Constituents of the Vietnamese medicinal plant Orthosiphon stamineus.

PubMed

Tezuka, Y; Stampoulis, P; Banskota, A H; Awale, S; Tran, K Q; Saiki, I; Kadota, S

2000-11-01

From the MeOH extract of the aerial part of Vietnamese Orthosiphon stamineus, five new isopimarane-type diterpenes [orthosiphols F-J (1-5)] and two new diterpenes [staminols A (6) and B (7)] with a novel carbon-framework, to which we proposed the name "staminane", and three new highly-oxygenated staminane-type diterpenes [staminolactones A (8) and B (9) and norstaminol A (10)1 were isolated. Moreover, staminolactone A (8) is 8,14-secostaminane-type and staminolactone B (9) is 13,14-secostaminane-type, while norstaminol A (10) is 14-norstaminen-type. Together with these new diterpenes, sixteen known compounds were also isolated and identified to be: 7,3',4'-tri-O-methylluteolin (11), eupatorin (12), sinensetin (13), 5-hydroxy-6,7,3',4'-tetramethoxyflavone (14), salvigenin (15), ladanein (16), tetramethylscutellarein (17), 6-hydroxy-5,7,4'-trimethoxyflavone (18), vomifoliol (19), aurantiamide acetate (20), rosmarinic acid (21), caffeic acid (22), oleanolic acid (23), ursolic acid (24), betulinic acid (25), and beta-sitosterol (26). All the isolated compounds were tested for their cytotoxicity towards highly liver metastatic murine colon 26-L5 carcinoma cells, and the new diterpenes, except for 4, and flavonoids (11, 12, 16, 18) showed cytotoxicity with an ED50 value between 10 and 90 microg/ml.

Production of Putative Diterpene Carboxylic Acid Intermediates of Triptolide in Yeast

DOE Office of Scientific and Technical Information (OSTI.GOV)

Forman, Victor; Callari, Roberta; Folly, Christophe

The development of medical applications exploiting the broad bioactivities of the diterpene therapeutic triptolide from Tripterygium wilfordii is limited by low extraction yields from the native plant. Furthermore, the extraordinarily high structural complexity prevents an economically attractive enantioselective total synthesis. An alternative production route of triptolide through engineered Saccharomyces cerevisiae (yeast) could provide a sustainable source of triptolide. A potential intermediate in the unknown biosynthetic route to triptolide is the diterpene dehydroabietic acid. Here, we report a biosynthetic route to dehydroabietic acid by transient expression of enzymes from T. wilfordii and Sitka spruce (Picea sitchensis) in Nicotiana benthamiana. The combinationmore » of diterpene synthases TwTPS9, TwTPS27, and cytochromes P450 PsCYP720B4 yielded dehydroabietic acid and a novel analog, tentatively identified as ‘miltiradienic acid’. This biosynthetic pathway was reassembled in a yeast strain engineered for increased yields of the pathway intermediates, the diterpene olefins miltiradiene and dehydroabietadiene. Introduction in that strain of PsCYP720B4 in combination with two alternative NADPH-dependent cytochrome P450 reductases resulted in scalable in vivo production of dehydroabietic acid and its analog from glucose. Approaching future elucidation of the remaining biosynthetic steps to triptolide, our findings may provide an independent platform for testing of additional recombinant candidate genes, and ultimately pave the way to biotechnological production of the high value diterpenoid therapeutic.« less

Production of Putative Diterpene Carboxylic Acid Intermediates of Triptolide in Yeast

DOE PAGES

Forman, Victor; Callari, Roberta; Folly, Christophe; ...

2017-06-13

The development of medical applications exploiting the broad bioactivities of the diterpene therapeutic triptolide from Tripterygium wilfordii is limited by low extraction yields from the native plant. Furthermore, the extraordinarily high structural complexity prevents an economically attractive enantioselective total synthesis. An alternative production route of triptolide through engineered Saccharomyces cerevisiae (yeast) could provide a sustainable source of triptolide. A potential intermediate in the unknown biosynthetic route to triptolide is the diterpene dehydroabietic acid. Here, we report a biosynthetic route to dehydroabietic acid by transient expression of enzymes from T. wilfordii and Sitka spruce (Picea sitchensis) in Nicotiana benthamiana. The combinationmore » of diterpene synthases TwTPS9, TwTPS27, and cytochromes P450 PsCYP720B4 yielded dehydroabietic acid and a novel analog, tentatively identified as ‘miltiradienic acid’. This biosynthetic pathway was reassembled in a yeast strain engineered for increased yields of the pathway intermediates, the diterpene olefins miltiradiene and dehydroabietadiene. Introduction in that strain of PsCYP720B4 in combination with two alternative NADPH-dependent cytochrome P450 reductases resulted in scalable in vivo production of dehydroabietic acid and its analog from glucose. Approaching future elucidation of the remaining biosynthetic steps to triptolide, our findings may provide an independent platform for testing of additional recombinant candidate genes, and ultimately pave the way to biotechnological production of the high value diterpenoid therapeutic.« less

Investigation on traditional medicines of Guarany Indio and studies on diterpenes from Scoparia dulcis.

PubMed

Hayashi, Toshimitsu

2011-01-01

In interviews on the traditional herbal medicines of Tupi-Guarany Indians at the herbal market of Asuncion and questionnaire from their users, it was clarified that various useful medicinal plants are available in Paraguay and most of them are generally used without drying. In the search for bioactive substances from those plants, a β-glucuronidase-inhibitory diterpene called scoparic acid A (SA) was isolated from Scoparia dulcis L. together with scoparic acid B, scoparic acid C, and the aphidicolin-like tetracyclic diterpenes scopadulcic acid A (SDA) and scopadulcic acid B (SDB). HPLC analysis of diterpenes in the individual plants of Paraguayan and Asian S. dulcis revealed the presence of three chemotypes based on major component, i.e., SA type, SDB type, and SDX type containing mainly scopadiol and scopadulciol (SDC). SA and SDB were elucidated to be mainly biosynthesized in the leaves via 2-C-methyl-D-erythritol- 4-phosphate pathway, and a leaf organ culture system containing methyl jasmonate 10 µM was found to enhance the production of diterpenes by activation of Ca-signal transduction systems such as calmodulin and protein kinase C. On the other hand, SDB and SDC were found to show multifaceted pharmacological effects such as inhibitory effects on gastric acid excretion, bone resorption, replication of herpes simplex virus type 1 (HSV-1), etc. In addition, SDC was suggested to be applicable to cancer gene therapy using ganciclovir or acyclovir and the HSV-1 thymidine kinase gene called the suicide gene.

Diterpenes from rosemary (Rosmarinus officinalis): Defining their potential for anti-cancer activity.

PubMed

Petiwala, Sakina M; Johnson, Jeremy J

2015-10-28

Recently, rosemary extracts standardized to diterpenes (e.g. carnosic acid and carnosol) have been approved by the European Union (EU) and given a GRAS (Generally Recognized as Safe) status in the United States by the Food and Drug Administration (FDA). Incorporation of rosemary into our food system and through dietary selection (e.g. Mediterranean Diet) has increased the likelihood of exposure to diterpenes in rosemary. In consideration of this, a more thorough understanding of rosemary diterpenes is needed to understand its potential for a positive impact on human health. Three agents in particular have received the most attention that includes carnosic acid, carnosol, and rosmanol with promising results of anti-cancer activity. These studies have provided evidence of diterpenes to modulate deregulated signaling pathways in different solid and blood cancers. Rosemary extracts and the phytochemicals therein appear to be well tolerated in different animal models as evidenced by the extensive studies performed for approval by the EU and the FDA as an antioxidant food preservative. This mini-review reports on the pre-clinical studies performed with carnosic acid, carnosol, and rosmanol describing their mechanism of action in different cancers. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Insights Into the Bifunctional Aphidicolan-16-ß-ol Synthase Through Rapid Biomolecular Modeling Approaches.

