood clots are broken down too quickly. This type ... the baby is ready to be born). Aminocaproic acid is also used to control bleeding in the ...

  14. Aspartic acid

    Science.gov (United States)

    ... body work. It plays a role in: Hormone production and release Normal nervous system function Plant sources of aspartic acid include: avocado, asparagus, and molasses. Animal sources of aspartic acid include: ...

  15. Correlation between arachidonic acid oxygenation and luminol-induced chemiluminescence in neutrophils: inhibition by diethyldithiocarbamate.

    Science.gov (United States)

    Chabannes, B; Perraut, C; El Habib, R; Moliere, P; Pacheco, Y; Lagarde, M

    1997-04-01

    Neutrophils from allergic subjects were hypersensitive to stimulation by low calcium ionophore concentration (0.15 microM), resulting in an increased formation of leukotriene B4 (LTB4), 5S-hydroxy-6,8,11,14-(E,Z,Z,Z)-eicosatetraenoic acid (5-HETE), and other arachidonic acid metabolites through the 5-lipoxygenase pathway. In parallel, luminol-dependent chemiluminescence was also higher in neutrophils from allergic patients at the basal state and after stimulation by calcium ionophore, revealing an enhancement of radical oxygen species and peroxide production. The activity of glutathione peroxidase, the main enzyme responsible for hydroperoxide reduction, was lowered in these cells. Diethyl-dithiocarbamate (DTC) induced a concentration-dependent decrease in chemiluminescence and arachidonic acid metabolism after neutrophil stimulation. These data show that the elevation of arachidonic acid metabolism in neutrophils from allergic patients is strongly correlated with oxidative status. This elevation may be the consequence of an increased cellular hydroperoxide known to activate 5-lipoxygenase (5-LOX) activity and/or an increased arachidonic acid availability, due either to phospholipase A2 (PLA2) activation or inhibition of arachidonate reesterification into phospholipids. Lowering this oxidative status was associated with a concomitant decrease of this metabolism. Our results suggest that the effect of DTC may be the consequence of an inhibition of peroxyl radical and cellular lipid hydroperoxide production. Thus, DTC may modulate arachidonic acid metabolism in neutrophils by modulating the cellular hydroperoxide level.

  16. A novel approach for the preparation of nanocrystalline cellulose by using phosphotungstic acid.

    Science.gov (United States)

    Liu, Yefei; Wang, Haisong; Yu, Guang; Yu, Qingxue; Li, Bin; Mu, Xindong

    2014-09-22

    In this work, a sustainable and green process to prepare nanocrystalline cellulose (NCC) from bleached hardwood pulp was demonstrated. Rod-like nanocrystalline cellulose with the size of 15-40 nm in width and hundreds of nanometers in length was obtained through H3PW12O40 (HPW)-catalyzed hydrolysis of bleached pulp fibers under the mild reaction conditions. Thermogravimetric analysis revealed that the resulting NCC exhibited much higher thermal stability than the partially sulfated NCC (prepared by sulfuric acid). In addition, the concentrated HPW could be easily recovered and recycled through the extraction with diethyl ether, and the recovered HPW could be reused for several rounds of cellulose hydrolysis without activity lost. These fundamental studies are of crucial importance for the development and application of NCC products/NCC-based biomaterials with good thermal stability.

  17. Synthesis of diethyl malonate over phosphotungstic acid supported on activated carbon%活性炭负载磷钨酸催化合成丙二酸二乙酯的研究

    Institute of Scientific and Technical Information of China (English)

    王升文; 李继忠

    2007-01-01

    以丙二酸和乙醇为原料,采用活性炭负载磷钨酸作催化剂合成丙二酸二乙酯.考察了催化剂用量、酸醇物质的量比、带水剂用量以及反应时间等因素对收率的影响.确定最佳酯化反应条件:n(丙二酸):n(乙醇):n(催化剂)=1:3:0.007,带水剂甲苯15 mL,反应时间90 min.收率可达96.25%.

  18. Fatty acids - trans fatty acids

    Science.gov (United States)

    The data supporting a negative effect of dietary trans fatty acids on cardiovascular disease risk is consistent. The primary dietary sources of trans fatty acids include partially hydrogenated fat and rudiment fat. The adverse effect of trans fatty acids on plasma lipoprotein profiles is consisten...

  19. GC/Mass analysis of the volatile compounds of P. hyrcanicum diethyl ether extract and GC profiling of some Iranian Polygonum species

    Directory of Open Access Journals (Sweden)

    S. Saeidnia

    2014-01-01

    Full Text Available In this study, the relationship among four species of Polygonum (including P. hyrcanicum (three samples, P. persicaria, P. avicular, and P. hydropiper was investigated by GC profiling. Furthermore, the major compounds of the ethylic ether extract of P. hyrcanicum were identified by GC/MS as: α-bisabolol (17.5%, cedrol (15.9%, sesquisabinene hydrate (13.0%, α-elemol (10.5% and trans-longipinocarveol (10.1%. All the identified compounds were sesquiterpenes and no monoterpene, fatty acid and/or hydrocarbone were detected in the extract. Chemical distances among the mentioned species were calculated in order to construct the dendrogram of closely related samples. Results indicated that the distance between two samples of P. hyrcanicum was considered to be short and their GC profiles were quite similar to each other and also there was a close relationship between the two samples of Polygonum with P. avicular. P. hydropiper was observed far from the two samples of P. hyrcanicum in comparison to other samples. Interestingly, P. hyrcanicum, gathered from Veresk, had no close relationship with other pairs of P. hyrcanicum.The results of this study support the phylogenetic relationships among these Polygonum species which was previously reported.

  20. Synthesis and pharmacology of glutamate receptor ligands: new isothiazole analogues of ibotenic acid.

    Science.gov (United States)

    Jørgensen, Charlotte G; Clausen, Rasmus P; Hansen, Kasper B; Bräuner-Osborne, Hans; Nielsen, Birgitte; Metzler, Bjørn; Metzler, Birgitte Bjørn; Kehler, Jan; Krogsgaard-Larsen, Povl; Madsen, Ulf

    2007-02-07

    The naturally occurring heterocyclic amino acid ibotenic acid (Ibo) and the synthetic analogue thioibotenic acid (Thio-Ibo) possess interesting but dissimilar pharmacological activity at ionotropic and metabotropic glutamate receptors (iGluRs and mGluRs). Therefore, a series of Thio-Ibo analogues was synthesized. The synthesis included introduction of substituents by Suzuki and Grignard reactions on 4-halogenated 3-benzyloxyisothiazolols, reduction of the obtained alcohols, followed by introduction of the amino acid moiety by use of 2-(N-tert-butoxycarbonylimino)malonic acid diethyl ester. The obtained Thio-Ibo analogues (1, 2a-g) were characterized in functional assays on recombinant mGluRs and in receptor binding assays on native iGluRs. At mGluRs, the activity at Group II was retained for compounds with small substituents (2a-2d), whereas the Group I and Group III receptor activities for all new compounds were lost. Detection of NMDA receptor affinity prompted further characterization, and two-electrode voltage-clamp recordings at recombinant NMDA receptor subtypes NR1/NR2A-D expressed in Xenopus oocytes were carried out for compounds with small substituents (chloro, bromo, methyl or ethyl, compounds 2a-d). This series of Thio-Ibo analogues defines a structural threshold for NMDA receptor activation and reveals that the individual subtypes have different steric requirements for receptor activation. The compounds 2a and 2c are the first examples of agonists discriminating individual NMDA subtypes.

  1. 乙醚-甲醇-正丁醇多元系汽液平衡的热力学性质%Thermodynamic Properties for Vapor-Liquid Equilibrium of Diethyl Ether Methanol-n-Butanol Multicomponent System

    Institute of Scientific and Technical Information of China (English)

    高大明; 张凌云; 管航敏; 孙虹; 陈红; 朱德春

    2011-01-01

    Under different liquid phase compositions, the isobaric vapor-liquid equilibrium (VLE) data of three binary systems (diethyl ether-methanol, diethyi ether-n-butanol and methanol-n-butanol) and one ternary system (diethyl ether-methanol-n-butanol) were determined at 101.325 kPa by using a novel pump-ebullionmeter.The vapor-phase compositions y of above three binary systems were calculated from T,p,x by the indirect method.The activity coefficients of the three binary systems were correlated separately with Wilson, N-RTL, Margules and van Laar models, and the parameters of liquid phase activity coefficient models were calculated through the least square method, and then the obtained parameters were used to calculate the vapor-phase compositions y. The obtained activity coefficients were used to calculate the excess Gibbs function (GE/RT) of the three binary systems,and the results show that all the systems studied here do not exhibit azeotropes. Using the obtained parameters of Wilson, NRTL, Margules and van Laar models, the experimental VLE data of the ternary system were correlated to construct the thermodynamic model of VLE for the ternary system and to calculate its equilibrating vapor-phase composition y and the bubble point, respectively. The calculated bubble points agree with the experimental data well, and the thermodynamic consistency of the phase equilibrium data of the three binary systems calculated by those model parameters were checked with area test method and got satisfactory results.%用新型泵式沸点仪测定了在101.325 kPa下乙醚-甲醇、乙醚-正丁醇、甲醇-正丁醇3个二元系以及乙醚-甲醇-正丁醇三元系在不同液相组成时的沸点,并用间接法Tpx推算了3个二元系的汽相平衡组成y.3个二元体系活度系数分别用Wilson模型、NRTL模型、Margules模型和van Laar模型进行关联,用最小二乘法求出了它们的液相活度系数模型参数,同时,用这些模型参数来计算它们的

  2. Synthesis of Diethyl Carbonate by Transesterification of Propylene Carbonate and Ethanol Catalyzed by Tetramethyl-Guanidine%四甲基胍催化碳酸丙烯酯与乙醇酯交换合成碳酸二乙酯

    Institute of Scientific and Technical Information of China (English)

    郭莲; 王默; 赵新强; 安华良; 王延吉

    2011-01-01

    采用半连续操作方式,对四甲基胍(TMG)催化碳酸丙烯酯(PC)与乙醇酯交换合成碳酸二乙酯(DEC)反应进行了研究,重点考察了操作条件对合成DEC反应的影响.实验结果表明,TMG催化合成DEC的适宜反应条件为:催化剂用量为初始反应物质量的2.6%,乙醇与PC的摩尔比为10,反应温度80~85℃,反应时间为8h,乙醇滴加速率为1.5 mL/min,全回流时间为0.在此条件下,PC转化率为95.8%,DEC收率为90.7%,DEC选择性为94.7%;说明TMG对PC与乙醇酯交换合成DEC反应具有良好的催化性能.%Synthesis of diethyl carbonate(DEC) through transesterification of propylene carbonate (PC) and ethanol over tetramethyl-guanidine(TMG) catalyst was studied in a set of semi-continuous apparatus. The influences of the reaction conditions on the DEC synthesis were investigated. Under the suitable reaction conditions of mass fraction of catalyst 2.6% (based on mass of the initial reactants), mole ratio of ethanol to PC 10, reaction temperature 80-85 t, reaction time 8 h, drip feed rate of ethanol 1.5 mL/min and total reflux time 0, the conversion of PC, the yield and the selectivity of DEC were 95. 8% , 90.7% and 94.7% , respectively.

  3. Photodegradation of diethyl phthalate with PANi/CNT/TiO{sub 2} immobilized on glass plate irradiated with visible light and simulated sunlight—effect of synthesized method and pH

    Energy Technology Data Exchange (ETDEWEB)

    Hung, Chung-Hsuang, E-mail: jeremyh@ccms.nkfust.edu.tw [Department of Safety, Health and Environmental Engineering, National Kaohsiung First University of Science and Technology, No. 1, University Rd., Yenchau Dist., Kaohsiung 824, Taiwan (China); Yuan, Ching, E-mail: caroline@nuk.edu.tw [Department of Civil and Environmental Engineering, National University of Kaohsiung, No. 700, Kaohsiung University Rd., Nan-Tzu Dist., Kaohsiung City 811, Taiwan (China); Li, Huei-Wen, E-mail: soillab@nuk.edu.tw [Department of Civil and Environmental Engineering, National University of Kaohsiung, No. 700, Kaohsiung University Rd., Nan-Tzu Dist., Kaohsiung City 811, Taiwan (China)

    2017-01-15

    Highlights: • Photocatalysts doped with polyaniline and functionalized CNTs onto TiO{sub 2} were developed. • The PANi/CNT/TiO{sub 2} photocatalysts possessed both advantages of PANi and CNTs. • The fabricated PANi/CNT/TiO{sub 2} photocatalysts exhibited high photocatalytic activity under sunlight. • The hydrothermal synthesized PANi/CNT/TiO{sub 2} presented a good photocatalytic activity and the sol–gel ones presented a good photocatalytic stability. - Abstract: Diethyl phthalate (DEP) is one of the most common phthalates for industrial use and has widely spread in environment. A series of PANi/CNT/TiO{sub 2} potocatalysts immobilized on glass plate irradiated with visible light were presented to degrade DEP in this study. The PANi/CNT/TiO{sub 2} potocatalysts were fabricated by co-doping with polyaniline (PANi) and two functionalized CNT (CNT-COCl and CNT-COOH) onto TiO{sub 2} followed by a hydrothermal synthesis and a sol–gel hydrolysis. Doping of PANi resulted in the absorption edge of the fabricated potocatalysts shifting to 421–437 nm and the most distinguished red-shift effect was found in hydrothermal synthesized photocatalysts. The best DEP degradation of 41.5–59.0% and 44.5–67.4% was found in the simulated sunlight system irradiated for 120 min for sol–gel hydrolysis PANi/CNT/TiO{sub 2} photocatalysts and hydrothermal synthesized ones, respectively. The optimum pH was determined at 5.0 and 7.0 for the two PANi/CNT/TiO{sub 2} photocatalysts mentioned above, respectively. The reusability of the sol–gel hydrolyzed photocatalysts up to 5 times was observed no decline in the photodegradation efficiency but less photocatalytic stability of the hydrothermal synthesized ones was found. Meanwhile, the active species of OH radicals generated in the DEP degradation system was identified by free radical scavenging experiments.

  4. Discovery of diethyl 2,5-diaminothiophene-3,4-dicarboxylate derivatives as potent anticancer and antimicrobial agents and screening of anti-diabetic activity: synthesis and in vitro biological evaluation. Part 1.

    Science.gov (United States)

    Bozorov, Khurshed; Ma, Hai-Rong; Zhao, Jiang-Yu; Zhao, Hai-Qing; Chen, Hua; Bobakulov, Khayrulla; Xin, Xue-Lei; Elmuradov, Burkhon; Shakhidoyatov, Khusnutdin; Aisa, Haji A

    2014-09-12

    Series of diethyl 2,5-diaminothiophene-3,4-dicarboxylate (DDTD) derivatives: azomethines of DDTD (2a-l) have been synthesized and screened for their anticancer, antimicrobial and anti-diabetic activities. The novel synthesized compounds were characterized by (1)H, (13)C NMR, MS and FT-IR analyses. All compounds were evaluated for their antiproliferative activity against three types of cancer cell line such as T47D and MCF-7 (human breast cancer), Hela (human cervical cancer) and Ishikawa (human endometrial cancer) lines. The results showed that most compounds exhibited significant antiproliferative activity against breast cancer cells. The majority of azomethines DDTD influenced strongly against breast cancer cells T47D and MCF-7, among them compounds 2b (2.3 μM), 2c (12.1 μM), 2e (13.2 μM), 2i (14.9 μM), 2j (16.0 μM), 2k (7.1 μM), 2l (8.6 μM) manifest potent anticancer activity against cancer cell T47D than Doxorubicin (DOX, 15.5 μM). Compound 2j has shown potent activity on all three types of cancer cells concurrently and IC50 values were considerably low in comparison with positive control DOX. In addition, all compounds were tested for antimicrobial activity against Staphylococcus aureus ATCC 6538 (Gram positive bacteria), Escherichia coli ATCC 11229 (Gram negative bacteria) and Candida albicans ATCC 10231 (Fungi) strains and 2j which contains in the ring nitrofurfural fragment, showed the highest effect on the three species of microbial pathogens simultaneously. Some compounds induced enzymatic inhibition in a concentration-dependent manner on PTP-1B inhibitor.

  5. 甲醇-乙醚团簇的多光子电离和从头算%The multiphoton ionization and ab initio calculation methanol and diethyl ether cluster

    Institute of Scientific and Technical Information of China (English)

    乔光; 王艳; 张树东; 孔祥和

    2008-01-01

    在355 nm波长下用激光电离飞行时间质谱装置研究了氢键团簇甲醇/乙醚混合团簇的多光子电离,飞行时间质谱仪观测到一系列质子化团簇,为了探讨质子化团簇的形成机理,在B3LYP/6-31++G(d,p)//B3LYP/6-311++G(d,p)基组水平上计算了CH30H-(C2H5)2O离子和中性团簇的稳定几何结构和解离通道和解离能,发现存在一个质子转移过程,解离产物主要为CH3O和[(C2H5)2O]H+.%Methanol and diethyl ether molecular beam ,produced via superonic expansion of their mixture sample carried with neon gas through a pulsed valve, was ionized by ultraviolet pulsed laser of 355 nm, a series of protonated mixture clusters were observed with time-of -flight mass spectrometer. In order to find the basic mechanism of protonated clusters, the CH3OH-(C2H5)2O system was studied by ab initio calculation at B 3LYP/6-31 + +G(d,p)//B3LYP/6-311+ +G(d,p) levels ,according to the results we obtained the geometric structures, dissociation channels and dissociation energies of neutral and ionized clusters. There is a process of proton transfer and the main decompounds are CH3O and [C2H5]2OH+.

  6. Folic Acid

    Science.gov (United States)

    ... damage. 10 Do I need folic acid after menopause? Yes. Women who have gone through menopause still need 400 micrograms of folic acid every ... United States: 2003–2006 . American Journal of Clinical Nutrition; 91(1): 231–237. Hamner, H.C., Cogswell, ...

  7. Acidic electrolyzed water efficiently improves the flavour of persimmon (Diospyros kaki L. cv. Mopan) wine.

    Science.gov (United States)

    Zhu, Wanqi; Zhu, Baoqing; Li, Yao; Zhang, Yanyan; Zhang, Bolin; Fan, Junfeng

    2016-04-15

    The ability of acidic (AcW) and alkaline electrolyzed waters (AlW) to improve the flavour of persimmon (Diospyros kaki L.) wine was evaluated. Wines made with AcW (WAcW) were significantly better than wines made with AlW or pure water (PW) in aroma, taste, and colour. Volatile analysis showed that WAcW has high alcohol and ester contents, including 2-phenylethanol, isopentanol, isobutanol, ethyl dodecanoate, phenethyl acetate, and butanedioic acid diethyl ester. The total amino acid content of persimmon slurry soaked with AcW reached 531.2 mg/l, which was much higher than those of the slurries soaked in AlW (381.3 mg/l) and PW (182.7 mg/l). The composition of major amino acids in the AcW-soaked slurry may contribute to the strong ester flavour of WAcW. This is the first report to suggest that electrolyzed functional water (EFW) can be used to improve wine flavour, leading to the possible use of EFW in food processing.

  8. Comparison of accuracy between petroleum ether and diethyl ether to determine the fat content in sugary samples%石油醚与乙醚测定含糖类样品中脂肪含量的准确率比较

    Institute of Scientific and Technical Information of China (English)

    邱清莲; 蔡伟江; 房家祥

    2016-01-01

    目的:为了提高脂肪提取的准确度,采用石油醚及乙醚对含糖类样品进行提取并比对。方法采用GB/T 5009.6-2003《食品中脂肪测定》第二法对其进行提取。结果结果显示,含糖类样品中脂肪测定时,用乙醚提取后测定的结果比用石油醚提取后测定的结果高。由于水解后的物质,更易溶解在极性相对较高的乙醚中,却不会较好地溶解在石油醚中,因而,乙醚提取脂肪含量偏高,准确度下降。结论实验表明,含糖类样品脂肪测定时,用石油醚测定脂肪的准确度高。%Objective To improve the accuracy of fat extraction, petroleum ether and diethyl ether were used as extracts to compare the results.MethodsThe second method of GB/T 5009.6-2003 "Determination of fat in food" was applied to determine the content of fat. Results It showed that when the fat content in the sugary samples was measured, the results by using diethyl ether as extracts were higher than those of using petroleum ether as extracts, which was due to the materials be hydrolyzed in the samples was better dissolved in the relatively high polarity ether, not in the oil ether. So, the fat content by using diethyl ether as extracts was higher, with lower accuracy.Conclusion It showed that when the fat content in sugary samples was measured, the accuracy with petroleum ether as extracts was higher than that of diethyl ether.

  9. Comparison of accuracy between petroleum ether and diethyl ether to determine the fat content in sugary samples%石油醚与乙醚测定含糖类样品中脂肪含量的准确率比较

    Institute of Scientific and Technical Information of China (English)

    邱清莲; 蔡伟江; 房家祥

    2016-01-01

    目的:为了提高脂肪提取的准确度,采用石油醚及乙醚对含糖类样品进行提取并比对。方法采用GB/T 5009.6-2003《食品中脂肪测定》第二法对其进行提取。结果结果显示,含糖类样品中脂肪测定时,用乙醚提取后测定的结果比用石油醚提取后测定的结果高。由于水解后的物质,更易溶解在极性相对较高的乙醚中,却不会较好地溶解在石油醚中,因而,乙醚提取脂肪含量偏高,准确度下降。结论实验表明,含糖类样品脂肪测定时,用石油醚测定脂肪的准确度高。%ABSTRACT:Objective To improve the accuracy of fat extraction, petroleum ether and diethyl ether were used as extracts to compare the results. Methods The second method of GB/T 5009.6-2003"Determination of fat in food"was applied to determine the content of fat. Results It showed that when the fat content in the sugary samples was measured, the results by using diethyl ether as extracts were higher than those of using petroleum ether as extracts, which was due to the materials be hydrolyzed in the samples was better dissolved in the relatively high polarity ether, not in the oil ether. So, the fat content by using diethyl ether as extracts was higher, with lower accuracy. Conclusion It showed that when the fat content in sugary samples was measured, the accuracy with petroleum ether as extracts was higher than that of diethyl ether.

  10. Effects of Lewis-acid polymer on the electrochemical properties of alkylphosphate-based non-flammable gel electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Lalia, Boor Singh; Yoshimoto, Nobuko; Egashira, Minato; Morita, Masayuki [Department of Applied Chemistry, Graduate School of Science and Engineering, Yamaguchi University, 2-16-1 Tokiwadai, Ube 755-8611 (Japan)

    2009-10-20

    Non-flammable polymer gel electrolytes (NPGE) consisting of 1.0 mol dm{sup -3} (=M) LiBF{sub 4}/EC + DEC + TEP (55:25:20 volume ratio) + PVdF-HFP (EC: ethylene carbonate, DEC: diethyl carbonate, TEP: triethylphosphate, PVdF-HFP: poly(vinyledenefluoride-co-hexafluoropropylene)) have been developed for rechargeable lithium batteries. The effects of addition of Lewis-acid polymer (LAP) with different mole ratio in NPGE have been studied. The addition of LAP improved physico-chemical properties of NPGE, viz ionic conductivity and lithium ion transport number, as well as mechanical and thermal properties. The ionic conductivity of the gel electrolyte containing LAP reached that of the base solution electrolyte (1.0 M LiBF{sub 4}/EC + DEC + TEP (55:25:20)) along with better mechanical properties. Interfacial resistance at Li-metal electrode/NPGE was also improved by introducing LAP in the gel. (author)

  11. Effects of Lewis-acid polymer on the electrochemical properties of alkylphosphate-based non-flammable gel electrolyte

    Science.gov (United States)

    Lalia, Boor Singh; Yoshimoto, Nobuko; Egashira, Minato; Morita, Masayuki

    Non-flammable polymer gel electrolytes (NPGE) consisting of 1.0 mol dm -3 (=M) LiBF 4/EC + DEC + TEP (55:25:20 volume ratio) + PVdF-HFP (EC: ethylene carbonate, DEC: diethyl carbonate, TEP: triethylphosphate, PVdF-HFP: poly(vinyledenefluoride-co-hexafluoropropylene)) have been developed for rechargeable lithium batteries. The effects of addition of Lewis-acid polymer (LAP) with different mole ratio in NPGE have been studied. The addition of LAP improved physico-chemical properties of NPGE, viz ionic conductivity and lithium ion transport number, as well as mechanical and thermal properties. The ionic conductivity of the gel electrolyte containing LAP reached that of the base solution electrolyte (1.0 M LiBF 4/EC + DEC + TEP (55:25:20)) along with better mechanical properties. Interfacial resistance at Li-metal electrode/NPGE was also improved by introducing LAP in the gel.

  12. Folic acid

    Science.gov (United States)

    ... taking a specific nutritional supplement, containing vitamin B3 (nicotinamide), a compound isolated from grains (azelaic acid), zinc, ... lung cancer in most people. A type of skin cancer called melanoma. Limited research suggests that taking ...

  13. Folic Acid

    Science.gov (United States)

    ... B-complex vitamin needed by the body to manufacture red blood cells. A deficiency of this vitamin ... prepared from dried yeast, fruit, and fresh leafy green vegetables to increase the folic acid in your ...

  14. Study on the degradation of diethyl phthalate by UV/Fe0 system%UV/Fe0体系降解邻苯二甲酸二乙酯的研究

    Institute of Scientific and Technical Information of China (English)

    胡菲菲; 邵庆国

    2013-01-01

    尝试利用UV/Fe0体系降解邻苯二甲酸二乙酯(DEP)废水,探讨了pH、Fe0投加量、DEP初始浓度等影响因素对降解效果的影响.结果表明,对于24 mg/L的DEP废水,在pH=3、Fe0投加量为20mg/L时,反应60 min后的DEP降解率可达93.5%,并且该降解过程符合准一级反应动力学规律;在UV/Fe0体系降解DEP过程中,Fe2+、Fe3+浓度均在反应一定时间后趋于平衡,并且Fe2+的浓度始终高于Fe3+;UV、Fe0在DEP的降解中存在协同作用.UV/Fe0体系对DEP废水具有良好的降解效果,并且不需要额外添加高价的H2O2,为DEP废水的工业化处理提供了一种较好的方法.%UV/Fe° system was applied for the treatment of diethyl phthalate (DEP) containing wastewater. The effect of pH,Fe° dosage, and initial DEP concentration on DEP degradation efficiency was investigated. The results showed that when the initial DEP was 24 mg/L,Fe° dosage was 20 mg/L and pH was 3,the degradation rate of DEP could reach to 93. 5 % after 60 min of reaction,and the degradation process could be better fitted by pseudo first-order kinetics. During the degradation process,the concentration of Fe2+ , Fe3+ in UV/Fe° system reached equilibrium after a certain time of reaction,and Fe2+ was consistently higher than Fe3+. There was synergistic effect found between UV and Fe° in the DEP degradation process. UV/Fe° system exhibited perfect DEP degradation efficiency without adding high-priced H2O2 ,so it was a suitable method for the industrialized treatment of DEP containing wastewater.

  15. New insight of coordination and extraction of uranium(VI) with N-donating ligands in room temperature ionic liquids: N,N'-diethyl-N,N'-ditolyldipicolinamide as a case study.