PubMed

Hirte, Max; Meese, Nicolas; Mertz, Michael; Fuchs, Monika; Brück, Thomas B

2018-01-01

Diterpene synthases catalyze complex, multi-step C-C coupling reactions thereby converting the universal, aliphatic precursor geranylgeranyl diphosphate into diverse olefinic macrocylces that form the basis for the structural diversity of the diterpene natural product family. Since catalytically relevant crystal structures of diterpene synthases are scarce, homology based biomolecular modeling techniques offer an alternative route to study the enzyme's reaction mechanism. However, precise identification of catalytically relevant amino acids is challenging since these models require careful preparation and refinement techniques prior to substrate docking studies. Targeted amino acid substitutions in this protein class can initiate premature quenching of the carbocation centered reaction cascade. The structural characterization of those alternative cyclization products allows for elucidation of the cyclization reaction cascade and provides a new source for complex macrocyclic synthons. In this study, new insights into structure and function of the fungal, bifunctional Aphidicolan-16-ß-ol synthase were achieved using a simplified biomolecular modeling strategy. The applied refinement methodologies could rapidly generate a reliable protein-ligand complex, which provides for an accurate in silico identification of catalytically relevant amino acids. Guided by our modeling data, ACS mutations lead to the identification of the catalytically relevant ACS amino acid network I626, T657, Y658, A786, F789, and Y923. Moreover, the ACS amino acid substitutions Y658L and D661A resulted in a premature termination of the cyclization reaction cascade en-route from syn-copalyl diphosphate to Aphidicolan-16-ß-ol. Both ACS mutants generated the diterpene macrocycle syn-copalol and a minor, non-hydroxylated labdane related diterpene, respectively. Our biomolecular modeling and mutational studies suggest that the ACS substrate cyclization occurs in a spatially restricted location of the enzyme's active site and that the geranylgeranyl diphosphate derived pyrophosphate moiety remains in the ACS active site thereby directing the cyclization process. Our cumulative data confirm that amino acids constituting the G-loop of diterpene synthases are involved in the open to the closed, catalytically active enzyme conformation. This study demonstrates that a simple and rapid biomolecular modeling procedure can predict catalytically relevant amino acids. The approach reduces computational and experimental screening efforts for diterpene synthase structure-function analyses.

Insights into the bifunctional Aphidicolan-16-ß-ol synthase through rapid biomolecular modelling approaches

NASA Astrophysics Data System (ADS)

Hirte, Max; Meese, Nicolas; Mertz, Michael; Fuchs, Monika; Brück, Thomas B.

2018-04-01

Diterpene synthases catalyze complex, multi-step C-C coupling reactions thereby converting the universal, aliphatic precursor geranylgeranyl diphosphate into diverse olefinic macrocylces that form the basis for the structural diversity of the diterpene natural product family. Since catalytically relevant crystal structures of diterpene synthases are scarce, homology based biomolecular modelling techniques offer an alternative route to study the enzyme’s reaction mechanism. However, precise identification of catalytically relevant amino acids is challenging since these models require careful preparation and refinement techniques prior to substrate docking studies. Targeted amino acid substitutions in this protein class can initiate premature quenching of the carbocation centered reaction cascade. The structural characterization of those alternative cyclization products allows for elucidation of the cyclization reaction cascade and provides a new source for complex macrocyclic synthons. In this study, new insights into structure and function of the fungal, bifunctional Aphidicolan-16-ß-ol synthase were achieved using a simplified biomolecular modelling strategy. The applied refinement methodologies could rapidly generate a reliable protein-ligand complex, which provides for an accurate in silico identification of catalytically relevant amino acids. Guided by our modelling data, ACS mutations lead to the identification of the catalytically relevant ACS amino acid network I626, T657, Y658, A786, F789 and Y923. Moreover, the ACS amino acid substitutions Y658L and D661A resulted in a premature termination of the cyclization reaction cascade en-route from syn-copalyl diphosphate to Aphidicolan-16-ß-ol. Both ACS mutants generated the diterpene macrocycle syn-copalol and a minor, non-hydroxylated labdane related diterpene, respectively. Our biomolecular modelling and mutational studies suggest that the ACS substrate cyclization occurs in a spatially restricted location of the enzyme’s active site and that the geranylgeranyl diphosphate derived pyrophosphate moiety remains in the ACS active site thereby directing the cyclization process. Our cumulative data confirm that amino acids constituting the G-loop of diterpene synthases are involved in the open to the closed, catalytically active enzyme conformation. This study demonstrates that a simple and rapid biomolecular modelling procedure can predict catalytically relevant amino acids. The approach reduces computational and experimental screening efforts for diterpene synthase structure-function analyses.

The identity of Romanian amber (rumanite) with Baltic amber (succinite).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stout, E. C.; Beck, C. W.; Anderson, K. B.

Romanian amber (rumanite) has been considered to be a separate species of fossil resin for more than a century. While earlier investigators held it to be very similar to succinite (Baltic amber), modern scholars have assigned it a distinctly different botanical origin. We have found that almost all of the constituents of the ether-soluble fractions of 13 specimens of authentic rumanite identified by gas chromatography-mass spectrometry have previously been reported in the soluble fraction of succinite, including succinic acid and its monoterpene esters. Additionally and significantly, the soluble fraction of rumanite contains a number defunctionalized compounds that do not preexistmore » in succinite, but that are produced by pyrolysis of whole succinite or of its insoluble polymeric fraction. Simultaneous methylation pyrolysis-gas chromatography-mass spectrometry of the polymeric fraction of seven of the rumanite specimens yielded further copious amounts of dimethyl succinate, a number of diterpene resin acid methyl esters, and additional defunctionalized compounds known to be pyrolysis products of succinite. The evidence shows conclusively that the botanical origin of rumanite is not distinct from that of succinite. Rather, rumanite is a succinite that has suffered partial thermal degradation in the course of the folding of the Oligocene Kliwa sandstone formation in which it is most commonly found.« less

Identification and Functional Characterization of Monofunctional ent-Copalyl Diphosphate and ent-Kaurene Synthases in White Spruce Reveal Different Patterns for Diterpene Synthase Evolution for Primary and Secondary Metabolism in Gymnosperms1[W][OA

PubMed Central

Keeling, Christopher I.; Dullat, Harpreet K.; Yuen, Mack; Ralph, Steven G.; Jancsik, Sharon; Bohlmann, Jörg

2010-01-01

The biosynthesis of the tetracyclic diterpene ent-kaurene is a critical step in the general (primary) metabolism of gibberellin hormones. ent-Kaurene is formed by a two-step cyclization of geranylgeranyl diphosphate via the intermediate ent-copalyl diphosphate. In a lower land plant, the moss Physcomitrella patens, a single bifunctional diterpene synthase (diTPS) catalyzes both steps. In contrast, in angiosperms, the two consecutive cyclizations are catalyzed by two distinct monofunctional enzymes, ent-copalyl diphosphate synthase (CPS) and ent-kaurene synthase (KS). The enzyme, or enzymes, responsible for ent-kaurene biosynthesis in gymnosperms has been elusive. However, several bifunctional diTPS of specialized (secondary) metabolism have previously been characterized in gymnosperms, and all known diTPSs for resin acid biosynthesis in conifers are bifunctional. To further understand the evolution of ent-kaurene biosynthesis as well as the evolution of general and specialized diterpenoid metabolisms in gymnosperms, we set out to determine whether conifers use a single bifunctional diTPS or two monofunctional diTPSs in the ent-kaurene pathway. Using a combination of expressed sequence tag, full-length cDNA, genomic DNA, and targeted bacterial artificial chromosome sequencing, we identified two candidate CPS and KS genes from white spruce (Picea glauca) and their orthologs in Sitka spruce (Picea sitchensis). Functional characterization of the recombinant enzymes established that ent-kaurene biosynthesis in white spruce is catalyzed by two monofunctional diTPSs, PgCPS and PgKS. Comparative analysis of gene structures and enzyme functions highlights the molecular evolution of these diTPSs as conserved between gymnosperms and angiosperms. In contrast, diTPSs for specialized metabolism have evolved differently in angiosperms and gymnosperms. PMID:20044448

Labdane-type diterpenes active against acne from pine cones (Pinus densiflora).

PubMed

Sultan, Md Zakir; Jeon, Young-Min; Moon, Surk-Sik

2008-03-01

Bioassay-guided extraction and fractionation of the aqueous methanolic extract of the cones of Pinus densiflora (Pinaceae) afforded one new labdane-type diterpene aldehyde, 15-nor-14-oxolabda-8(17),12 E-diene-18-oic acid, along with eight known diterpenes. Their structures were elucidated using spectroscopic methods as well as by comparison with previously reported data. The isolates showed antibacterial (Propionibacterium acnes) and antifungal activities.