    Science.gov (United States)

    Yuan, Li-Yong; Sun, Man; Mei, Lei; Wang, Lin; Zheng, Li-Rong; Gao, Zeng-Qiang; Zhang, Jing; Zhao, Yu-Liang; Chai, Zhi-Fang; Shi, Wei-Qun

    2015-02-16

    Room temperature ionic liquids (RTILs) represent a recent new class of solvents applied in liquid/liquid extraction based nuclear fuel reprocessing, whereas the related coordination chemistry and detailed extraction processes are still not well understood and remain of deep fundamental interest. The work herein provides a new insight of coordination and extraction of uranium(VI) with N-donating ligands, e.g., N,N'-diethyl-N,N'-ditolyldipicolinamide (EtpTDPA), in commonly used RTILs. Exploration of the extraction mechanism, speciation analyses of the extracted U(VI), and crystallographic studies of the interactions of EtpTDPA with U(VI) were performed, including the first structurally characterized UO2(EtpTDPA)2(NTf2) and UO2(EtpTDPA)2(PF6)2 compounds and a first case of crystallographic differentiation between the extracted U(VI) complexes in RTILs and in molecular solvents. It was found that in RTILs two EtpTDPA molecules coordinate with one U(VI) ion through the carbonyl and pyridine nitrogen moieties, while NTf2(-) and PF6(-) act as counterions. The absence of NO3(-) in the complexes is coincident with a cation-exchange extraction. In contrast, both the extracted species and extraction mechanisms are greatly different in dichloromethane, in which UO2(2+) coordinates in a neutral complex form with one EtpTDPA molecule and two NO3(-) cations. In addition, the complex formation in RTILs is independent of the cation exchange since incorporating UO2(NO3)2, EtpTDPA, and LiNTf2 or KPF6 in a solution also produces the same complex as that in RTILs, revealing the important roles of weakly coordinating anions on the coordination chemistry between U(VI) and EtpTDPA. These findings suggest that cation-exchange extraction mode for ILs-based extraction system probably originates from the supply of weakly coordinating anions from RTILs. Thus the coordination of uranium(VI) with extractants as well as the cation-exchange extraction mode may be potentially changed by varying the

  16. Kinetics of transesterification of dimethyl carbonate with diethyl carbonate catalyzed by basic ionic liquids%碱性离子液体催化合成碳酸甲乙酯反应动力学

    Institute of Scientific and Technical Information of China (English)

    张运茂; 邵晓楠; 刘威华; 刘涛; 刘勇

    2016-01-01

    The transesterification reaction of dimethyl carbonate ( DMC) and diethyl carbonate ( DEC) for the synthesis of ethyl methyl carbonate ( EMC ) in the presence of several basic liquids was studied . Among these catalysts,1-butyl-3-methylimidazolium butyrate [C4mim][CH3(CH2)2COO] exhibited the best catalysis activity .The effects of reaction temperature ,catalyst loading and reactants molar ratio on the conversion of DEC on reaction rate were studied .Under the reaction temperature 363.15 K,catalyst load-ing 6%( based on the mass of all reactants),n(DMC)∶n(DEC)=1.5∶1,reaction time 6 h,the conver-sion of DEC was 50%.A pseudo-homogeneous ( PH) kinetic model was used to correlate the experimen-tal data.The activation energies of the positive and reverse reactions were 56.10,46.70 kJ/mol,and the pre-exponential factors were 1.17 ▍105,1.57 ▍103 L2/(mol· min· g),respectively.%以不同碱性离子液体催化碳酸二甲酯(DMC)与碳酸二乙酯(DEC)酯交换反应合成碳酸甲乙酯(EMC),研究了反应温度、催化剂的用量、反应物摩尔配比等因素对反应速率的影响。结果表明,碱性离子液体1-丁基-3-甲基咪唑丁酸盐[C4mim][CH3(CH2)2COO]显示出高的催化活性,在反应温度363.15 K,催化剂用量6%(占反应物总质量百分数),n(DMC)∶n(DEC)=1.5∶1,反应时间6 h的条件下,DEC转化率达50%。建立了拟均相动力学模型,得出正逆反应活化能分别为56.10,46.70 kJ/mol,指前因子分别为1.17▍105,1.57▍103 L2/(mol· min· g)。

  17. 草酸二乙酯和草酸二甲酯加氢反应热力学对比分析%Comparative Thermodynamic Analysis of Hydrogenations of Diethyl Oxalate and Dimethyl Oxalate

    Institute of Scientific and Technical Information of China (English)

    张旭; 王保伟

    2011-01-01

    采用Benson基团贡献法、Constantinou - Gani法和Rihani - Dorasiwamy法计算了草酸二乙酯(DEO)、乙醇酸乙酯、草酸二甲酯(DMO)和乙醇酸甲酯等物质的标准生成焓、标准生成吉布斯自由能和摩尔定压热容.在473 ~513 K和1.0~3.5 MPa下,分别计算了DEO和DMO加氢反应的焓变、吉布斯自由能变和平衡常数.计算结果表明,除在低压高温条件下乙醇酸甲酯加氢生成乙二醇的反应为非自发反应外,DEO和DMO加氢都是自发进行的放热反应;低温高压有利于生成乙二醇;与DMO的加氢反应相比,DEO加氢反应具有更高的平衡常数.%Standard enthalpies of formation △H-f, standard Gibbs free energies of formation △fG-298 and molar heat capacities at constant pressure Cpm of diethyl oxalate(DEO) , ethyl glycolate, dimethyl oxalate(DMO) and methyl glycollate(MG) etc. , and further the enthalpy changes △rHT Gibbs free energy changes △rGT and equilibrium constants Kp in hydrogenations of DEO and DMO under 473 -513 K and 1.0-3.5 Mpa were calculated by different methods, including Benson group contribution method, Constantinou-Gani method and Rihani-Dorasiwamy method. The results show that the hydrogenations of DEO and DMO are spontaneous exothermic reactions, except for the production of ethylene glycol from MG, which is not spontaneous at low pressure and high temperature. Low temperature and high pressure are propitious to synthesis of ethylene glycol. Kp of DEO hydrogenation is higher than that of DMO hydrogenation.

  18. Ibotenic acid and thioibotenic acid

    DEFF Research Database (Denmark)

    Hermit, Mette B; Greenwood, Jeremy R; Nielsen, Birgitte

    2004-01-01

    with the conformations preferred by the ligands upon docking to mGlu1 and models of the other mGlu subtypes, we propose that unlike other subtypes, group III mGlu receptor binding sites require a ligand conformation at an energy level which is prohibitively expensive for ibotenic acid, but not for thioibotenic acid....... These studies demonstrate how subtle differences in chemical structures can result in profound differences in pharmacological activity....

  19. Diethyl [(4-nitrobenzamido(phenylmethyl]phosphonate

    Directory of Open Access Journals (Sweden)

    Jing-Wei Chen

    2014-05-01

    Full Text Available In the title compound, C18H21N2O6P, the dihedral angle between the benzene and phenyl rings is 85.1 (2°. In the crystal, molecules are linked via pairs of N—H...O(=P hydrogen bonds, forming inversion dimers with graph-set notation R22(10. One of the ethyl groups is disordered over two sets of sites, with occupancies 0.746 (11 and 0.254 (11.

  20. MICROWAVE IRRADIATED ALKYLATION OF DIETHYL ACETAMIDOMALONATE

    Institute of Scientific and Technical Information of China (English)

    张雅文; 沈宗旋; 陆军

    1995-01-01

    Ethyl acetamidomalonate was alkylated using three alkylating agents, both by microtwave irradiation of a mixture of the malonate,the alkylating agent, potassium carbonate,TEBA,and DMF for 0.5 to 1.5 min and by heating a solution of the malonate, sodium ethoxide, and the alkylatlng agent in ethanol for several hours. The two metlmds gave comparable results.

  1. Diethyl (1-hydroxy-1,2-diphenylethylphosphonate

    Directory of Open Access Journals (Sweden)

    Nurcan Acar

    2009-06-01

    Full Text Available In the title compound, C18H23O4P, the dihedral angle between the aromatic ring planes is 69.94 (14°. Both ethyl side chains are disordered over two sets of sites, with occupancy ratios of 80:20 and 70:30. In the crystal, inversion dimers linked by pairs of O—H...O hydrogen bonds occur, leading to R21(8 loops, and C—H...O and weak C—H...π interactions are also seen.

  2. Not in My Navy. A Legal Guide to Drug Abuse.

    Science.gov (United States)

    1984-06-01

    psychotanimetics, dysleptics or psychedelics. These drugs include mescaline, peyote, lysergic acid diethylamide (LSD), psilocybin, dimethyltryptamine (DMTr) and...powdered, or liquid form. DMT ( dimethyltryptamine ) is a more recent addition to the list of presently abused hallucinogenic agents. Although prepared

  3. 76 FR 65537 - Controlled Substances: Proposed Aggregate Production Quotas for 2012

    Science.gov (United States)

    2011-10-21

    ... site for easy reference. Paper comments that duplicate the electronic submission are not necessary as... Heroin 20 Hydromorphinol 2 Hydroxypethidine 2 Ibogaine 5 Lysergic acid diethylamide (LSD) 16 Marihuana...

  4. LSD

    Science.gov (United States)

    ... Loss Surgery? A Week of Healthy Breakfasts Shyness LSD KidsHealth > For Teens > LSD A A A What's ... How Can Someone Quit? Avoiding LSD What Is LSD? LSD is short for d-lysergic acid diethylamide. ...

  5. LSD

    Science.gov (United States)

    ... Can I Help Someone Who's Being Bullied? Volunteering LSD KidsHealth > For Teens > LSD Print A A A ... Quit? Avoiding LSD en español LSD What Is LSD? LSD is short for d-lysergic acid diethylamide. ...

  6. LSD and Genetic Damage

    Science.gov (United States)

    Dishotsky, Norman I.; And Others

    1971-01-01

    Reviews studies of the effects of lysergic acid diethylamide (LSD) on man and other organisms. Concludes that pure LSD injected in moderate doses does not cause chromosome or detectable genetic damage and is not a teratogen or carcinogen. (JM)

  7. LSD and Genetic Damage

    Science.gov (United States)

    Dishotsky, Norman I.; And Others

    1971-01-01

    Reviews studies of the effects of lysergic acid diethylamide (LSD) on man and other organisms. Concludes that pure LSD injected in moderate doses does not cause chromosome or detectable genetic damage and is not a teratogen or carcinogen. (JM)

  8. 78 FR 36591 - Importer of Controlled Substances; Notice of Application; Lipomed

    Science.gov (United States)

    2013-06-18

    ... Federal Register on September 23, 1975, 40 FR 43745-46, all applicants for registration to import a basic... Homologue (7298) I Lysergic acid diethylamide (7315) I 2C-T-7 (7348) I Marihuana (7360)...

  9. 78 FR 32457 - Importer of Controlled Substances; Notice of Application; United States Pharmacopeial Convention

    Science.gov (United States)

    2013-05-30

    ... September 23, 1975, 40 FR 43745-46, all applicants for registration to import a basic classes of any... Methaqualone (2565) I Lysergic acid diethylamide (7315) I Marihuana (7360) I Tetrahydrocannabinols (7370) I...

  10. Structure Effect of Diacid/Triacid on Self-Assembly of Binary Organogels Based on Glutamic Acid Amino Derivative

    Directory of Open Access Journals (Sweden)

    Jinming Dai

    2013-01-01

    Full Text Available The gelation behaviors of binary organogels composed of N-(4-aminobenzoyl-L-glutamic acid diethyl ester with sebacic acid and citric acid in various organic solvents were designed and investigated. Their gelation behaviors in 20 solvents were tested as new binary organic gelators. It showed that the molecular structures and organic solvents have played a crucial role in the gelation behavior of all gelator mixtures. More carboxyl groups in molecular skeletons in the present mixture gelators are unfavorable for the gelation of organic solvents. The mixture containing sebacic acid can form 5 kinds of organogels, while another mixture containing citric acid can only form 3 kinds of organogels in different solvents. Morphological studies revealed that the gelator molecules self-assemble into different aggregates from wrinkle and belt to fiber with change of solvents. Spectral studies indicated that there existed different H-bond formations and hydrophobic forces, depending on solvents and molecular structures. The as-prepared nanomaterials have wide perspectives in nanoscience and functional textile materials with special microstructures.

  11. Acid Rain

    Science.gov (United States)

    Bricker, Owen P.; Rice, Karen C.; Dietrich, W.E.; Sposito, Garrison

    1997-01-01

    Acid deposition, or acid rain as it is more commonly referred to, has become a widely publicized environmental issue in the U.S. over the past decade. The term usually conjures up images of fish kills, dying forests, "dead" lakes, and damage to monuments and other historic artifacts. The primary cause of acid deposition is emission of S02 and NOx to the atmosphere during the combustion of fossil fuels. Oxidation of these compounds in the atmosphere forms strong acids - H2SO4 and HNO3 - which are returned to the Earth in rain, snow, fog, cloud water, and as dry deposition.Although acid deposition has only recently been recognized as an environmental problem in the U.S., it is not a new phenomenon (Cogbill & Likens 1974). As early as the middle of the 17th century in England, the deleterious effects of industrial emissions on plants, animals, and humans, and the atmospheric transport of pollutants between England and France had become issues of concern (Evelyn 1661, Graunt 1662). It is interesting that well over three hundred years ago in England, recommendations were made to move industry outside of towns and build higher chimneys to spread the pollution into "distant parts." Increasing the height of smokestacks has helped alleviate local problems, but has exacerbated others. In the U.S. the height of the tallest smokestack has more than doubled, and the average height of smokestacks has tripled since the 1950s (Patrick et al 1981). This trend occurred in most industrialized nations during the 20th century and has had the effect of transforming acid rain from a local urban problem into a problem of global scale.

  12. Perfluorooctanoic acid

    NARCIS (Netherlands)

    de Voogt, P.; Wexler, P.

    2014-01-01

    Perfluorooctanoic acid (PFOA, 335-67-1) is used in fluoropolymer production and firefighting foams and persists in the environment. Human exposure to PFOA is mostly through the diet. PFOA primarily affects the liver and can cause developmental and reproductive toxic effects in test animals.

  13. Determination of acetylsalicylic acid and its major metabolite, salicylic acid, in human plasma using liquid chromatography-tandem mass spectrometry: application to pharmacokinetic study of Astrix in Korean healthy volunteers.

    Science.gov (United States)

    Bae, Soo Kyung; Seo, Kyung Ah; Jung, Eun Ji; Kim, Ho-Sook; Yeo, Chang-Woo; Shon, Ji-Hong; Park, Kyung-Mi; Liu, Kwang-Hyeon; Shin, Jae-Gook

    2008-06-01

    The first liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for determination of acetylsalicylic acid (aspirin, ASA) and one of its major metabolites, salicylic acid (SA), in human plasma using simvastatin as an internal standard has been developed and validated. For ASA analysis, a plasma sample containing potassium fluoride was extracted using a mixture of ethyl acetate and diethyl ether in the presence of 0.5% formic acid. SA, a major metabolite of ASA, was extracted from plasma using protein precipitation with acetonitrile. The compounds were separated on a reversed-phase column with an isocratic mobile phase consisting of acetonitrile and water containing 0.1% formic acid (8:2, v/v). The ion transitions recorded in multiple reaction monitoring mode were m/z 179 --> 137, 137 --> 93 and 435 --> 319 for ASA, SA and IS, respectively. The coefficient of variation of the assay precision was less than 9.3%, and the accuracy exceeded 86.5%. The lower limits of quantification for ASA and SA were 5 and 50 ng/mL, respectively. The developed assay method was successfully applied for the evaluation of pharmacokinetics of ASA and SA after single oral administration of Astrix (entero-coated pellet, 100 mg of aspirin) to 10 Korean healthy male volunteers.

  14. Comparison of amino acid derivatization reagents for LC-ESI-MS analysis. Introducing a novel phosphazene-based derivatization reagent.

    Science.gov (United States)

    Rebane, Riin; Oldekop, Maarja-Liisa; Herodes, Koit

    2012-09-01

    Amino acid analysis with high performance liquid chromatography with electrospray ionization mass spectrometry (LC-ESI-MS) is an emerging method. For more sensitive analysis, derivatization is used and next to commercially available derivatization reagents such as dansyl chloride (DNS), 9-fluorenylmethyl chloroformate (FMOC-Cl) and diethyl ethoxymethylenemalonate (DEEMM), new derivatization reagents are designed specially for LC-ESI-MS, like p-N,N,N-trimethylammonioanilyl N'-hydroxysuccinimidyl carbamate iodide (TAHS) which provides very low limits of detection. In this work, a novel phosphazene based derivatization reagent (FOSF) that provides comparable limits of quantitation (LoQ) to TAHS is introduced. Moreover, a thorough comparison between FOSF, TAHS, DNS, FMOC-Cl and DEEMM is carried out for 7 different amino acids - Arg, Asp, Gly, β-Ala, Pro, Trp and Phe. This is a first time that thorough comparison is carried out on the same instrument for amino acid derivatization reagents. Results on the same instrument for five amino acid derivatization reagents show that novel reagents are sensitive with LoQ values around 80 fmol but have disadvantages such as problematic chromatographic separation. Next to novel reagents, DEEMM offers very good LoQ-s (average of 150 fmol) and wide dynamic linear range.

  15. Hydroxycarboxylic acids and salts

    Energy Technology Data Exchange (ETDEWEB)

    Kiely, Donald E; Hash, Kirk R; Kramer-Presta, Kylie; Smith, Tyler N

    2015-02-24

    Compositions which inhibit corrosion and alter the physical properties of concrete (admixtures) are prepared from salt mixtures of hydroxycarboxylic acids, carboxylic acids, and nitric acid. The salt mixtures are prepared by neutralizing acid product mixtures from the oxidation of polyols using nitric acid and oxygen as the oxidizing agents. Nitric acid is removed from the hydroxycarboxylic acids by evaporation and diffusion dialysis.

  16. Acylation of Antioxidant of Bamboo Leaves with Fatty Acids by Lipase and the Acylated Derivatives’ Efficiency in the Inhibition of Acrylamide Formation in Fried Potato Crisps

    Science.gov (United States)

    Ma, Xiang; Wang, Erpei; Lu, Yuyun; Wang, Yong; Ou, Shiyi; Yan, Rian

    2015-01-01

    This study selectively acylated the primary hydroxyl groups on flavonoids in antioxidant of bamboo leaves (AOB) using lauric acid with Candida antarctica lipase B in tert-amyl-alcohol. The separation and isolation of acylated derivatives were performed using silica gel column chromatography with a mixture of dichloromethane/diethyl ether/methanol as eluents. Both thin layer chromatography and high-performance liquid chromatography analyses confirmed the high efficiency of the isolation process with the purified orientin-6″-laurate, isoorientin-6″-laurate, vitexin-6″-laurate, and isovitexin-6″-laurate that were obtained. The addition of AOB and acylated AOB reduced acrylamide formation in fried potato crisps. Results showed that 0.05% AOB and 0.05% and 0.1% acylated AOB groups significantly (p acrylamide in potato crisps by 30.7%, 44.5%, and 46.9%, respectively. PMID:26098744

  17. Acylation of Antioxidant of Bamboo Leaves with Fatty Acids by Lipase and the Acylated Derivatives' Efficiency in the Inhibition of Acrylamide Formation in Fried Potato Crisps.

    Science.gov (United States)

    Ma, Xiang; Wang, Erpei; Lu, Yuyun; Wang, Yong; Ou, Shiyi; Yan, Rian

    2015-01-01

    This study selectively acylated the primary hydroxyl groups on flavonoids in antioxidant of bamboo leaves (AOB) using lauric acid with Candida antarctica lipase B in tert-amyl-alcohol. The separation and isolation of acylated derivatives were performed using silica gel column chromatography with a mixture of dichloromethane/diethyl ether/methanol as eluents. Both thin layer chromatography and high-performance liquid chromatography analyses confirmed the high efficiency of the isolation process with the purified orientin-6″-laurate, isoorientin-6″-laurate, vitexin-6″-laurate, and isovitexin-6″-laurate that were obtained. The addition of AOB and acylated AOB reduced acrylamide formation in fried potato crisps. Results showed that 0.05% AOB and 0.05% and 0.1% acylated AOB groups significantly (p < 0.05) reduced the content of acrylamide in potato crisps by 30.7%, 44.5%, and 46.9%, respectively.

  18. Acylation of Antioxidant of Bamboo Leaves with Fatty Acids by Lipase and the Acylated Derivatives' Efficiency in the Inhibition of Acrylamide Formation in Fried Potato Crisps.

    Directory of Open Access Journals (Sweden)

    Xiang Ma

    Full Text Available This study selectively acylated the primary hydroxyl groups on flavonoids in antioxidant of bamboo leaves (AOB using lauric acid with Candida antarctica lipase B in tert-amyl-alcohol. The separation and isolation of acylated derivatives were performed using silica gel column chromatography with a mixture of dichloromethane/diethyl ether/methanol as eluents. Both thin layer chromatography and high-performance liquid chromatography analyses confirmed the high efficiency of the isolation process with the purified orientin-6″-laurate, isoorientin-6″-laurate, vitexin-6″-laurate, and isovitexin-6″-laurate that were obtained. The addition of AOB and acylated AOB reduced acrylamide formation in fried potato crisps. Results showed that 0.05% AOB and 0.05% and 0.1% acylated AOB groups significantly (p < 0.05 reduced the content of acrylamide in potato crisps by 30.7%, 44.5%, and 46.9%, respectively.

  19. Progress in the Synthesis of 4 -Trifluoromethylphenyl Acetic Acid%对三氟甲基苯乙酸的合成研究进展

    Institute of Scientific and Technical Information of China (English)

    邓绍平; 陈洁

    2012-01-01

    Research progress on the synthesis method of 4 -trifluoromethylphenyl acetic acid and its application as pharmaceutical intermediate in the synthesis of pharmaceuticals were described. The methods including 4 -trifluoromethyl beryl chloride, 4 -trifluoromethyl acetophenone, diethyl malonate and 4 - trifluoromethyl aniline were reviewed and summarized.%叙述了对三氟甲基苯乙酸合成方法的研究进展,及其作为医药中间体在药物合成中的应用。将对三氟甲基氯苄法、对三氟甲基苯乙酮法、丙二酸二乙酯法、对三氟甲基苯胺法合成对三氟甲基苯乙酸进行了概括总结。

  20. SYNTHESIS AND PROPERTIES OF POLYACETYLENES CONTAINING CARBAZOLE AND AMINO ACID MOIETIES

    Institute of Scientific and Technical Information of China (English)

    Feng Jiang; Jin-qing Qu; Huan-qin Chen

    2009-01-01

    Novel 9-proparylcarbazole monomers containing amino acid moieties, 2-N-(tert-butoxycarbonyl)-L-alanine-9-proparylcarbazole ester (1), 2-N-(tert-butoxycarbonyl)-L-O-cyclohexyI-L-glutamic acid-9-proparylcarbazole ester (2) and 2-N-(tert-butoxycarbonyl)-L-phenylalanine-9-proparylcarbazole ester (3) were synthesized and polymerized with (nbd)Rh~+[η~6-C_6H_5B~-(C_6H_5)_3 ] to give the corresponding polymers with number-average molecular weights ranging from 7050 to 10500 in 70%-86% yields. The polymers were completely soluble in toluene, CHCl_3 , CH_2Cl_2, THF and DMSO, but insoluble in hexane, diethyl ether and MeOH. The specific rotation studies revealed that poly(1)-poly(3) do not took predominantly one-handed helical structures in the solvents although they possess chiral groups. The polymers emitted fluorescence in 0.40%-2.35% quantum yields. The cyclic voltammograms of the polymers indicated that the polymers exhibited electrochemical properties.

  1. Hydrofluoric acid poisoning

    Science.gov (United States)

    Fluorhydric acid ... stomach, or intestine have holes (perforations) from the acid. ... Hydrofluoric acid is especially dangerous. The most common accidents involving hydrofluoric acid cause severe burns on the skin ...

  2. Return of the lysergamides. Part III: Analytical characterization of N(6) -ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1-propionyl ETH-LAD (1P-ETH-LAD).

    Science.gov (United States)

    Brandt, Simon D; Kavanagh, Pierce V; Westphal, Folker; Elliott, Simon P; Wallach, Jason; Stratford, Alexander; Nichols, David E; Halberstadt, Adam L

    2017-03-24

    The psychoactive properties of lysergic acid diethylamide (LSD) have fascinated scientists across disciplines and the exploration of other analogs and derivatives has been motivated by deepening the understanding of ligand-receptor interactions at the molecular level as well as by the search for new therapeutics. Several LSD congeners have appeared on the new psychoactive substances (NPS) market in the form of blotters or powders. Examples include 1-propionyl-LSD (1P-LSD), AL-LAD and LSZ. The absence of analytical data for novel compounds is a frequent challenge encountered in clinical and toxicological investigations. Two newly emerging lysergamides N(6) -ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1P-ETH-LAD were characterized by gas chromatography mass spectrometry (GC-MS), low and high mass accuracy electrospray MS(/MS), GC solid-state infrared analysis, high performance liquid chromatography diode array detection as well as nuclear magnetic resonance spectroscopy. Limited analytical data for ETH-LAD were previously available, whereas information about 1P-ETH-LAD has not previously been encountered in scientific literature. This study extends the characterization of lysergamides distributed on the NPS market, which will help to make analytical data available to clinicians, toxicologists and other stakeholders who are likely to encounter these substances. The analysis of a test incubation of 1P-ETH-LAD with human serum at 37 °C by LC single quadrupole MS at various time points (0-6 h, once per hour and one measurement after 24 h) revealed the formation of ETH-LAD, suggesting that 1P-ETH-LAD might serve as a pro-drug. 1P-ETH-LAD was still detectable in serum after 24 h.

  3. Usnic acid potassium salt: an alternative for the control of Biomphalaria glabrata (Say, 1818.

    Directory of Open Access Journals (Sweden)

    Mônica C B Martins

    Full Text Available In Brazil, the snail Biomphalaria glabrata is the most important vector of schistosomiasis due to its wide geographical distribution, high infection rate and efficient disease transmission. Among the methods of schistosomiasis control, the World Health Organization recommends the use of synthetic molluscicides, such as niclosamide. However, different substances of natural origin have been tested as alternatives for the control or eradication of mollusks. The literature describes the antitumor, antimicrobial and antiviral properties of usnic acid as well as other important activities of common interest between medicine and the environment. However, usnic acid has a low degree of water solubility, which can be a limiting factor for its use, especially in aquatic environments, since the organic solvents commonly used to solubilize this substance can have toxic effects on aquatic biota. Thus, the aim of the present study was to test the potassium salt of usnic acid (potassium usnate with regard to molluscicidal activity and toxicity to brine shrimp (Artemia salina. To obtain potassium usnate, usnic acid was extracted with diethyl ether isolated and purified from the lichen Cladonia substellata. Biological assays were performed with embryos and adult snails of B. glabrata exposed for 24 h to the usnate solution solubilized in dechlorinated water at 2.5; 5 and 10 µg/ml for embryos, 0.5; 0.9; 1;5 and 10 µg/ml for mollusks and 0.5; 1; 5; 10 µg/ml for A. salina. The lowest lethal concentration for the embryos and adult snails was 10 and 1 µg/ml, respectively. No toxicity to A. salina was found. The results show that modified usnic acid has increased solubility (100% without losing its biological activity and may be a viable alternative for the control of B. glabrata.

  4. Usnic acid potassium salt: an alternative for the control of Biomphalaria glabrata (Say, 1818).

    Science.gov (United States)

    Martins, Mônica C B; Silva, Monique C; Silva, Luanna R S; Lima, Vera L M; Pereira, Eugênia C; Falcão, Emerson P S; Melo, Ana M M A; da Silva, Nicácio Henrique

    2014-01-01

    In Brazil, the snail Biomphalaria glabrata is the most important vector of schistosomiasis due to its wide geographical distribution, high infection rate and efficient disease transmission. Among the methods of schistosomiasis control, the World Health Organization recommends the use of synthetic molluscicides, such as niclosamide. However, different substances of natural origin have been tested as alternatives for the control or eradication of mollusks. The literature describes the antitumor, antimicrobial and antiviral properties of usnic acid as well as other important activities of common interest between medicine and the environment. However, usnic acid has a low degree of water solubility, which can be a limiting factor for its use, especially in aquatic environments, since the organic solvents commonly used to solubilize this substance can have toxic effects on aquatic biota. Thus, the aim of the present study was to test the potassium salt of usnic acid (potassium usnate) with regard to molluscicidal activity and toxicity to brine shrimp (Artemia salina). To obtain potassium usnate, usnic acid was extracted with diethyl ether isolated and purified from the lichen Cladonia substellata. Biological assays were performed with embryos and adult snails of B. glabrata exposed for 24 h to the usnate solution solubilized in dechlorinated water at 2.5; 5 and 10 µg/ml for embryos, 0.5; 0.9; 1;5 and 10 µg/ml for mollusks and 0.5; 1; 5; 10 µg/ml for A. salina. The lowest lethal concentration for the embryos and adult snails was 10 and 1 µg/ml, respectively. No toxicity to A. salina was found. The results show that modified usnic acid has increased solubility (100%) without losing its biological activity and may be a viable alternative for the control of B. glabrata.

  5. Depletion of hepatic uridine diphosphoglucuronic acid decreases the biliary excretion of drugs.

    Science.gov (United States)

    Gregus, Z; Watkins, J B; Thompson, T N; Klaassen, C D

    1983-05-01

    Hepatic levels of uridine diphosphoglucuronic acid (UDPGA) in rats decreased substantially (greater than 80%) 40 min after galactosamine (GAL) (600 mg/kg i.p.) or after 1 hr of diethyl ether (DE) narcosis. Biliary excretion of several cholephils requiring glucuronidation before excretion was reduced by GAL 76, 62, 92, 90 and 97% for bilirubin, diethylstilbestrol, iopanoic acid, phenolphthalein and valproic acid, respectively. GAL treatment caused delayed plasma clearances of the parent compounds and reductions in plasma concentrations and biliary excretions of glucuronide conjugates. The degree of this reduction was related to the maximal excretion rate of the individual compounds. For phenolphthalein glucuronide and phenol-3,6-dibromphthalein disulfonate, which do not undergo conjugation, GAL had no effect on their biliary excretion. DE-induced UDPGA depletion had no effect on phenolphthalein glucuronide excretion but reduced that of phenol-3,6-dibromphthalein disulfonate 25%. DE did not affect the plasma elimination or biliary secretion of phenolphthalein. Of the other cholephils requiring conjugation, DE reduced the excretion of bilirubin, diethylstilbestrol, iopanoic acid and valproic acid by 41, 29, 76 and 28%, respectively. DE decreased the plasma elimination of the parent compounds and the appearance of the conjugates in both plasma and bile. Reduction of glucuronide excretion into bile was less pronounced at higher doses of the cholephilic anions. Neither treatment reduced in vitro hepatic UDP-glucuronosyltransferase activity toward these substrates or substantially altered extrahepatic UDPGA concentrations. Thus, both GAL and DE decreased UDPGA to similar concentrations, but the biliary excretion of compounds requiring glucuronidation before secretion was depressed to a greater extent by GAL.