Labdane diterpenes from Juniperus communis L. berries.

PubMed

Martin, Anne Marie; Queiroz, Emerson Ferreira; Marston, Andrew; Hostettmann, Kurt

2006-01-01

A phytochemical study of the methanol extract of Juniperus communis berries was undertaken. The crude extract was analysed by HPLC-UV and the isolation of the minor compounds was performed by centrifugal partition chromatography. By this means, five diterpenes were isolated, one of which was a new labdane diterpene 15,16-epoxy-12-hydroxy-8(17),13(16),14-labdatrien-19-oic acid. The structures of the isolated compounds were elucidated by spectroscopic methods, including UV, NMR, MS and HR-MS.

Helikaurolides A-D with a Diterpene-Sesquiterpene Skeleton from Supercritical Fluid Extracts of Helianthus annuus L. var. Arianna.

PubMed

Torres, Ascensión; Molinillo, José M G; Varela, Rosa M; Casas, Lourdes; Mantell, Casimiro; Martínez de la Ossa, Enrique J; Macías, Francisco A

2015-10-02

Four novel compounds (1-4) with an unprecedented skeleton that combines a sesquiterpene lactone and a kaurane diterpene acid were isolated from Helianthus annuus L. var. Arianna extract, which was obtained under supercritical conditions. The structures of 1-4 were elucidated by NMR and MS analyses. The biosynthetic routes involve sesquiterpene lactones and kauranic acid, both of which were previously isolated from this species.

Antifungal diterpenes from Hypoestes serpens (Acanthaceae).

PubMed

Rasoamiaranjanahary, Lalao; Marston, Andrew; Guilet, David; Schenk, Kurt; Randimbivololona, Fanantenanirainy; Hostettmann, Kurt

2003-02-01

Two new diterpenes, fusicoserpenol A and dolabeserpenoic acid A, with antifungal activity, were isolated from leaves of Hypoestes serpens (Acanthaceae). Their structures were elucidated by means of spectrometric methods including 1D and 2D NMR experiments and MS analysis. X-ray crystallographic analysis confirmed the structure of fusicoserpenol A and established the relative configuration.

Diterpenes from Xylopia langsdorffiana inhibit cell growth and induce differentiation in human leukemia cells.

PubMed

Castello Branco, Marianna V S; Anazetti, Maristella C; Silva, Marcelo S; Tavares, Josean F; Diniz, Margareth F F Melo; Frungillo, Lucas; Haun, Marcela; Melo, Patrícia S

2009-01-01

Two new diterpenes were isolated from stems and leaves of Xylopia langsdorffiana, ent-atisane-7alpha,16alpha-diol (xylodiol) and ent-7alpha-acetoxytrachyloban-18-oic acid (trachylobane), along with the known 8(17),12E,14-labdatrien-18-oic acid (labdane). We investigated their antitumour effects on HL60, U937 and K562 human leukemia cell lines. We found that xylodiol was the most potent diterpene in inhibiting cell proliferation of HL60, U937 and K562 cells, with mean IC50 values of 90, 80 and 50 microM, respectively. Based on the nitroblue tetrazolium (NBT) reduction assay, all the diterpenes were found to induce terminal differentiation in HL60 and K562 cells, with xylodiol being the most effective. NBT reduction was increased by almost 120% after 12 h exposure of HL60 cells to xylodiol at a concentration lower than the IC50 (50 microM). Thus, xylodiol inhibited human leukemia cell growth in vitro partly by inducing cell differentiation, and merits further studies to examine its mechanism of action as a potential antitumoural agent.

Elucidation of terpenoid metabolism in Scoparia dulcis by RNA-seq analysis.

PubMed

Yamamura, Yoshimi; Kurosaki, Fumiya; Lee, Jung-Bum

2017-03-07

Scoparia dulcis biosynthesize bioactive diterpenes, such as scopadulcic acid B (SDB), which are known for their unique molecular skeleton. Although the biosynthesis of bioactive diterpenes is catalyzed by a sequence of class II and class I diterpene synthases (diTPSs), the mechanisms underlying this process are yet to be fully identified. To elucidate these biosynthetic machinery, we performed a high-throughput RNA-seq analysis, and de novo assembly of clean reads revealed 46,332 unique transcripts and 40,503 two unigenes. We found diTPSs genes including a putative syn-copalyl diphosphate synthase (SdCPS2) and two kaurene synthase-like (SdKSLs) genes. Besides them, total 79 full-length of cytochrome P450 (CYP450) genes were also discovered. The expression analyses showed selected CYP450s associated with their expression pattern of SdCPS2 and SdKSL1, suggesting that CYP450 candidates involved diterpene modification. SdCPS2 represents the first predicted gene to produce syn-copalyl diphosphate in dicots. In addition, SdKSL1 potentially contributes to the SDB biosynthetic pathway. Therefore, these identified genes associated with diterpene biosynthesis lead to the development of genetic engineering focus on diterpene metabolism in S. dulcis.

Elucidation of terpenoid metabolism in Scoparia dulcis by RNA-seq analysis

PubMed Central

Yamamura, Yoshimi; Kurosaki, Fumiya; Lee, Jung-Bum

2017-01-01

Scoparia dulcis biosynthesize bioactive diterpenes, such as scopadulcic acid B (SDB), which are known for their unique molecular skeleton. Although the biosynthesis of bioactive diterpenes is catalyzed by a sequence of class II and class I diterpene synthases (diTPSs), the mechanisms underlying this process are yet to be fully identified. To elucidate these biosynthetic machinery, we performed a high-throughput RNA-seq analysis, and de novo assembly of clean reads revealed 46,332 unique transcripts and 40,503 two unigenes. We found diTPSs genes including a putative syn-copalyl diphosphate synthase (SdCPS2) and two kaurene synthase-like (SdKSLs) genes. Besides them, total 79 full-length of cytochrome P450 (CYP450) genes were also discovered. The expression analyses showed selected CYP450s associated with their expression pattern of SdCPS2 and SdKSL1, suggesting that CYP450 candidates involved diterpene modification. SdCPS2 represents the first predicted gene to produce syn-copalyl diphosphate in dicots. In addition, SdKSL1 potentially contributes to the SDB biosynthetic pathway. Therefore, these identified genes associated with diterpene biosynthesis lead to the development of genetic engineering focus on diterpene metabolism in S. dulcis. PMID:28266568

Diterpenes and other constituents from Croton draco (Euphorbiaceae).

PubMed

Murillo, R M; Jakupovic, J; Rivera, J; Castro, V H

2001-03-01

Croton draco (Euphorbiaceae) from Guadalupe, San José, Costa Rica was collected in July 1992 and phytochemically studied (leaves, seeds, wood, bark, sap and flowers separately). Commonly known compounds such as 1-hydroxyjunenol, p-hydroxybenzaldehyde, p-methoxybenzoic acid, 3,4,5-trimethoxycinnamyl alcohol, the coumarin scopoletin, the nor-terpenoids 9-dehydrovomifoliol and 2,3-dihydrovomifoliol were obtained. Taspine, two aporphinic alkaloids, the diterpenes 9(11)-dehydrokaurenic acid, hardwikiic acid, the corresponding new 12-oxo derivative as well as five clerodanes and a phorbol ester were also isolated. Three clerodanes were not previously described and their NMR spectroscopical data and MS fragmentation patterns are reported.

Antiproliferative Diterpenes from a Malleastrum sp. from the Madagascar dry forest[1

PubMed Central

Liu, Yixi; Wiedle, C. Houston; Brodie, Peggy J.; Callmander, Martin W.; Rakotondrajaona, R.; Rakotobe, Etienne; Rasamison, Vincent E.

2015-01-01

An ethanol extract of leaves of the plant species Malleastrum sp. collected in northern Madagascar afforded the new clerodane diterpene 18-oxo-cleroda-3,13-dien-16,15-olide (1), together with the three known clerodane diterpenes 16,18-dihydroxykolavenic acid lactone (2), solidagolactone (3) and (−)-kolavenol (4), and the known labdane diterpene 3-oxo-ent-Iabda-8(17),13-dien-15,16-olide (5). Compounds 1, 3, and 4 showed moderate antiproliferative activities against the A2780 ovarian cancer cell line, with the IC50 values of 3.01 ± 0.8, 7.84 ± 0.2, and 17.9 ± 3 μM, respectively. The structure elucidations of all compounds were carried out based on analysis of NMR and mass spectroscopic data. The relative stereochemistry of compound 1 was determined by NOESY NMR spectrum. PMID:26594745

New approaches on the analyses of thermolabile coffee diterpenes by gas chromatography and its relationship with cup quality.