  6. Dehydroabietic acid

    Directory of Open Access Journals (Sweden)

    Xiao-Ping Rao

    2009-10-01

    Full Text Available The title compound [systematic name: (1R,4aS,10aR-7-isopropyl-1,4a-dimethyl-1,2,3,4,4a,9,10,10a-octahydrophenanthrene-1-carboxylic acid], C20H28O2, has been isolated from disproportionated rosin which is obtained by isomerizing gum rosin with a Pd-C catalyst.. Two crystallographically independent molecules exist in the asymmetric unit. In each molecule, there are three six-membered rings, which adopt planar, half-chair and chair conformations. The two cyclohexane rings form a trans ring junction with the two methyl groups in axial positions. The crystal structure is stabilized by intermolecular O—H...O hydrogen bonds.

  7. 胺鲜酯和镉对蓖麻幼苗光合生理特性的影响%RESPONSES OF PHOTOSYNTHETIC TRAITS OF CASTOR BEAN SEEDLINGS TO CADMIUM AND DIETHYL AMINOETHYL HEXANOATE

    Institute of Scientific and Technical Information of China (English)

    张铮; 钱宝云; 程晓庆; 刘彩凤; 史刚荣

    2011-01-01

    To determine whether diethyl aminoethyl hexanoate ( DA-6 ) pretreatment alleviated the cadmium ( Cd) toxicity to castor bean ( Ricinus communis L. ) seedlings, tffects of Cd (0, 50μmol · L-1 CdCl2 ) and DA-6 (0 , 0. 1, 10 and lOOOmg · L-1 ) , and their interactions on plant growth and photosynthesis were investigated. Results showed that 50 ixmol · L-1 CdCl2 inhibited plant growth and photosynthesis of castor seedlings. Under Cd exposure, the net photosynthetic rate (Pn) , stomatal conductance (Gs) and transpiration rate (E) , photosynthetic pigment contents (Chi a, Chi b, Chi a + b, Car and Chi /Car) and chlorophyll fluorescence parameters (Fm, Fv/Fm, Fv/Foand ⅡPS Ⅱ) decreased, whereas the intercellular CO2 concentration (Ci) , Chi a/b and Fo increased. Presoaking seeds with different concentrations of DA-6 did not change the plant growth regardless of Cd. In the absence of Cd, DA-6 pretreatment significantly enhanced the pigment contents (Chi a, Chi b, Chi a + b and Car) in castor leaves, while the ratio of pigment content ( Chi a/b, Chi/Car) , chlorophyll fluorescence parameters, and gas exchange parameters remained unaffected. In the present of Cd, presoaking seeds with 10 and lOOOmg · L-1 DA-6 caused a reduction in pigment contents (Chi a, Chi b, Chi a + b and Car) , gas exchange parameters (Pn, E and Gs) , as well as chlorophyllfluorescence parameters (Fm, Fv/Fm, Fv/Foand ΦPS Ⅱ) in castor seedlings. It was indicated that DA-6 presoaking might aggravate, rather than alleviate, the inhibition of Cd on photosynthesis of castor bean seedlings.%以蓖麻(Ricinus communis L.)为研究对象,通过水培试验研究胺鲜酯(DA-6)和镉(Cd)对蓖麻生长和光合生理特性的交互作用,探讨DA-6浸种对植物Cd毒害是否具有缓解作用.研究结果表明,50μmol·L-1CdCl2对蓖麻幼苗生长和光合作用具有抑制作用.Cd处理显著降低蓖麻叶片的光合速率(Pn)、气孔导度(Gs)和蒸腾速率(E),而胞间CO2浓度(Ci)则明

  8. Electroencephalographic studies on the development of tolerance and cross tolerance to mescaline in the rat.

    Science.gov (United States)

    Colasanti, B; Khazan, N

    1975-09-17

    Recordings of the electroencephalogram (EEG) and the electromyogram (EMG) were collected continuously from rats equipped with permanent cortical and temporalis muscle electrodes. Automatic injections of mescaline were administered through indwelling i.p. cannulas at an initial dose of 30 mg/kg every 6 hrs for the first 2 days. This dose was then increased to 60 mg/kg 6 hr which was given for the duration of the study. The initial injections of the mescaline induced an immediate desynchronization of the EEG and behavioral arousal of the rat, which endured for 2-3 hrs. After this time, slow wave (SW) sleep and rapid eye movement (REM) sleep episodes reappeared, with the return of regular alternations of the sleep-wakefulness cycle. Upon continued administration of the drug, partial tolerance to the arousal effects of mescaline developed, which was reflected by a gradual reduction in the latencies to onset of SW sleep and REM sleep. Rats rendered tolerant to mescaline in this manner were found to be cross tolerant to lysergic acid diethylamide (LSD) and N,N-diethyl-tryptamine (DET). In contrast, cross tolerance did not occur to amphetamine, which exerts similar arousal and EEG desynchronizing effects. These results agree with physiological and behavioral studies of tolerance and cross tolerance among hallucinogens and support the usefulness of the EEG as a quantitative indicator of central nervous system function.

  9. 利用气相色谱-质谱联用技术测定燕麦中脂肪酸的组成%Determination of fatty acids in oats by gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    李金玉

    2011-01-01

    Anhydrous diethyl ether-petroleum ether solvents, Soxhlet extraction lift crude fat oats, after KOH-methanol methyl ester with n-hexane extraction and determination of fatty acid methyl esters by GC-MS analysis identified 15 types of fatty acids, and determination of the relative concentration of fatty acids, and unsaturated fatty acid content of about 79.45%, to oleic acid, linoleic acid and linolenic acid mainly.%以无水乙醚-石油醚为溶剂,用索氏抽提法提取燕麦中粗脂肪,经KOH-甲醇进行甲酯化后以正已烷萃取,用气相色谱-质谱测定脂肪酸甲酯,分析鉴定出15种脂肪酸,并测定出各脂肪酸的相对含量,其中不饱和脂肪酸相对含量约占79.45%,以油酸、亚油酸、亚麻酸为主.

  10. Synthesis and NMR Elucidation of Novel Octa-Amino Acid Resorcin[4

    African Journals Online (AJOL)

    NICO

    involves alkylation of compound 1 with methyl-2-bromoacetate ... catalytic amount of sodium iodide. The reaction ... fied on silica gel chromatography, using 3 % methanol in chloro- ... rate of interconversion. ..... twice with diethyl ether (50 mL).

  11. [Determination of phthalic acid esters in textiles by solid phase extraction-gas chromatography].

    Science.gov (United States)

    Niu, Zengyuan; Ye, Xiwen; Fang, Liping; Xue, Qiuhong; Sun, Zhongsong

    2006-09-01

    A method was established for the simultaneous determination of some phthalic acid esters, namely, dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPrP), dibutyl phthalate (DBP), diamyl phthalate (DAP), dihexyl phthalate (DHP), benzyln-butyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), dicyclohexyl phthalate (DCHP), di-n-octyl phthalate (DNOP), diisononyl phthalate (DINP) and diisodecyl phthalate (DIDP) in textiles by solid phase extraction (SPE) coupled with gas chromatography (GC). The phthalic acid esters in textiles were extracted by Soxhlet extraction with hexane, the extracts were then cleaned up and enriched by a strong anion exchange (SAX) SPE cartridge. The parameters affecting the purification efficiency of SPE cartridge, such as solvent conditioning, rinsing, and elution, were studied. Conditioning with 5 mL hexane and rinsing with 3 mL isooctane were proved to be the optimal conditions. Of the several solvent ratios (ethylacetate in hexane) used for selective elution of phthalic acid esters from the SAX SPE cartridge, the 15% (v/v) content for ethylacetate in hexane gave the best result. Under the optimized conditions, the recoveries of phthalic acid esters for spiked standards (n=7) were 86.3%-102.7%, and the relative standard deviations (RSDs) were less than 5%. In this method the detection limits for DMP, DEP, DPrP, DBP, DAP, BBP, DCHP, DEHP, DNOP were all below 1 mg/kg, and the detection limits for DINP and DIDP were 1.74 mg/kg and 1.55 mg/kg respectively. This SPE-GC method is sensitive, accurate and suitable for the analysis of phthalate environmental hormones in textiles.

  12. Synthesis and characterization of 5-(4-hydroxy-3-methoxy-phenyl-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidine-2,6-dicarboxylic acid 2-ethyl ester 6-methyl ester and its 6-ethyl ester 5-naphthalene derivative

    Directory of Open Access Journals (Sweden)

    H. Nagarajaiah

    2015-11-01

    Full Text Available The compounds 5-(4-hydroxy-3-methoxy-phenyl-3,7-dimethyl-5H-thiazolo[3,2-a]pyrimidine-2,6-dicarboxylic acid 2-ethyl ester 6-methyl ester (2a and 3,7-dimethyl-5-naphthalen-1-yl-5H-thiazolo[3,2-a]pyrimidine-2,6-dicarboxylic acid diethyl ester (2b were synthesized by the base catalyzed cyclocondensation of 3,4-dihydropyrimidine-2-thione with ethylacetoacetate. IR, 1H NMR, 13C NMR spectra and elemental analysis were used to characterize these compounds. The structures were determined by single crystal X-ray diffraction. The crystal structure is stabilized by intermolecular O–H…N, C–H…O, C–H…π and π…π weak interactions.

  13. Amino acids in the sedimentary humic and fulvic acids

    Digital Repository Service at National Institute of Oceanography (India)

    Sardessai, S.

    to the coastal sedimentary humic acids implying higher association of amino acids with the carbonaceous and fine grained sedimentary humic acids. Both the humic and fulvic acids are composed of neutral, acidic, basic, aromatic and sulphur containing amino acids....

  14. Inhibition of hypoxia-inducible factor (HIF) hydroxylases by citric acid cycle intermediates: possible links between cell metabolism and stabilization of HIF.

    Science.gov (United States)

    Koivunen, Peppi; Hirsilä, Maija; Remes, Anne M; Hassinen, Ilmo E; Kivirikko, Kari I; Myllyharju, Johanna

    2007-02-16

    The stability and transcriptional activity of the hypoxia-inducible factors (HIFs) are regulated by two oxygen-dependent events that are catalyzed by three HIF prolyl 4-hydroxylases (HIF-P4Hs) and one HIF asparaginyl hydroxylase (FIH). We have studied possible links between metabolic pathways and HIF hydroxylases by analyzing the abilities of citric acid cycle intermediates to inhibit purified human HIF-P4Hs and FIH. Fumarate and succinate were identified as in vitro inhibitors of all three HIF-P4Hs, fumarate having K(i) values of 50-80 microM and succinate 350-460 microM, whereas neither inhibited FIH. Oxaloacetate was an additional inhibitor of all three HIF-P4Hs with K(i) values of 400-1000 microM and citrate of HIF-P4H-3, citrate being the most effective inhibitor of FIH with a K(i) of 110 microM. Culturing of cells with fumarate diethyl or dimethyl ester, or a high concentration of monoethyl ester, stabilized HIF-1alpha and increased production of vascular endothelial growth factor and erythropoietin. Similar, although much smaller, changes were found in cultured fibroblasts from a patient with fumarate hydratase (FH) deficiency and upon silencing FH using small interfering RNA. No such effects were seen upon culturing of cells with succinate diethyl or dimethyl ester. As FIH was not inhibited by fumarate, our data indicate that the transcriptional activity of HIF is quite high even when binding of the coactivator p300 is prevented. Our data also support recent suggestions that the increased fumarate and succinate levels present in the FH and succinate dehydrogenase-deficient tumors, respectively, can inhibit the HIF-P4Hs with consequent stabilization of HIF-alphas and effects on tumor pathology.

  15. [Teichoic acids from lactic acid bacteria].

    Science.gov (United States)

    Livins'ka, O P; Harmasheva, I L; Kovalenko, N K

    2012-01-01

    The current view of the structural diversity of teichoic acids and their involvement in the biological activity of lactobacilli has been reviewed. The mechanisms of effects of probiotic lactic acid bacteria, in particular adhesive and immunostimulating functions have been described. The prospects of the use of structure data of teichoic acid in the assessment of intraspecific diversity of lactic acid bacteria have been also reflected.

  16. Plasma amino acids

    Science.gov (United States)

    Amino acids blood test ... types of methods used to determine the individual amino acid levels in the blood. ... test is done to measure the level of amino acids in the blood. An increased level of a ...

  17. Uric acid test (image)

    Science.gov (United States)

    Uric acid urine test is performed to check for the amount of uric acid in urine. Urine is collected over a 24 ... testing. The most common reason for measuring uric acid levels is in the diagnosis or treatment of ...

  18. POLYELEOSTEARIC ACID VESICLES

    Institute of Scientific and Technical Information of China (English)

    LI Zichen; XIE Ximng; FAN Qinghua; FANG Yifei

    1992-01-01

    α-Eleostearic acid and β-eleostearic acid formed vesicles in aqueous medium when an ethanol solutionofeleostearic acid was injected rapidly into a vigorously vortexed aqueous phase. Formation of the vesicles was demonstrated by electron microscopic observation and bromothymol blue encapsulation experiments. Polymerizations of the eleostearic acids in the formed vesicles carried out by UV irradiation produced poly-α-eleostearic acid and poly-β-eleostearic acid vesicles.

  19. Acid distribution in phosphoric acid fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Okae, I.; Seya, A.; Umemoto, M. [Fuji Electric Co., Ltd., Chiba (Japan)

    1996-12-31

    Electrolyte acid distribution among each component of a cell is determined by capillary force when the cell is not in operation, but the distribution under the current load conditions had not been clear so far. Since the loss of electrolyte acid during operation is inevitable, it is necessary to store enough amount of acid in every cell. But it must be under the level of which the acid disturbs the diffusion of reactive gases. Accordingly to know the actual acid distribution during operation in a cell is very important. In this report, we carried out experiments to clarify the distribution using small single cells.