PubMed

Novaes, Fábio Junior Moreira; Oigman, Silvia Siag; de Souza, Rodrigo Octavio Mendonça Alves; Rezende, Claudia Moraes; de Aquino Neto, Francisco Radler

2015-07-01

A new gas chromatography method using pulsed split injector (PS-GC) was validated to quantify thermolabile diterpenes cafestol, kahweol and isokahweol in methanolysed Arabica coffee oils. Linearity was 0.99 from 8 to 69mgmL(-1), recovery ranged from 99% to 101% and precision of less than 4% was obtained. Besides, Soxhlet extraction time was evaluated and Tukey׳s test indicated that the mass of diterpenes obtained in 4h is equivalent to a 16h period, which represents a space-time yield four times higher. The microwave assisted methanolysis proved to be efficient to quantitatively convert the natural diterpene esters in their respective alcohols and fatty acid methyl esters, accompanied by PS-GC. Also, the intact diterpene esters were analyzed by GC for the first time by the comparison between cold on-column (COC) and PS injection techniques. In all these stages, the molecular integrity of the thermolabile furokaurane diterpenes was maintained. The methanolysed oils from 13 samples of green Brazilian Arabica coffees were analyzed by PS-GC and the diterpenes composition varied from 8 to 12% w/w in oil and 0.7-1% in coffee beans. The ratio between cafestol and kahweol was successfully used to predict the quality of coffee even before the roasting and brewing processes. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of ent-kaurane diterpene monoglycosides.

PubMed

Chaturvedula, Venkata Sai Prakash; Klucik, Josef; Upreti, Mani; Prakash, Indra

2011-10-03

Synthesis of two ent-kaurane diterpene glycosides, steviol 19-O-β-D-glucopyranosiduronic acid (steviol glucuronide, 5), and 13-hydroxy ent-kaur-16-en-19-oic acid-β-D-glucopyranosyl ester (7) has been achieved from a common starting material, steviol, using phase transfer catalyst. Also, synthesis of an additional 17-nor-ent-kaurane glycoside, namely 13-methyl-16-oxo-17-nor-ent-kauran-19-oic acid-β-D-glucopyranosyl ester (10) was performed using the starting material isosteviol and similar synthetic methodology. Synthesis of all three steviol glycosides was performed using straightforward chemistry and their structures were characterized on the basis of 1D and 2D NMR as well as mass spectral (MS) data.

Variability of some diterpene esters in coffee beverages as influenced by brewing procedures.

PubMed

Moeenfard, Marzieh; Erny, Guillaume L; Alves, Arminda

2016-11-01

Several coffee brews, including classical and commercial beverages, were analyzed for their diterpene esters content (cafestol and kahweol linoleate, oleate, palmitate and stearate) by high performance liquid chromatography with diode array detector (HPLC-DAD) combined with spectral deconvolution. Due to the coelution of cafestol and kahweol esters at 225 nm, HPLC-DAD did not give accurate quantification of cafestol esters. Accordingly, spectral deconvolution was used to deconvolve the co-migrating profiles. Total cafestol and kahweol esters content of classical coffee brews ranged from 5-232 to 2-1016 mg/L, respectively. Commercial blends contained 1-54 mg/L of total cafestol esters and 2-403 mg/L of total kahweol esters. Boiled coffee had the highest diterpene esters content, while filtered and instant brews showed the lowest concentrations. However, individual diterpene esters content was not affected by brewing procedure as in terms of kahweol esters, kahweol palmitate was the main compound in all samples, followed by kahweol linoleate, oleate and stearate. Higher amounts of cafestol palmitate and stearate were also observed compared to cafestol linoleate and cafestol oleate. The ratio of diterpene esters esterified with unsaturated fatty acids to total diterpene esters was considered as measure of their unsaturation in analyzed samples which varied from 47 to 52%. Providing new information regarding the diterpene esters content and their distribution in coffee brews will allow a better use of coffee as a functional beverage.

Chemical diversity of labdane-type bicyclic diterpene biosynthesis in Actinomycetales microorganisms.

PubMed

Yamada, Yuuki; Komatsu, Mamoru; Ikeda, Haruo

2016-07-01

Five pairs of bacterial type-A and type-B diterpene synthases have been characterized: BAD86798/BAD86797, AHK61133/AHK61132, BAB39207/BAB39206, CldD/CldB and RmnD/RmnB, and are involved in the formation of pimara-9(11),15-diene, terpente-3,13,15-triene and labda-8(17),12(E),14-triene. Mining of bacterial genome data revealed an additional four pairs of type-A and type-B diterpene synthases: Sros_3191/Sros_3192 of Streptosporangium roseum DSM 43021, Sare_1287/Sare_1288 of Salinispora arenicola CNS-205, SCLAV_5671/SCLAV_5672 and SCLAV_p0491/SCLAV_p0490 of Streptomyces clavuligerus ATCC 27064. Since SCLAV_p0491/SCLAV_p0490 is similar to the labdane-type diterpene synthase pairs, CldD/CldB and RmnD/RmnB based on the alignment of the deduced amino acid sequences and phylogenetic analyses of the aligned sequences, these predicted diterpene synthases were characterized by an enzymatic reaction using a pair of recombinant type-A and type-B diterpene synthases prepared in Escherichia coli and the heterologous expression of two genes encoding type-A and type-B diterpene synthases in an engineered Streptomyces host. The generation of labda-8(17),12(E),14-triene (1) by CldB and CldD was reconfirmed by enzymatic synthesis. Furthermore, labda-8(17),13(16),14-triene (2) was generated by SCLAV_p0491 and CldB, and ladba-7,12(E),14-triene (3) by CldD and SCLAV_p0490. SCLAV_p0491 and SCLAV_p0490 catalyzed the generation of the novel diterpene hydrocarbon, labda-7,13(16),14-triene (4).

Contrasting Patterns of Diterpene Acid Induction by Red Pine and White Spruce to Simulated Bark Beetle Attack, and Interspecific Differences in Sensitivity Among Fungal Associates

Treesearch

Charles J. Mason; Kier D. Klepzig; Brian J. Kopper; Philip J. Kersten; Barbara L. Illman; Kenneth F. Raffa

2015-01-01

Conifers possess a suite of physiochemical defenses that protect their subcortical tissues from bark beetle -fungal complexes. These defenses include rapid induction of terpenoids and phenolics at the site of attack. Studies of the distribution, induction, and bioactivity of conifer terpenoids have focused heavily on monoterpenes. We assessed induction of diterpene...

Synthesis of a new allelopathic agent from the biotransformation of ent-15α-hydroxy-16-kauren-19-oic acid with Fusarium proliferatum.

PubMed

Rocha, A D; Vieira, H da S; Takahashi, J A; Boaventura, M A D

2017-11-01

The use of kaurane diterpenes as substrates in fungal biotransformation to achieve bioactive compounds has been widely reported. In this work, the natural product kaurenoic acid, a diterpene widely distributed in the plant Kingdom, was chemically converted into ent-15α-hydroxy-kaur-16-en-19-oic acid (1). Substrate 1 was subjected to biotransformation by the fungus Fusarium proliferatum, furnishing a new derivative, ent-2α,15α-dihydroxy-kaur-16-en-19-oic acid (2). The structure of metabolite 2 was deduced on the basis of spectroscopy and MS data. Derivative 2 showed allelopathic activity on germination and growth of root and stem of lettuce (Lactuca sativa), inhibiting 100% of germination and growth of roots and stem, at higher concentration assayed (10 -4  mol/L).

Identification of new diterpene esters from green Arabica coffee beans, and their platelet aggregation accelerating activities.

PubMed

Wang, Xia; Meng, QianQian; Peng, XingRong; Hu, GuiLin; Qiu, MingHua

2018-10-15

Eight new ent-kaurane diterpene fatty acid esters, namely caffarolides A-H (1-8), were isolated from green beans of Coffea arabica. Their chemical structures were confirmed by extensive spectroscopic analysis including 1D, 2D NMR (HSQC, HMBC, 1 H- 1 H COSY, and ROESY), HRMS, IR and CD spectra and by GC-FID analysis. Interestingly, the diterpene moiety of these new compounds first occurred in genus Coffea. All the isolates were evaluated for platelet aggregation activity in vitro. As the results, caffarolides C, D and F (3, 4 and 6) showed induction effect for platelet aggregation and the possible structure-activity relationships have been discussed briefly. Copyright © 2018 Elsevier Ltd. All rights reserved.

New cassane diterpenes from Caesalpinia echinata.

PubMed

Cota, Betania Barros; de Oliveira, Djalma Menezes; de Siqueira, Ezequias Pessoa; Souza-Fagundes, Elaine Maria; Pimenta, Adriano M C; Santos, Daniel M; Rabello, Ana; Zani, Carlos Leomar

2011-10-01

An investigation of the ethanolic extract from stems of Caesalpinia echinata Lam (Leguminosae-Caesalpinioideae) led to the isolation of five new cassane diterpenes along with known lambertianic acid. Their structures were determined based on spectroscopic methods. A preliminary study on leishmanicidal activity demonstrated that compounds 1, 2 and 6 were found to inhibit the growth of amastigote-like forms of Leishmania amazonensis without affecting mononuclear cells obtained from human peripheral blood. Copyright © 2011 Elsevier B.V. All rights reserved.

Elucidation of the biosynthesis of carnosic acid and its reconstitution in yeast

NASA Astrophysics Data System (ADS)

Scheler, Ulschan; Brandt, Wolfgang; Porzel, Andrea; Rothe, Kathleen; Manzano, David; Božić, Dragana; Papaefthimiou, Dimitra; Balcke, Gerd Ulrich; Henning, Anja; Lohse, Swanhild; Marillonnet, Sylvestre; Kanellis, Angelos K.; Ferrer, Albert; Tissier, Alain

2016-10-01

Rosemary extracts containing the phenolic diterpenes carnosic acid and its derivative carnosol are approved food additives used in an increasingly wide range of products to enhance shelf-life, thanks to their high anti-oxidant activity. We describe here the elucidation of the complete biosynthetic pathway of carnosic acid and its reconstitution in yeast cells. Cytochrome P450 oxygenases (CYP76AH22-24) from Rosmarinus officinalis and Salvia fruticosa already characterized as ferruginol synthases are also able to produce 11-hydroxyferruginol. Modelling-based mutagenesis of three amino acids in the related ferruginol synthase (CYP76AH1) from S. miltiorrhiza is sufficient to convert it to a 11-hydroxyferruginol synthase (HFS). The three sequential C20 oxidations for the conversion of 11-hydroxyferruginol to carnosic acid are catalysed by the related CYP76AK6-8. The availability of the genes for the biosynthesis of carnosic acid opens opportunities for the metabolic engineering of phenolic diterpenes, a class of compounds with potent anti-oxidant, anti-inflammatory and anti-tumour activities.

A new rearranged dolabellane diterpene from the soft coral Clavularia inflata.

PubMed

Alea, Glenn V; Bowden, Bruce F; Ragasa, Consolacion Y

2008-06-15

A new dolabellane type diterpene 1 has been isolated through its acetate 1a. The structure of 1a was elucidated by extensive 1D and 2D NMR spectroscopy and confirmed by mass spectrometry. The structure of 1 was deduced by comparison of its NMR spectral data with those of 1a, while its relative stereochemistry was deduced by NOESY. The absolute stereochemistry of C-7 was determined by analyses of 1 separately esterified with R and S O-mandelic acids.

Differences in ponderosa pine isocupressic acid concentrations across space and time

USDA-ARS?s Scientific Manuscript database

Ponderosa Pine (Pinus ponderosa) is distributed throughout the western half of North America, where it is the most widely adapted and ubiquitous conifer. Ponderosa Pine contains isocupressic acid, a diterpene acid, which has been shown to be responsible for its abortifacient activity. The objectiv...

Genus Cistus: a model for exploring labdane-type diterpenes' biosynthesis and a natural source of high value products with biological, aromatic and pharmacological properties

NASA Astrophysics Data System (ADS)

Papaefthimiou, Dimitra; Papanikolaou, Antigoni; Falara, Vasiliki; Givanoudi, Stella; Kostas, Stefanos; Kanellis, Angelos

2014-06-01

The family Cistaceae (Angiosperm, Malvales) consists of 8 genera and 180 species, with 5 genera native of the Mediterranean area (Cistus, Fumara, Halimium, Helianthemum and Tuberaria). Traditionally, a number of Cistus specie have been used in Mediterranean folk medicine as herbal tea infusions for healing, digestive problems and colds, as extracts for the treatment of diseases, and as fragrances. The resin, ladano, secreted by the glandular trichomes of certain Cistus species contains a number of phytochemicals with antioxidant, antibacterial, antifungal and anticancer properties. Furthermore, total leaf aqueous extracts possess anti-influenza virus activity. All these properties have been attributed to phytochemicals such as terpenoids, including diterpenes, labdane-type diterpenes and clerodanes, phenylpropanoids, including flavonoids and ellagitannins, several groups of alkaloids and other types of secondary metabolites. In the past 20 years, research on Cistus involved chemical, biological and phylogenetic analysis but recent investigations have involved genomic and molecular approaches. Our lab is exploring the biosynthetic machinery that generates terpenoids and phenylpropanoids, with a goal to harness their numerous properties that have applications in the pharmaceutical, chemical and aromatic industries. This review focuses on the systematics, botanical characteristics, geographic distribution, chemical analyses, biological function and biosynthesis of major compounds, as well as genomic analyses and biotechnological approaches of the main Cistus species found in the Mediterranean basin, namely C. albidus, C. creticus, C. crispus, C. parviflorus, C. monspeliensis, C. populifolius, C. salviifolius, C. ladanifer, C. laurifolius and C. clusii.

Antisecretory actions of Baccharis trimera (Less.) DC aqueous extract and isolated compounds: analysis of underlying mechanisms.

PubMed

Biondo, Thais Maíra A; Tanae, Mirtes M; Coletta, Eliana Della; Lima-Landman, Maria Teresa R; Lapa, Antonio J; Souccar, Caden

2011-06-22

Baccharis trimera (Less.) DC. (Asteraceae) is a species native to South America used in Brazilian folk medicine to treat gastrointestinal and liver diseases, kidney disorders and diabetes. Previous studies from this laboratory confirmed the antacid and antiulcer activities of the plant aqueous extract (AE) in rat and mouse models. To investigate the mechanisms involved in the antacid action of AE and isolated compounds from Baccharis trimera. AE was assayed in vivo in cold-restraint stress gastric ulcers and in pylorus-ligated mice. Nine fractions (F2-F10) previously isolated from AE were assayed in vitro on acid secretion measured as [(14)C]-aminopyrine ([(14)C]-AP) accumulation in rabbit gastric glands, and on gastric microsomal H(+), K(+)-ATPase preparations. Chlorogenic acids (F2, F3, F6, F7), flavonoids (F9), an ent-clerodane diterpene (F8) and a dilactonic neo-clerodane diterpene (F10) have been identified in these fractions. Intraduodenal injection of AE (1.0 and 2.0 g/kg) in 4h pylorus-ligated mice decreased the volume (20 and 50%) and total acidity (34 and 50%) of acid secretion compared to control values. Administered orally at the same doses AE protected against gastric mucosal lesions induced in mice by restraint at 4°C. Exposure of isolated rabbit gastric glands to fractions F8 (10-100 μM) and F9 (10-300 μg/ml) decreased the basal [(14)C]-AP uptake by 50 and 60% of control (Ratio=6.2±1.1), whereas the remaining fractions were inactive. In the presence of the secretagogues F2 and F4 (30-300 μg/ml) decreased the [(14)C]-AP uptake induced by histamine (His) with a 100-fold lower potency than that of ranitidine. F5 and F6 reduced the [(14)C]-AP uptake stimulated by carbachol (CCh), but they were 10 to 20-fold less potent than atropine. F8 (diterpene 2) and F9 (flavonoids) decreased both the His- and CCh-induced [(14)C]-AP uptake, whereas F10 (diterpene 1) was inactive against the [(14)C]-AP uptake stimulated by secretagogues. Diterpene 2 was the most active of all tested compounds being 7-fold less potent than ranitidine and equipotent to atropine in reducing acid secretion in vitro. This compound also reduced the gastric H(+), K(+)-ATPase activity by 20% of control, while the remaining fractions were inactive on the proton pump in vitro. The results indicate that Baccharis trimera presents constituents that inhibit gastric acid secretion by acting mainly on the cholinergic regulatory pathway. The plant extract also contains compounds that exert moderate inhibition of the histaminergic regulatory pathway of acid secretion and the gastric proton pump. Altogether these active constituents appear to provide effective inhibition of acid secretion in vivo, which may explain the reputed antiulcer activity of the plant extract. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

Minor diterpene glycosides from the leaves of Stevia rebaudiana.