  20. Metabolism and metabolic inhibition of gamboglc acid in rat liver microsomes

    Institute of Scientific and Technical Information of China (English)

    Yi-tong LIU; Kun HAO; Xiao-quan LIU; Guang-Ji WANG

    2006-01-01

    Aim: To study the metabolism of gambogic acid (GA) and the effects of selective cytochrome P-450 (CYP450) inhibitors on the metabolism of GA in rat liver microsomes in vitro. Methods: Rat liver micrp,so,rn,e$ were used to perform metabolism studies. Various selective CYP450 inhibitors were used to investigate their effects on the metabolism of GA and the principal CYP450 isoform involved in the formation of major metabolite M1 in rat liver microsomes. Types of inhibition in an enzyme kinetics model were used to model the interaction. Results: GA was rapidly metabolized to two phase Ⅰ metabolites,, M1 and M2, in rat liver microsomes. M1 and M2 were tentatively presumed to be the hydration metabolite and epoxide metabolite of GA, respectively. α-Naphthoflavone uncompetitively inhibited the formation of M1 while ketoconazole, sulfophenazole, diethyl dithiocarbamate and quinidine had little or no inhibitory effects on the formation of M1. Conclusion: GA is rapidly metabolized in rat liver microsomes and M1 is crucial for the elimination of GA. Cytochrome P-450 1A2 is the major rat CYP involved in the metabolism of GA.

  1. Enzymatic hydrolysis of structurally diverse phthalic acid esters by porcine and bovine pancreatic cholesterol esterases.

    Science.gov (United States)

    Saito, Takao; Hong, Peng; Tanabe, Rima; Nagai, Kazuo; Kato, Katsuya

    2010-12-01

    A weak hydrolyzing activity against bis (2-ethylhexyl) phthalate (DEHP) was discovered in a commercial crude lipase (EC 3.1.1.3) preparation from porcine pancreas. DEHP was hydrolyzed to mono (2-ethylhexyl) phthalate (MEHP) not by a pancreatic lipase but by a cholesterol esterase (CEase, EC 3.1.1.13), a trace contaminant in the crude lipase preparation. Enzymatic hydrolysis of phthalic acid esters (PAEs), suspected to be endocrine-disrupting chemicals, was investigated using CEases from two species of mammals and a microorganism. Eight structurally diverse PAEs, namely diethyl phthalate (DEP), di-n-propyl phthalate (DPrP), di-n-butyl phthalate (DBP), di-n-pentyl phthalate (DPeP), di-n-hexyl phthalate (DHP), DEHP, n-butyl benzyl phthalate (BBP), and dicyclohexyl phthalate (DCHP), were hydrolyzed to their corresponding monoesters by both porcine and bovine pancreatic CEases, while a microbial CEase from Pseudomonas sp. had no hydrolyzing activity against these PAEs. The hydrolysis experiments with bovine pancreatic CEase (50 U) indicated complete hydrolysis of every PAE (5 μmole) except for BBP and DCHP within 15 min; BBP and DCHP were hydrolyzed within 30 min and 6h, respectively. The rates of PAE hydrolysis could be affected by the bulkiness of alkyl side chains in the PAEs. This study provides important evidence that mammalian pancreatic CEases, such as those from porcine and bovine sources, are potential enzymes for nonspecific degradation of structurally diverse PAEs.

  2. Coaxially Aligned Polyaniline Nanofibers Doped with 3-Thiopheneacetic Acid through Interfacial Polymerization

    Directory of Open Access Journals (Sweden)

    Lixia Zhang

    2011-01-01

    Full Text Available Coaxially aligned polyaniline (PANI nanofibers doped with 3-thiopheneacetic acid (TAA were chemically synthesized by the interfacial polymerization of aniline in the presence of TAA, using iron (III chloride hexahydrate (FeCl3·6H2O as the oxidant. The morphology, crystallinity, room temperature conductivity, and coaxial alignment of the PANI-TAA nanofibers were highly dependent on the organic solvent used for the interfacial polymerization, the oxidant, and also the molar ratio of the aniline to TAA. Hexane, diethyl ether, dichloromethane, chloroform, and acetone were used as the organic solvents, and chloroform proved to be the best solvent for the formation of PANI-TAA nanofibers. The redox potential of the oxidant is the key to controlling the morphology and diameter of the PANI-TAA nanofibers. The use of FeCl3 as the oxidant leads to the formation of thin (∼50 nm PANI-TAA nanofibers, which increased in length, crystallinity, conductivity, and coaxial alignment as the molar ratio of TAA to aniline was increased from 0.1 : 1 to 1 : 1. By comparison, only granular PANI was obtained when ammonium persulfate (APS, which has a higher redox potential, was used as the oxidant. The doping function of TAA in the PANI-TAA nanofibers was confirmed by means of FTIR and UV-Visible spectroscopy.

  3. Performance, kinetic, and biodegradation pathway evaluation of anaerobic fixed film fixed bed reactor in removing phthalic acid esters from wastewater

    Science.gov (United States)

    Ahmadi, Ehsan; Yousefzadeh, Samira; Ansari, Mohsen; Ghaffari, Hamid Reza; Azari, Ali; Miri, Mohammad; Mesdaghinia, Alireza; Nabizadeh, Ramin; Kakavandi, Babak; Ahmadi, Peyman; Badi, Mojtaba Yegane; Gholami, Mitra; Sharafi, Kiomars; Karimaei, Mostafa; Ghoochani, Mahboobeh; Brahmand, Masoud Binesh; Mohseni, Seyed Mohsen; Sarkhosh, Maryam; Rezaei, Soheila; Asgharnia, Hosseinali; Dehghanifard, Emad; Jafari, Behdad; Mortezapour, Alireza; Moghaddam, Vahid Kazemi; Mahmoudi, Mohammad Molla; Taghipour, Nader

    2017-02-01

    Emerging and hazardous environmental pollutants like phthalic acid esters (PAEs) are one of the recent concerns worldwide. PAEs are considered to have diverse endocrine disrupting effects on human health. Industrial wastewater has been reported as an important environment with high concentrations of PAEs. In the present study, four short-chain PAEs including diallyl phthalate (DAP), diethyl phthalate (DEP), dimethyl phthalate (DMP), and phthalic acid (PA) were selected as a substrate for anaerobic fixed film fixed bed reactor (AnFFFBR). The process performances of AnFFFBR, and also its kinetic behavior, were evaluated to find the best eco-friendly phthalate from the biodegradability point of view. According to the results and kinetic coefficients, removing and mineralizing of DMP occurred at a higher rate than other phthalates. In optimum conditions 92.5, 84.41, and 80.39% of DMP, COD, and TOC were removed. DAP was found as the most bio-refractory phthalate. The second-order (Grau) model was selected as the best model for describing phthalates removal.

  4. Performance, kinetic, and biodegradation pathway evaluation of anaerobic fixed film fixed bed reactor in removing phthalic acid esters from wastewater

    Science.gov (United States)

    Ahmadi, Ehsan; Yousefzadeh, Samira; Ansari, Mohsen; Ghaffari, Hamid Reza; Azari, Ali; Miri, Mohammad; Mesdaghinia, Alireza; Nabizadeh, Ramin; Kakavandi, Babak; Ahmadi, Peyman; Badi, Mojtaba Yegane; Gholami, Mitra; Sharafi, Kiomars; Karimaei, Mostafa; Ghoochani, Mahboobeh; Brahmand, Masoud Binesh; Mohseni, Seyed Mohsen; Sarkhosh, Maryam; Rezaei, Soheila; Asgharnia, Hosseinali; Dehghanifard, Emad; Jafari, Behdad; Mortezapour, Alireza; Moghaddam, Vahid Kazemi; Mahmoudi, Mohammad Molla; Taghipour, Nader

    2017-01-01

    Emerging and hazardous environmental pollutants like phthalic acid esters (PAEs) are one of the recent concerns worldwide. PAEs are considered to have diverse endocrine disrupting effects on human health. Industrial wastewater has been reported as an important environment with high concentrations of PAEs. In the present study, four short-chain PAEs including diallyl phthalate (DAP), diethyl phthalate (DEP), dimethyl phthalate (DMP), and phthalic acid (PA) were selected as a substrate for anaerobic fixed film fixed bed reactor (AnFFFBR). The process performances of AnFFFBR, and also its kinetic behavior, were evaluated to find the best eco-friendly phthalate from the biodegradability point of view. According to the results and kinetic coefficients, removing and mineralizing of DMP occurred at a higher rate than other phthalates. In optimum conditions 92.5, 84.41, and 80.39% of DMP, COD, and TOC were removed. DAP was found as the most bio-refractory phthalate. The second-order (Grau) model was selected as the best model for describing phthalates removal. PMID:28216654

  5. 2-吲哚乙酸乙酯的合成%Synthesis of 2-indoleacetic Acid Ethyl Ester

    Institute of Scientific and Technical Information of China (English)

    陈芬; 覃宇

    2015-01-01

    丙二酸二乙酯在醇溶液中,与氢氧化钾皂化得到丙二酸单乙酯钾盐,然后在N, N'-羰基二咪唑(CDI)作用下,与2-硝基苯乙酸进行亲核加成得到4-(2-硝基苯基)-乙酰乙酸乙酯,再经三氯化钛的催化还原环化制得医药中间体2-吲哚乙酸乙酯,收率达72.2%。%2- indole acetic acid ethyl ester, the important drug intermediate, was synthesized from diethyl malonate by saponification reaction with potassium hydroxide in the presence of alcohol solution to give ethyl malonate potassium salt and nucleophilic addition with 2-nitrophenyl acetic acid to give 4-(2-nitrophenyl)-ethylacetoacetate using N,N'-carbonyldiimidazole(CDI), and then reduct cyclization reaction upon the catalysis of titanium trichloride with an overall yield of about 72.2%.

  6. Assessing human exposure to phthalic acid and phthalate esters from mineral water stored in polyethylene terephthalate and glass bottles.

    Science.gov (United States)

    Montuori, P; Jover, E; Morgantini, M; Bayona, J M; Triassi, M

    2008-04-01

    Phthalic acid and phthalate esters are of growing interest due to their significant usage and potential toxicity. Polyethylene terephthalate (PET) and glass are both widely used materials for bottled drinking water. In this study, phthalic acid (PhA), bis(2-ethylhexyl) phthalate (DEHP), dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DiisoBP) and dibutyl phthalate (DBP) were analysed in a large number of Italian bottled water samples. These samples showed different concentrations of phthalates are nearly 20 times higher in samples bottled in PET than those from glass bottles with total levels of phthalates of 3.52 and 0.19 microg l(-1), respectively. However, the observed levels do not represent a significant exposure pathway when considering the US Environmental Protection Agency (USEPA) reference dose (an estimate of a daily oral exposure to the human population, including sensitive subgroups, that is likely to be without an appreciable risk of deleterious effects during a lifetime). In addition, no significant correlation was found between the phthalate concentrations and the physicochemical properties of the different water samples, apart from the still/sparkling water parameter for the PET samples. In this instance, slightly higher concentrations were observed for the PET bottled still water samples than for the sparkling water samples, although no explanation has been found yet.

  7. Synthesis of the enantiomers of diethyl 2,3-diisopropylsuccinate and the application of them in polypropylene catalyst%琥珀酸酯对映异构体的合成及其用于丙烯聚合催化剂

    Institute of Scientific and Technical Information of China (English)

    张锐; 周奇龙; 宋维玮; 谭忠

    2013-01-01

    The different enantiomers of diethyl 2,3-diisopropylsuccinate (DISE) were prepared and used as internal donors in the polypropylene catalyst.It has been proved in this work that only the Di-D-menthyl-(+)-2,3-diisopropylsuccinate synthesized by D-menthol could be purified through crystallization,which is the key point in the preparation of the corresponding diethyl (+)-2,3-diisopropylsuccinate.The affects of the different enantiomers of DISE as the internal donor on the polypropylene catalyst were also studied.The results showed that both of the enantiomers of DISE could endow the catalyst with the excellecent performance and showed no significant differences in spite of the different molecular conformation.%合成了具有不同旋光性的2,3-二异丙基琥珀酸二乙酯(DISE)对映异构体并作为内给电子体用于丙烯聚合催化剂.本工作发现,只有使用D-薄荷醇制备的R,R构型的(+)-2,3-二异丙基琥珀酸二-D-薄荷醇酯才能够通过结晶分离得到纯品,这也是进一步制备相应的(+)-2,3-二异丙基琥珀酸二乙酯的关键所在.本工作还研究了不同旋光性的2,3-二异丙基琥珀酸二乙酯作为内给电子体对丙烯聚合催化剂性能的影响.实验结果表明,尽管两种对映异构体分子构型不同,但其作为内给电子体的性能没有显著的差别,并且都能够赋予催化剂很好的聚合性能.

  8. Di-μ-acetato-bis-(dimethyl-formamide)-penta-kis-(μ-N,2-dioxidobenzene-1-car-boximidato)tetra-kis-(1-ethyl-imidazole)-penta-manganese(III)-manganese(II)-diethyl ether-dimethyl-foramide-methanol-water (1/1/1/1/0.12).

    Science.gov (United States)

    Tigyer, Benjamin R; Zeller, Matthias; Zaleski, Curtis M

    2011-08-01

    The title compound [Mn(6)(C(7)H(4)NO(3))(5)(CH(3)CO(2))(2)(C(5)H(8)N(2))(4)(C(3)H(7)NO)(2)]·(C(2)H(5))(2)O·C(3)H(7)NO·CH(3)OH·0.12H(2)O, abbreviated as Mn(II)(OAc)(2)[15-MC(MnIII(N)shi)-5](EtIm)4(DMF)2·diethyl ether·DMF·MeOH·0.12H(2)O (where (-)OAc is acetate, MC is metallacrown, shi(3-) is salicylhydroximate, EtIM is n-ethylimidazole, DMF is N,N-dimethylformamide, and MeOH is methanol) contains five Mn(III) ions as members of the metallacrown ring and an Mn(II) ion bound in the central cavity. The central Mn(II) ion is seven-coordinate with a distorted face-capped trigonal-prismatic geometry. The five Mn(III) ions of the metallacrown ring are six-coordinate with distorted octa-hedral geometries. The configuration of the Mn(III) ions about the metallacrown ring follow a ΔΛΔPP pattern, with P representing planar. The four 1-ethyl-imidazole ligands are bound to four different Mn(III) ions. A diethyl ether solvent mol-ecule was found to be disordered over two mutually exclusive sites with an occupancy ratio of 0.568 (7):0.432 (7). A methanol solvent mol-ecule was found to be disordered over two mutually exclusive sites by being hydrogen bonded either to a dimethyl-formamide solvent mol-ecule (major occupancy component) or to an O atom of the main mol-ecule (minor occupancy component). The occupancy ratio refined to 0.678 (11):0.322 (11). Associated with the minor component is a partially occupied water mol-ecule [total occupancy 0.124 (15)].