PubMed

Ibrahim, Mohamed A; Rodenburg, Douglas L; Alves, Kamilla; Fronczek, Frank R; McChesney, James D; Wu, Chongming; Nettles, Brian J; Venkataraman, Sylesh K; Jaksch, Frank

2014-05-23

Two new diterpene glycosides in addition to five known glycosides have been isolated from a commercial extract of the leaves of Stevia rebaudiana. Compound 1 (rebaudioside KA) was shown to be 13-[(O-β-d-glucopyranosyl)oxy]ent-kaur-16-en-19-oic acid 2-O-β-d-glucopyranosyl-β-d-glucopyranosyl ester and compound 2, 12-α-[(2-O-β-d-glucopyranosyl-β-d-glucopyranosyl)oxy]ent-kaur-16-en-19-oic acid β-d-glucopyranosyl ester. Five additional known compounds were identified, rebaudioside E, rebaudioside M, rebaudioside N, rebaudioside O, and stevioside, respectively. Enzymatic hydrolysis of stevioside afforded the known ent-kaurane aglycone 13-hydroxy-ent-kaur-16-en-19-oic acid (steviol) (3). The isolated metabolite 1 possesses the ent-kaurane aglycone steviol (3), while compound 2 represents the first example of the isomeric diterpene 12-α-hydroxy-ent-kaur-16-en-19-oic acid existing as a glycoside in S. rebaudiana. The structures of the isolated metabolites 1 and 2 were determined based on comprehensive 1D- and 2D-NMR (COSY, HSQC, and HMBC) studies. A high-quality crystal of compound 3 has formed, which allowed the acquisition of X-ray diffraction data that confirmed its structure. The structural similarities between the new metabolites and the commercially available stevioside sweeteners suggest the newly isolated metabolites should be examined for their organoleptic properties. Accordingly rebaudiosides E, M, N, O, and KA have been isolated in greater than gram quantities.

Neuroprotective Effects of Ferruginol, Jatrophone, and Junicedric Acid Against Amyloid-β Injury in Hippocampal Neurons.

PubMed

Zolezzi, Juan M; Lindsay, Carolina B; Serrano, Felipe G; Ureta, Roxana C; Theoduloz, Cristina; Schmeda-Hirschmann, Guillermo; Inestrosa, Nibaldo C

2018-01-01

Soluble amyloid-β (Aβ) oligomers have been recognized as early neurotoxic intermediates with a key role in the synaptic dysfunction observed in Alzheimer's disease (AD). Aβ oligomers block hippocampal long-term potentiation (LTP) and impair rodent spatial memory. Additionally, the presence of Aβ oligomers is associated with imbalanced intracellular calcium levels and apoptosis in neurons. In this context, we evaluated the effects of three diterpenes (ferruginol, jatrophone, and junicedric acid) that are found in medicinal plants and have several forms of biological activity. The intracellular calcium levels in hippocampal neurons increased in the presence of ferruginol, jatrophone, and junicedric acid, a result that was consistent with the observed increase in CA1 synaptic transmission in mouse hippocampal slices. Additionally, assays using Aβ peptide demonstrated that diterpenes, particularly ferruginol, restore LTP and reduce apoptosis. Recovery of the Aβ oligomer-induced loss of the synaptic proteins PSD-95, synapsin, VGlut, and NMDA receptor subunit 2A was observed in mouse hippocampal slices treated with junicedric acid. This cascade of events may be associated with the regulation of kinases, e.g., protein kinase C (PKC) and calcium/calmodulin-dependent protein kinase II (CaMKII), in addition to the activation of the canonical Wnt signaling pathway and could thus provide protection against Aβ oligomers, which trigger synaptic dysfunction. Our results suggest a potential neuroprotective role for diterpenes against the Aβ oligomers-induced neurodegenerative alterations, which make them interesting molecules to be further studied in the context of AD.

Involvement of 2-C-methyl-D-erythritol-4-phosphate pathway in biosynthesis of aphidicolin-like tetracyclic diterpene of Scoparia dulcis.

PubMed

Nkembo, Marguerite Kasidimoko; Lee, Jung-Bum; Nakagiri, Takeshi; Hayashi, Toshimitsu

2006-05-01

Specific inhibitors of the MVA pathway (pravastatin) and the MEP pathway (fosmidomycin) were used to interfere with the biosynthetic flux which leads to the production of aphidicolin-like diterpene in leaf organ cultures of Scoparia dulcis. Treatment of leaf organs with fosmidomycin resulted in dose dependent inhibition of chlorophylls, carotenoids, scopadulcic acid B (SDB) and phytol production, and no effect on sterol production was observed. In response to the pravastatin treatment, a significant decrease in sterol and perturbation of SDB production was observed.

A new labdane diterpene from the rhizomes of Alpinia officinarum.

PubMed

Zou, Qiong-Yu; Wu, Hai-Feng; Tang, Yu-Lian; Chen, Di-Zhao

2016-01-01

A new labdane diterpene, (Z)-12,14-labdadien-15(16)-olide-17-oic acid (1), and a new natural cadinane sesquiterpene, 4-isopropyl-6-methyl-1-naphthalenemethanol (2), were isolated from the ethanolic extract of the rhizomes of Alpinia officinarum, together with three other products, galangin (3), kaempferol (4) and quercetin (5). Their structures were elucidated by using extensive spectroscopic methods. Compounds 1 and 2 showed no remarkable cytotoxic activity against HeLa and HepG2 cancer cell lines with IC50>50 μg mL(- 1).

Synthesis, Antiviral and Cytotoxic Activity of Novel Terpenyl Hybrid Molecules Prepared by Click Chemistry.

PubMed

Pertino, Mariano Walter; Petrera, Erina; Alché, Laura Edith; Schmeda-Hirschmann, Guillermo

2018-06-03

Naturally occurring terpenes were combined by click reactions to generate sixteen hybrid molecules. The diterpene imbricatolic acid (IA) containing an azide group was used as starting compound for the synthesis of all the derivatives. The alkyne group in the terpenes cyperenoic acid, dehydroabietinol, carnosic acid γ-lactone, ferruginol, oleanolic acid and aleuritolic acid was obtained by esterification using appropriate alcohols or acids. The hybrid compounds were prepared by combining the IA azide function with the different terpene-alkynes under click chemistry conditions. The cytotoxic activity of the terpene hybrids 1 ⁻ 16 was assessed against Vero cells and tumour cell lines (HEP-2, C6 and Raw 264.7). Compounds 1 , 2 , 3 and 7 showed cytotoxic activity against the tested cell lines. The antiviral activity of the compounds was evaluated against HSV-1 KOS, Field and B2006 strain. For the pairs of hybrid compounds formed between IA-diterpene (compounds 3 ⁻ 8 , except for compound 7 ), a moderate activity was observed against the three HSV-1 strains with an interesting selectivity index (SI ≥10, SI = CC 50 /CE 50 ) for some compounds.

Stimulant Paste Preparation and Bark Streak Tapping Technique for Pine Oleoresin Extraction.

PubMed

Füller, Thanise Nogueira; de Lima, Júlio César; de Costa, Fernanda; Rodrigues-Corrêa, Kelly C S; Fett-Neto, Arthur G

2016-01-01

Tapping technique comprises the extraction of pine oleoresin, a non-wood forest product consisting of a complex mixture of mono, sesqui, and diterpenes biosynthesized and exuded as a defense response to wounding. Oleoresin is used to produce gum rosin, turpentine, and their multiple derivatives. Oleoresin yield and quality are objects of interest in pine tree biotechnology, both in terms of environmental and genetic control. Monitoring these parameters in individual trees grown in the field provides a means to examine the control of terpene production in resin canals, as well as the identification of genetic-based differences in resinosis. A typical method of tapping involves the removal of bark and application of a chemical stimulant on the wounded area. Here we describe the methods for preparing the resin-stimulant paste with different adjuvants, as well as the bark streaking process in adult pine trees.

Structure activity relationship of phenolic diterpenes from Salvia officinalis as activators of the nuclear factor E2-related factor 2 pathway

PubMed Central

Fischedick, Justin T; Standiford, Miranda; Johnson, Delinda A.; Johnson, Jeffrey A.

2013-01-01

Nuclear factor E2-related factor 2 (Nrf2) is a transcription factor known to activate cytoprotective genes which may be useful in the treatment of neurodegenerative disease. In order to better understand the structure activity relationship of phenolic diterpenes from Salvia officinalis L., we isolated carnosic acid, carnosol, epirosmanol, rosmanol, 12-methoxy-carnosic acid, sageone, and carnosaldehyde using polyamide column, centrifugal partition chromatography, and semi-preparative high performance liquid chromatography. Isolated compounds were screened in-vitro for their ability to active the Nrf2 and general cellular toxicity using mouse primary cortical cultures. All compounds except 12-methoxy-carnosic acid were able to activate the antioxidant response element. Furthermore both carnosol and carnoasldehyde were able to induce Nrf2-dependent gene expression as well as protect mouse primary cortical neuronal cultures from H2O2 induced cell death. PMID:23507152

Antimicrobial monomeric and dimeric diterpenes from the leaves of Helichrysum tenax var tenax.

PubMed

Drewes, Siegfried E; Mudau, K Esther; van Vuuren, Sandy F; Viljoen, Alvaro M

2006-04-01

The hexane extract of fresh air-dried leaves of Helichrysum tenax (Asteraceae) afforded ent-beyer-15-en-19-ol (1), its 4-epimer ent-beyer-15-en-18-ol (2), 15beta,16beta-epoxide-ent-beyeran-19-ol (3), as well as (4) consisting of two units of (1) linked as a diester of malonic acid, and (5), a compound. Its constituents are (1) and (3) also linked as a diester of malonic acid. The leaves of the plant are densely covered in fine glandular trichomes. These are extremely sticky and exude a mixture of the above diterpenes. Antimicrobial tests showed that (1), in particular, was highly active (3.1 and 3.6 microg/ml) against Bacillus cereus and Staphylococcus epidermidis, respectively.

Indole-diterpenes and ergot alkaloids in Cynodon dactylon (Bermuda grass) infected with Claviceps cynodontis from an outbreak of tremors in cattle.

PubMed

Uhlig, Silvio; Botha, Christo J; Vrålstad, Trude; Rolén, Elin; Miles, Christopher O

2009-12-09

Tremorgenic syndromes in mammals are commonly associated with indole-diterpenoid alkaloids of fungal origin. Cattle are sometimes affected by tremors (also called "staggers") when they graze on toxic grass pastures, and Bermuda grass ( Cynodon dactylon , kweek) has been known to be associated with tremors for several decades. This study reports the identification of paspalitrems and paspaline-like indole-diterpenes in the seedheads of Claviceps cynodontis -infected Bermuda grass collected from a pasture that had caused a staggers syndrome in cattle in South Africa and thereby links the condition to specific mycotoxins. The highest concentration (about 150 mg/kg) was found for paspalitrem B. Ergonovine and ergine (lysergic acid amide), together with their C-8 epimers, were found to co-occur with the indole-diterpenes at concentrations of about 10 microg/kg. The indole-diterpene profile of the extract from the ergotized Bermuda grass was similar to that of Claviceps paspali sclerotia. However, the C. paspali sclerotia contained in addition agroclavine and elymoclavine. This is the first study linking tremors associated with grazing of Bermuda grass to specific tremorgenic indole-diterpenoid mycotoxins.

Acetylcholine esterase inhibitors and melanin synthesis inhibitors from Salvia officinalis.

PubMed

Sallam, Amal; Mira, Amira; Ashour, Ahmed; Shimizu, Kuniyoshi

2016-09-15

Salvia officinalis is a traditionally used herb with a wide range of medicinal applications. Many phytoconstituents have been isolated from S. officinalis, mainly phenolic diterpenes, which possess many biological activities. This study aimed to evaluate the ability of the phenolic diterpenes of S. officinalis to inhibit acetylcholine esterase (AChE) as well as their ability to inhibit melanin biosynthesis in B16 melanoma cells. The phenolic diterpenes isolated from the aerial parts of S. officinalis were tested for their effect on melanin biosynthesis in B16 melanoma cell lines. They were also tested for their ability to inhibit AChE using Ellman's method. Moreover, a molecular docking experiment was used to investigate the binding affinity of the isolated phenolic diterpenes to the amino acid residues at the active sites of AChE. Seven phenolic diterpenes-sageone, 12-methylcarnosol, carnosol, 7b-methoxyrosmanol, 7a-methoxyrosmanol, isorosmanol and epirosmanol-were isolated from the methanolic extract of the aerial parts of S. officinalis. Isorosmanol showed a melanin-inhibiting activity as potent as that of arbutin. Compounds 7a-methoxyrosmanol and isorosmanol inhibited AChE activity by 50% and 65%, respectively, at a concentration of 500 µM. The results suggest that isorosmanol is a promising natural compound for further studies on development of new medications which might be useful in ageing disorders such as the declining of cognitive functions and hyperpigmentation. Copyright © 2016 Elsevier GmbH. All rights reserved.

Relaxant effect of Ent-7α-hydroxytrachyloban-18-oic acid, a trachylobane diterpene from Xylopia langsdorfiana A. St-Hil. & Tul., on tracheal smooth muscle.

PubMed

Martins, Italo R R; Dos Santos, Rosimeire F; de C Correia, Ana C; de Oliveira, Gislaine A; Macêdo, Cibério L; de S Monteiro, Fabio; Dos Santos, Paula F; de A Cavalcante, Fabiana; Tavares, Josean F; da Silva, Bagnólia A

2013-01-01

Ent-7α-hydroxytrachyloban-18-oic acid, a trachylobane diterpene from Xylopia langsdorfiana, has previously been shown to relax the guinea-pig trachea in a concentration-dependent manner. In this study we aimed to elucidate the mechanisms underlying this action and so contribute to the discovery of natural products with therapeutic potential. A possible interaction between diterpene and the Ca(2+)-calmodulin complex was eliminated as chlorpromazine (10(-6) M), a calmodulin inhibitor, did not significantly alter the diterpene-induced relaxation (pD2 = 4.38 ± 0.07 and 4.25 ± 0.07; mean ± S.E.M., n=5). Trachylobane-318 showed a higher relaxant potency when the trachea was contracted by 18 mM KCl than it did with 60 mM KCl (pD2 = 4.90 ± 0.25 and 3.88 ± 0.01, n=5), suggesting the possible activation of K(+) channels. This was confirmed, as in the presence of 10 mM TEA(+) (a non-selective K(+) channel blocker), diterpene relaxation potency was significantly reduced (pD2 = 4.38 ± 0.07 to 4.01 ± 0.06, n=5). Furthermore, K(+) channel subtypes KATP, KV, SKCa and BKCa seem to be modulated positively by trachylobane-318 (pD2 = 3.91 ± 0.003, 4.00 ± 0.06, 3.45 ± 0.14 and 3.80 ± 0.05, n=5) but not the Kir subtype channel (pD2 = 4.15 ± 0.10, n=5). Cyclic nucleotides were not involved as the relaxation due to aminophylline (pD2 = 4.27 ± 0.09, n=5) was not altered in the presence of 3 × 10(-5) M trachylobane-318 (pD2 = 4.46 ± 0.08, n=5). Thus, at a functional level, trachylobane-318 seems to relax the guinea-pig trachea by positive modulation of K(+) channels, particularly the KATP, KV, SKCa and BKCa subtypes.