  9. Dolomite flotation of high magnesium phosphate ores using fatty acid soap collectors

    Science.gov (United States)

    Gu, Zhengxing

    The separation of dolomite from apatite has been recognized as one of the most difficult subjects in mineral processing due to the similarities in their physiochemical properties. In this study, selective surfactants were used with a fatty acid soap collector to improve the flotation performance of separating dolomite from high magnesium phosphate ores. Three surfactants, diethyl phthalate (DP), Tween-80 (TW) and derivative of sulfonate salt (DSS1) were used. Hallimond cell flotation was conducted using pure dolomite sample to determine the effects of various factors including dosages, particle size, Ca2+ ions and slimes on the dolomite flotation recovery. The results showed that the surfactants can significantly improve dolomite flotation performance by increasing collecting ability and tolerating the effect of calcium ions and slime contents. The stirrer-tank cell batch flotation tests were carried out using two natural high magnesium phosphate ore samples containing 3.3% and 1.5% MgO. The test results showed that the surfactant DP could improve dolomite flotation at low dosages, and DSS1 could enhance the separation of dolomite from phosphate by improving both collecting ability and flotation selectivity. When 10% of DSS1 was used with the fatty acid soap as collector, at least 10% more dolomite can be removed with less P2O5 loss. The effectiveness of the surfactant DSS1 in enhancing dolomite flotation was further demonstrated in modified packed column flotation with natural dolomitic phosphate ore sample. The addition of the surfactant DSS1 into fatty acid soap collector could improve its frothability and froth stability, and reduce the bubble size. It has been found that the dolomite flotation performance has a close relationship with the frothability and froth stability of the collector.

  10. Synthesis of pyrophosphonic acid analogues of farnesyl pyrophosphate

    NARCIS (Netherlands)

    Valentijn, A.R.P.M.; Berg, O. van den; Marel, G.A. van der; Cohen, L.H.; Boom, J.H. van

    1995-01-01

    The synthesis of four new analogues (i.e. 3-6) of farnesyl pyrophosphate (FPP), which may function as inhibitor of squalene synthase, is described. Compounds 3 and 4 were readily accessible by reaction of farnesal with diethyl phosphite or dimethyl lithiomethylphosphonate, respectively, followed by

  11. METAL COMPLEXES OF SALICYLHYDROXAMIC ACID AND 1,10 ...

    African Journals Online (AJOL)

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    After standing at room temperature for several hours this was suction filtered, washed ... diethyl ether and dried in a vacuum desiccator over P2O5. .... active centers of the cell constituents, resulting in interference with the normal cell process ...

  12. Synthesis of pyrophosphonic acid analogues of farnesyl pyrophosphate

    NARCIS (Netherlands)

    Valentijn, A.R.P.M.; Berg, O. van den; Marel, G.A. van der; Cohen, L.H.; Boom, J.H. van

    1995-01-01

    The synthesis of four new analogues (i.e. 3-6) of farnesyl pyrophosphate (FPP), which may function as inhibitor of squalene synthase, is described. Compounds 3 and 4 were readily accessible by reaction of farnesal with diethyl phosphite or dimethyl lithiomethylphosphonate, respectively, followed by

  13. 新型双核阳离子离子液体催化合成庚二酸二乙酯%SYNTHESIS OF DIETHYL PIMELATE BY A NEW IONIC LIQUID WITH BINUCLEAR CATIONS

    Institute of Scientific and Technical Information of China (English)

    赵振贵; 李华; 赵蕾

    2011-01-01

    A new ionic liquid with strong acid binuclear cations, namely, N, N'-alkyl-(3-methyl)-diimidazolium hydrogen sulfate, is used for the esterification of 1,7-pimelic acid and ethanol.The products and ionic liquids can be separated by simple methods.The esterification products could be easily separated in high yield from the reaction system via simple phase separation.The effects of the reaction conditions on the reaction results, such as the amount of catalyst, molar ratio of acid and alcohol, reaction time, etc, were examined and the optimal, conditions were obtained through orthogonally designed experiments based on single-factor experiments.The optimal conditions were found as follows: n(C2H5OH)∶ n(C7H1204)=3∶ 1, 11.1% catalyst , 5.5 h and 108 ℃.Under the optimal reaction conditions, the yield was 97.81%.Separated from the products, the ionic liquids could be reused for 5 times and the yields were up to 96.65%.Compared with the concentrated sulfuric acid, the traditional catalyst, the ionic liquids have the advantages of excellent stability, less pollution, less side reaction, good repeatability, and no organic solvent being required as water carrying agent.%制备一种新型强酸性双核阳离子离子液体N,N'-烷基-(3-甲基)-二咪唑硫酸氢盐,用于1,7-庚二酸和乙醇的酯化反应,通过简单的处理就可以实现产品和离子液体的分离.采用单因素和正交实验考察了催化剂用量、反应时间、反应温度和醇酸比对反应的影响,最佳反应条件为:n(CHOH):n(CHO)=3:1、催化剂用量11.1%、反应时间5.5 h、反应温度108℃,庚二酸二乙酯收率为97.81%.离子液体重复使用 5 次,庚二酸二乙酯的收率均在96.65%以上.

  14. Gas-phase Acidities of Aspartic Acid, Glutamic Acid, and their Amino Acid Amides.

    Energy Technology Data Exchange (ETDEWEB)

    Li, Zhong; Matus, Myrna H; Velazquez, Hector A; Dixon, David A; Cassady, Carolyn J

    2007-02-14

    Gas-phase acidities (GA or ΔGacid) for the two most acidic common amino acids, aspartic acid and glutamic acid, have been determined for the first time. Because of the amide linkage’s importance in peptides and as an aid in studying side chain versus main chain deprotonation, aspartic acid amide and glutamic acid amide were also studied. Experimental GA values were measured by proton transfer reactions in an electrospray ionization/Fourier transform ion cyclotron resonance mass spectrometer. Calculated GAs were obtained by density functional and molecular orbital theory approaches. The best agreement with experiment was found at the G3MP2 level; the MP2/CBS and B3LYP/aug-cc-pVDZ results are 3–4 kcal/mol more acidic than the G3MP2 results. Experiment shows that aspartic acid is more acidic than glutamic acid by ca. 3 kcal/mol whereas the G3MP2 results show a smaller acidity difference of 0.2 kcal/mol. Similarly, aspartic acid amide is experimentally observed to be ca. 2 kcal/mol more acidic than glutamic acid amide whereas the G3MP2 results show a correspondingly smaller energy difference of 0.7 kcal/mol. The computational results clearly show that the anions are all ring-like structures with strong hydrogen bonds between the OH or NH2 groups and the CO2- group from which the proton is removed. The two amino acids are main-chain deprotonated. In addition, use of the COSMO model for the prediction of the free energy differences in aqueous solution gave values in excellent agreement with the most recent experimental values for pKa. Glutamic acid is predicted to be more acidic than aspartic acid in aqueous solution due to differential solvation effects.

  15. A dual-template imprinted polymer-modified carbon ceramic electrode for ultra trace simultaneous analysis of ascorbic acid and dopamine.

    Science.gov (United States)

    Bali Prasad, Bhim; Jauhari, Darshika; Tiwari, Mahavir Prasad

    2013-12-15

    A dual-template imprinted polymer film containing dispersed multiwalled carbon nanotubes was exploited in the fabrication of a typical, reproducible, and rugged carbon ceramic electrode, adopting "surface grafting from" approach for the growth of a nanometer thin coating on its surface. For this, chloro groups were first introduced at the exterior surface of silica-carbon composite electrode through sol-gel modification using (3-chloropropyl)-trimethoxysilane, followed by an iniferter (sodium diethyl dithiocarbamate) initiated photopolymerization of functional monomer (2,4,6-trisacrylamido-1,3,5-triazine), mixed templates (ascorbic acid and dopamine), and cross-linker (ethylene glycol dimethacrylate), in the presence of multiwalled carbon nanotubes. The modified sensor was validated for the simultaneous analysis of ascorbic acid and dopamine in aqueous, blood serum, cerebrospinal fluid, and pharmaceutical samples, using differential pulse anodic stripping voltammetric technique. The oxidation peak potentials for both analytes were found to be well apart approximately by 300 mV, which was large enough to allow selective and sensitive analysis of one in the presence of other, without any cross reactivity, interferences and false-positives. The detection limits realized by the proposed sensor, under optimized conditions, were found to be as low as 2.24 ng mL(-1) for ascorbic acid and 0.21 ng mL(-1) for dopamine (S/N=3). Such stringent limits could be considered suitable for the primitive diagnosis of several chronic diseases, in clinical settings.

  16. Influence of steric hindrance on enantioseparation of Dns-amino acids and pesticides on terguride based chiral selectors in capillary electrophoresis.

    Science.gov (United States)

    Honzátko, Ales; Cvak, Jan; Vaingátová, Silvie; Flieger, Miroslav

    2005-05-01

    Three urea derivatives of ergoline-based chiral selectors (CSs), differing in the size of the urea side chain, i.e. dimethyl- (CSI), diethyl- (CSII), and diisopropylurea (CSIII), were used to study the effect of steric hindrance on the enantioseparation of dansyl amino acids (Dns-AAs), pesticides, and mandelic acid under condition of capillary electrophoresis (CE) in linear polyacrylamide coated capillaries. A mixture of organic modifiers (MeOH/THF, 4:1 v/v) in a BGE consisting of 100 mM beta-alanine-acetate was used to increase the solubility of CSs up to 25 mM. The capillary was filled with CS (high UV absorption), and the inlet and outlet vials contained buffer solutions only. The best enantioseparation of Dns-AAs was achieved on CSI. Increased steric hindrance of the chiral binding site led to reduction of both enantioselectivity and resolution. The opposite pattern was observed for the separation of mandelic acid enantiomers, where the best enantioseparation and resolution was obtained with CSIII. Most of the pesticides studied reached maximum selectivity on the diethylurea ergoline derivative (CSII). Enantioseparation of fenoxaprop was found to be independent of steric hindrance.

  17. Gas-phase acidities of aspartic acid, glutamic acid, and their amino acid amides

    Science.gov (United States)

    Li, Zhong; Matus, Myrna H.; Velazquez, Hector Adam; Dixon, David A.; Cassady, Carolyn J.

    2007-09-01

    Gas-phase acidities (GA or [Delta]Gacid) for the two most acidic common amino acids, aspartic acid and glutamic acid, have been determined for the first time. Because of the amide linkage's importance in peptides and as an aid in studying side chain versus main chain deprotonation, aspartic acid amide and glutamic acid amide were also studied. Experimental GA values were measured by proton transfer reactions in an electrospray ionization/Fourier transform ion cyclotron resonance mass spectrometer. Calculated GAs were obtained by density functional and molecular orbital theory approaches. The best agreement with experiment was found at the G3MP2 level; the MP2/CBS and B3LYP/aug-cc-pVDZ results are 3-4 kcal/mol more acidic than the G3MP2 results. Experiment shows that aspartic acid is more acidic than glutamic acid by ca. 3 kcal/mol whereas the G3MP2 results show a smaller acidity difference of 0.2 kcal/mol. Similarly, aspartic acid amide is experimentally observed to be ca. 2 kcal/mol more acidic than glutamic acid amide whereas the G3MP2 results show a correspondingly smaller energy difference of 0.7 kcal/mol. The computational results clearly show that the anions are all ring-like structures with strong hydrogen bonds between the OH or NH2 groups and the CO2- group from which the proton is removed. The two amino acids are main-chain deprotonated. In addition, use of the COSMO model for the prediction of the free energy differences in aqueous solution gave values in excellent agreement with the most recent experimental values for pKa. Glutamic acid is predicted to be more acidic than aspartic acid in aqueous solution due to differential solvation effects.

  18. Synthesis, characterization and in silico designing of diethyl-3-methyl-5-(6-methyl-2-thioxo-4-phenyl-1,2,3,4-tetrahydropyrimidine-5-carboxamido) thiophene-2,4-dicarboxylate derivative as anti-proliferative and anti-microbial agents.

    Science.gov (United States)

    Malani, Kalpesh; Thakkar, Sampark S; Thakur, Mukund Chandra; Ray, Arabinda; Doshi, Hiren

    2016-10-01

    A series of eight compounds diethyl-3-methyl-5-(6-methyl-2-thioxo-4-phenyl-1,2,3,4-tetrahydropyrimidine-5-carboxamido) thiophene-2,4-dicarboxilate (KM10-17) analogues have been prepared by conventional methods and characterized by IR, Mass, NMR and elemental analysis. In silico docking studies on Human topoisomerase IIbeta (PDB Id: 3QX3) have been performed for all molecules (KM10-17) synthesized. The compounds were tested for in vitro anti-proliferative activity on VERO and 786-O cell lines. Out of all the synthesized compounds, KM11 &KM16 showed moderate activity on both cell lines. In vitro anti-microbial activity was also checked against Bacillus subtilis (BS), Staphylococcus aurous (SA), Pseudomonas aeruginosa (PA), Escherichia coli (EC) and Candida albicans (CA) by well diffusion method. The compound KM11 was found to have highest zone of inhibition against BS, SA, PA and EC. The molecules KM13 and KM16 exhibited good activity against CA. The compounds KM14 and KM16 indicated good zone of inhibition against BS.

  19. Di-μ-chlorido-bis({4-[bis(trimethylsilylamino]-6-chloro-2,2,8,8-tetramethyl-5,7-bis(trimethylsilyl-3,5,7-triaza-4,6-diphospha-2,8-disilanon-3-en-4-ido-κ2P,P′}palladium(II diethyl ether disolvate

    Directory of Open Access Journals (Sweden)

    Martha Höhne

    2016-06-01

    Full Text Available The title compound, [Pd2(C18H54Cl2N4P2Si62Cl2]·2C4H10O, features a dinuclear chloride-bridged palladium complex bearing two equivalents of the novel monoanionic mixed valent (λ3-P—N—(λ5-P ligand. A metal catalyzed coupling of two aminoiminophosphines and a shift of one chlorine from the metal to the phosphorus results in the (λ3-P—N—(λ5-P ligand. The molecule contains a planar bimetallic Pd2Cl2 core with a crystallographic centre of inversion at the mid-point of the Pd...Pd line. The Pd atoms are in a distorted square-planar arrangement, where the P/Pd/P and Cl/Pd/Cl planes are twisted with respect to each other by a dihedral angle of 7.57 (4°. The P—Pd—P bite angle is 71.380 (18°. Intramolecular C—H...Cl interactions are observed. In the crystal, the diethyl ether solvent molecule is disordered over two sites, with an occupancy ratio of 0.788 (5:0.212 (5.

  20. Toxicity of adipic acid.

    Science.gov (United States)

    Kennedy, Gerald L

    2002-05-01

    Adipic acid has very low acute toxicity in rats with an LD50 > 5000 mg/kg. Adipic acid produced mild to no skin irritation on intact guinea pig skin as a 50% concentration in propylene glycol; it was not a skin sensitizer. Adipic acid caused mild conjunctival irritation in washed rabbit eyes; in unwashed rabbit eyes, there was mild conjunctival irritation, minimal iritis, but no corneal effects. Adipic acid dust may irritate the mucous membranes of the lungs and nose. In a 2-year feeding study, rats fed adipic acid at concentrations up to 5% in the diet exhibited only weight loss. Adipic acid is not genetically active in a wide variety of assay systems. Adipic acid caused no developmental toxicity in mice, rats, rabbits, or hamsters when administered orally. Adipic acid is partially metabolized in humans; the balance is eliminated unchanged in the urine. Adipic acid is slightly to moderately toxic to fish, daphnia, and algae in acute tests.

  1. Acid Thunder: Acid Rain and Ancient Mesoamerica

    Science.gov (United States)

    Kahl, Jonathan D. W.; Berg, Craig A.

    2006-01-01

    Much of Mesoamerica's rich cultural heritage is slowly eroding because of acid rain. Just as water dissolves an Alka-Seltzer tablet, acid rain erodes the limestone surfaces of Mexican archaeological sites at a rate of about one-half millimeter per century (Bravo et al. 2003). A half-millimeter may not seem like much, but at this pace, a few…

  2. Acid Thunder: Acid Rain and Ancient Mesoamerica

    Science.gov (United States)

    Kahl, Jonathan D. W.; Berg, Craig A.

    2006-01-01

    Much of Mesoamerica's rich cultural heritage is slowly eroding because of acid rain. Just as water dissolves an Alka-Seltzer tablet, acid rain erodes the limestone surfaces of Mexican archaeological sites at a rate of about one-half millimeter per century (Bravo et al. 2003). A half-millimeter may not seem like much, but at this pace, a few…

  3. Omega-3 Fatty Acids

    Science.gov (United States)

    Omega-3 fatty acids are used together with lifestyle changes (diet, weight-loss, exercise) to reduce the ... the blood in people with very high triglycerides. Omega-3 fatty acids are in a class of ...

  4. Omega-6 Fatty Acids

    Science.gov (United States)

    Omega-6 fatty acids are types of fats. Some types are found in vegetable oils, including corn, evening primrose seed, safflower, and soybean oils. Other types of omega-6 fatty acids are found in black currant ...

  5. Lactic acid test

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003507.htm Lactic acid test To use the sharing features on this page, please enable JavaScript. Lactic acid is mainly produced in muscle cells and red ...

  6. Catalytic Synthesis Lactobionic Acid

    Directory of Open Access Journals (Sweden)

    V.G. Borodina

    2014-07-01

    Full Text Available Gold nanoparticles are obtained, characterized and deposited on the carrier. Conducted catalytic synthesis of lactobionic acid from lactose. Received lactobionic acid identify on the IR spectrum.

  7. Amino Acid Metabolism Disorders

    Science.gov (United States)

    ... this process. One group of these disorders is amino acid metabolism disorders. They include phenylketonuria (PKU) and maple syrup urine disease. Amino acids are "building blocks" that join together to form ...

  8. Facts about Folic Acid

    Science.gov (United States)

    ... Partners About Us Information For… Media Policy Makers Facts About Folic Acid Language: English (US) Español ( ... a woman needs 400 micrograms (mcg) every day. Facts About Folic Acid Download and print this fact ...

  9. Azelaic Acid Topical

    Science.gov (United States)

    Azelaic acid gel and foam is used to clear the bumps, lesions, and swelling caused by rosacea (a skin ... redness, flushing, and pimples on the face). Azelaic acid cream is used to treat the pimples and ...

  10. Folic Acid Quiz

    Science.gov (United States)

    ... About Us Information For… Media Policy Makers Folic Acid Quiz Language: English (US) Español (Spanish) Recommend ... button beside the question. Good Luck! 1. Folic acid is: A a B vitamin B a form ...

  11. Aedes aegypti (Diptera: Culicidae) biting deterrence: structure-activity relationship of saturated and unsaturated fatty acids.

    Science.gov (United States)

    Ali, Abbas; Cantrell, Charles L; Bernier, Ulrich R; Duke, Stephen O; Schneider, John C; Agramonte, Natasha M; Khan, Ikhlas

    2012-11-01

    In this study we evaluated the biting deterrent effects of a series of saturated and unsaturated fatty acids against Aedes aegypti (L), yellow fever mosquito (Diptera: Culicidae) using the K & Dbioassay module system. Saturated (C6:0 to C16:0 and C18:0) and unsaturated fatty acids (C11:1 to C14:1, C16:1, C18:1, and C18:2) showed biting deterrence index (BDI) values significantly greater than ethanol, the negative control. Among the saturated fatty acids, mid chain length acids (C10:0 to C13:0) showed higher biting deterrence than short (C6:0 to C9:0) and long chain length acids (C14:0 to C18:0), except for C8:0 and C16:0 that were more active than the other short and long chain acids. The BDI values of mid chain length acids (C10:0 to C13:0) were not significantly less than N, N-diethyl-meta-toluamide (DEET), the positive control. Among the unsaturated fatty acids, C11:1 showed the highest activity (BDI = 1.05) and C18:2 had the lowest activity (BDI = 0.7). In C11:1, C12:1, and C14:1 BDI values were not significantly less than DEET. After the preliminary observations, residual activity bioassays were performed on C11:0, C12:0, C11:1, and C12:1 over a 24-h period. All the fatty acids (C11:0, C12:0, C11:1, and C12:1) and DEET showed significantly higher activity at all test intervals than the solvent control. At treatment and 1-h posttreatment, all fatty acids showed proportion not biting (PNB) values not significantly less than DEET. At 3-, 6-, and 12-h posttreatment, all fatty acids showed PNB values significantly greater than DEET. At 24-h posttreatment, only the PNB value for C12:0 was significantly higher than DEET. The dose-responses of C12:0 and DEET were determined at concentrations of 5-25 nmol/cm2. As in the residual activity bioassays, the PNB values for C12:0 and DEET at 25 nmol/cm(2) were not significantly different. However, at lower concentrations, the PNB values for C12:0 were significantly greater than DEET. These results clearly indicate that mid

  12. Peroxisomal Enzymes and 8-Hydroxydeoxyguanosine in Rat Liver Treated with Perfluorooctanoic Acid

    Directory of Open Access Journals (Sweden)

    Awad Abdellatif

    2003-01-01

    Full Text Available Although peroxisome proliferators are considered non-genotoxic agents, most of them, nevertheless, were found to promote and/or induce, hepatocellular carcinoma (HCC in rodents. The aim of the present study is, first, to investigate whether the peroxisome proliferator perfluorooctanoic acid (PFOA possesses inherent liver cancer promoting activity, and second, to study the possible mechanisms involved. To acheive these aims two protocols have been applied, a biphasic protocol (initiation by diethyl-nitrozamine (DEN 200 mg/kg i.p. followed by treatment with 0.005% or 0.02% perflourooctanoic acid (PFOA for 14 and 25 weeks and a triphasic initiation, selection-promotion (IS protocol (initiation by giving 200 mg/kg DEN i.p. followed by a selection procedure for 2 weeks consisting of giving 0.03% 2-acetylaminofluorene (2-AAF in diet. In the middle of this treatment a single oral dose of carbon tetrachloride (2.0 ml/kg was given, followed by giving diet containg 0.015% of PFOA for 25 weeks. After applying both protocols, our results showed slight increase in the catalase activity while acyl CoA oxidase activity was markedly increased. Both experiments indicated that PFOA has a liver cancer promoting activity. Other groups of rats were given either basal diet or diet containing 0.02% PFOA. Five or nine weeks later they were sacrificed and the levels of 8-hydroxydeoxyguanosine in the isolated DNA were estimated. The data showed a slight nonetheless insignificant increase in 8-hydroxydeoxyguanosine. From the present data, it is concluded that PFOA is a true liver cancer promoter that may not require extensive initial DNA damage for its promoting activity.

  13. Determination of plasma lactic acid concentration and specific activity using high-performance liquid chromatography.

    Science.gov (United States)

    Bleiberg, B; Steinberg, J J; Katz, S D; Wexler, J; LeJemtel, T

    1991-08-23

    Assessment of lactate metabolism is of particular interest during exercise and in disease states such as diabetes, shock, and absorptive abnormalities of short-chain fatty acids by the colon. We describe an analytical method that introduces radio-active tracers and high-performance liquid chromatography (HPLC) to simultaneously analyze concentrations and specific activities (SAs) of plasma lactate. The HPLC conditions included separation on a reversed-phase column (octadecylsilane) and an isocratic buffer (30% acetonitrile in water). [3H]Acetate served as an internal standard. Lactate and acetate were extracted from plasma samples with diethyl ether following a pH adjustment to less than 1.0 and back-extracted into a hydrophilic phase with sodium carbonate (2 mM, pH greater than 10.0). Lactate is detected in the ultraviolet range (242 and 320 nm) by derivatization with alpha-bromoacetophenone. Control plasma samples were studied after an overnight fast for precision and analytical recovery. Calibration curves were linear in the range 0.18-6.0 mM (r = 0.92). The precision was 3% and the analytical recovery was 87%. The detection limit of the method was 36 pmol. Determination of lactate metabolism was performed in a patient with chronic congestive heart failure who was administered primed-continuous L-[U-14C]lactate (10 microCi bolus and 0.3 microCi/min continuously) during a 60-min rest period. Mean arterial lactate concentration and SA were 1.69 +/- 0.2 mM and 253.8 +/- 22 dpm/mumol, respectively. Systemic lactate turnover was 25.65 mumol/kg per min. Lactic acid systemic turnover, organ uptake and release rates can be accurately determined by isocratic HPLC.

  14. Immunoglobulin and fatty acids

    DEFF Research Database (Denmark)

    2009-01-01

    The present invention relates to a composition comprising 0.1-10 w/w % immunoglobulin (Ig), 4-14 w/w % saturated fatty acids, 4-14 w/w % mono-unsaturated fatty acids and 0-5 w/w % poly-unsaturated fatty acids, wherein the weight percentages are based on the content of dry matter in the composition...

  15. The Acid Rain Reader.

    Science.gov (United States)

    Stubbs, Harriett S.; And Others

    A topic which is often not sufficiently dealt with in elementary school textbooks is acid rain. This student text is designed to supplement classroom materials on the topic. Discussed are: (1) "Rain"; (2) "Water Cycle"; (3) "Fossil Fuels"; (4) "Air Pollution"; (5) "Superstacks"; (6) "Acid/Neutral/Bases"; (7) "pH Scale"; (8) "Acid Rain"; (9)…

  16. Stomach acid test

    Science.gov (United States)

    Gastric acid secretion test ... of the cells in the stomach to release acid. The stomach contents are then removed and analyzed. ... 3.5). These numbers are converted to actual acid production in units of milliequivalents per hour (mEq/ ...

  17. Acid Lipase Disease

    Science.gov (United States)

    ... Page You are here Home » Disorders » All Disorders Acid Lipase Disease Information Page Acid Lipase Disease Information Page What research is being ... research to understand lipid storage diseases such as acid lipase deficiency. Additional research studies hope to identify ...

  18. Acid Rain Study Guide.

    Science.gov (United States)

    Hunger, Carolyn; And Others

    Acid rain is a complex, worldwide environmental problem. This study guide is intended to aid teachers of grades 4-12 to help their students understand what acid rain is, why it is a problem, and what possible solutions exist. The document contains specific sections on: (1) the various terms used in conjunction with acid rain (such as acid…

  19. The Acid Rain Reader.

    Science.gov (United States)

    Stubbs, Harriett S.; And Others

    A topic which is often not sufficiently dealt with in elementary school textbooks is acid rain. This student text is designed to supplement classroom materials on the topic. Discussed are: (1) "Rain"; (2) "Water Cycle"; (3) "Fossil Fuels"; (4) "Air Pollution"; (5) "Superstacks"; (6) "Acid/Neutral/Bases"; (7) "pH Scale"; (8) "Acid Rain"; (9)…

  20. Sulfur-H{sub z}(CH{sub x}){sub y}(z = 0,1) functionalized metal oxide nanostructure decorated interfaces: Evidence of Lewis base and Brönsted acid sites – Influence on chemical sensing

    Energy Technology Data Exchange (ETDEWEB)

    Laminack, William; Baker, Caitlin [Department of Physics, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Gole, James, E-mail: james.gole@physics.gatech.edu [Department of Physics, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Department of Mechanical Engineering, Georgia Tech, Atlanta, GA 30332 (United States)

    2015-06-15

    Nanostructure metal oxide decorated n-type extrinsic porous silicon (PS) semiconductor interfaces are modified through in-situ interaction with acidic ethane and butane thiols (EtSH, BuSH) and basic diethyl sulfide (Et{sub 2}S). Highly sensitive conductometric sensor evaluations and X-ray Photoelectron Spectroscopy demonstrate the effect of sulfur group functionalization modifying the acidity of the metal oxides and their interaction with NH{sub 3}. SEM micrographs demonstrate that the sulfur treated particles are less than 30 nm in size. EDAX studies confirm the chemical composition of the modified nanoparticles and suggest the surface interaction of the sulfides and thiols. The acidic thiols can form Brönsted acidic sites enhancing the acidity of the metal oxides, thus broadening the initial metal oxide acidity range. The sulfides interact to lower the Lewis acidity of nanostructured metal oxide sites. Conductometric response matrices with NH{sub 3} at room temperature, corresponding to the thiol and sulfide treated nanostructures of the metal oxides TiO{sub 2}, SnO{sub x}, Ni{sub x}O, Cu{sub x}O, and Au{sub x}O (x >> 1) are evaluated for a dominant electron transduction process forming the basis for reversible chemical sensing in the absence of chemical bond formation. Treatment with the acidic thiols enhances the metal center acidity. It is suggested that the thiols can interact to increase the Brönsted acidity of the doped metal oxide surface if they maintain SH bonds. This process may account for the shift in Lewis acidity as the Brönsted acid sites counter the decrease in Lewis acidity resulting from the interaction of S-(CH{sub x}){sub y} groups. In contrast, treatment with basic Et{sub 2}S decreases the Lewis acidity of the metal oxide sites, enhancing the basicity of the decorated interface. XPS measurements indicate a change in binding energy (BE) of the metal and oxygen centers. The observed changes in conductometric response do not represent a