Relaxant effect of Ent‑7α‑hydroxytrachyloban‑18-oic acid, a trachylobane diterpene from Xylopia langsdorfiana A. St-Hil. & Tul., on tracheal smooth muscle

PubMed Central

Martins, Italo R. R.; dos Santos, Rosimeire F.; Correia, Ana C. de C.; de Oliveira, Gislaine A.; Macêdo, Cibério L.; Monteiro, Fabio de S.; dos Santos, Paula F.; Cavalcante, Fabiana de A.; Tavares, Josean F.; da Silva, Bagnólia A.

2013-01-01

Ent-7α-hydroxytrachyloban-18-oic acid, a trachylobane diterpene from Xylopia langsdorfiana, has previously been shown to relax the guinea-pig trachea in a concentration-dependent manner. In this study we aimed to elucidate the mechanisms underlying this action and so contribute to the discovery of natural products with therapeutic potential. A possible interaction between diterpene and the Ca2+-calmodulin complex was eliminated as chlorpromazine (10-6 M), a calmodulin inhibitor, did not significantly alter the diterpene-induced relaxation (pD2 = 4.38 ± 0.07 and 4.25 ± 0.07; mean ± S.E.M., n=5). Trachylobane-318 showed a higher relaxant potency when the trachea was contracted by 18 mM KCl than it did with 60 mM KCl (pD2 = 4.90 ± 0.25 and 3.88 ± 0.01, n=5), suggesting the possible activation of K+ channels. This was confirmed, as in the presence of 10 mM TEA+ (a non-selective K+ channel blocker), diterpene relaxation potency was significantly reduced (pD2 = 4.38 ± 0.07 to 4.01 ± 0.06, n=5). Furthermore, K+ channel subtypes KATP, KV, SKCa and BKCa seem to be modulated positively by trachylobane-318 (pD2 = 3.91 ± 0.003, 4.00 ± 0.06, 3.45 ± 0.14 and 3.80 ± 0.05, n=5) but not the Kir subtype channel (pD2 = 4.15 ± 0.10, n=5). Cyclic nucleotides were not involved as the relaxation due to aminophylline (pD2 = 4.27 ± 0.09, n=5) was not altered in the presence of 3 × 10-5 M trachylobane-318 (pD2 = 4.46 ± 0.08, n=5). Thus, at a functional level, trachylobane-318 seems to relax the guinea-pig trachea by positive modulation of K+ channels, particularly the KATP, KV, SKCa and BKCa subtypes. PMID:23832615

Overexpression of an Isoprenyl Diphosphate Synthase in Spruce Leads to Unexpected Terpene Diversion Products That Function in Plant Defense1[W][OPEN

PubMed Central

Nagel, Raimund; Berasategui, Aileen; Paetz, Christian; Gershenzon, Jonathan; Schmidt, Axel

2014-01-01

Spruce (Picea spp.) and other conifers employ terpenoid-based oleoresin as part of their defense against herbivores and pathogens. The short-chain isoprenyl diphosphate synthases (IDS) are situated at critical branch points in terpene biosynthesis, producing the precursors of the different terpenoid classes. To determine the role of IDS and to create altered terpene phenotypes for assessing the defensive role of terpenoids, we overexpressed a bifunctional spruce IDS, a geranyl diphosphate and geranylgeranyl diphosphate synthase in white spruce (Picea glauca) saplings. While transcript level (350-fold), enzyme activity level (7-fold), and in planta geranyl diphosphate and geranylgeranyl diphosphate levels (4- to 8-fold) were significantly increased in the needles of transgenic plants, there was no increase in the major monoterpenes and diterpene acids of the resin and no change in primary isoprenoids, such as sterols, chlorophylls, and carotenoids. Instead, large amounts of geranylgeranyl fatty acid esters, known from various gymnosperm and angiosperm plant species, accumulated in needles and were shown to act defensively in reducing the performance of larvae of the nun moth (Lymantria monacha), a conifer pest in Eurasia. These results show the impact of overexpression of an IDS and the defensive role of an unexpected accumulation product of terpenoid biosynthesis with the potential for a broader function in plant protection. PMID:24346420

Cerumen of Australian stingless bees ( Tetragonula carbonaria): gas chromatography-mass spectrometry fingerprints and potential anti-inflammatory properties

NASA Astrophysics Data System (ADS)

Massaro, Flavia Carmelina; Brooks, Peter Richard; Wallace, Helen Margaret; Russell, Fraser Donald

2011-04-01

Cerumen, or propolis, is a mixture of plant resins enriched with bee secretions. In Australia, stingless bees are important pollinators that use cerumen for nest construction and possibly for colony's health. While extensive research attests to the therapeutic properties of honeybee ( Apis mellifera) propolis, the biological and medicinal properties of Australian stingless bee cerumen are largely unknown. In this study, the chemical and biological properties of polar extracts of cerumen from Tetragonula carbonaria in South East Queensland, Australia were investigated using gas chromatography-mass spectrometry (GC-MS) analyses and in vitro 5-lipoxygenase (5-LOX) cell-free assays. Extracts were tested against comparative (commercial tincture of A. mellifera propolis) and positive controls (Trolox and gallic acid). Distinct GC-MS fingerprints of a mixed diterpenic profile typical of native bee cerumen were obtained with pimaric acid (6.31 ± 0.97%, w/w), isopimaric acid (12.23 ± 3.03%, w/w), and gallic acid (5.79 ± 0.81%, w/w) tentatively identified as useful chemical markers. Characteristic flavonoids and prenylated phenolics found in honeybee propolis were absent. Cerumen extracts from T. carbonaria inhibited activity of 5-LOX, an enzyme known to catalyse production of proinflammatory mediators (IC50 19.97 ± 2.67 μg/ml, mean ± SEM, n = 4). Extracts had similar potency to Trolox (IC50 12.78 ± 1.82 μg/ml), but were less potent than honeybee propolis (IC50 5.90 ± 0.62 μg/ml) or gallic acid (IC50 5.62 ± 0.35 μg/ml, P < 0.001). These findings warrant further investigation of the ecological and medicinal properties of this stingless bee cerumen, which may herald a commercial potential for the Australian beekeeping industry.

Antimicrobial properties of some West African medicinal plants iv. Antimicrobial activity of xylopic acid and other constituente of the fruits of Xylopia aethiopica (Annonaceae).

PubMed

Boakye-Yiadom, K; Fiagbe, N I; Ayim, J S

1977-01-01

Xylopic acid and four other isolates from the fresh ripe fruits of Xylopia aethiopica a common ingredient in several Ghanaian folklore medicines and foods, have been examined for antimicrobial activity against five micro-organisms, Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Pseudomonas aeruginosa and Candida albicans. Xylopic acid and two other diterpene isolates were found to have antimicrobial properties.

Changes in fats and resins of Pinus radiata associated with heartwood formation

Treesearch

Richard W. Hemingway; W.E. Hillis

1971-01-01

In an analysis of Australian grown P. radiata marked changes were found in the relative proportions and compositions of the resin acids, fatty acids, and fatty acid esters associated with heartwood formation. While the proportion of resin acids increased substantially in the heartwood, there was little change in resin acid composition from outer...

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Partial phosphoric acid esters of polyester resins... of polyester resins. Partial phosphoric acid esters of polyester resins identified in this section... prescribed conditions: (a) For the purpose of this section, partial phosphoric acid esters of polyester...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2010 CFR

2010-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2013 CFR

2013-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2013-04-01 2013-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2014 CFR

2014-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2014-04-01 2014-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2012 CFR

2012-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2012-04-01 2012-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 573.120 - Acrylamide-acrylic acid resin.

Code of Federal Regulations, 2011 CFR

2011-04-01

...) ANIMAL DRUGS, FEEDS, AND RELATED PRODUCTS FOOD ADDITIVES PERMITTED IN FEED AND DRINKING WATER OF ANIMALS Food Additive Listing § 573.120 Acrylamide-acrylic acid resin. Acrylamide-acrylic acid resin... 21 Food and Drugs 6 2011-04-01 2011-04-01 false Acrylamide-acrylic acid resin. 573.120 Section 573...

21 CFR 176.110 - Acrylamide-acrylic acid resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Acrylamide-acrylic acid resins. 176.110 Section... Substances for Use Only as Components of Paper and Paperboard § 176.110 Acrylamide-acrylic acid resins. Acrylamide-acrylic acid resins may be safely used as components of articles intended for use in producing...

21 CFR 176.110 - Acrylamide-acrylic acid resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Acrylamide-acrylic acid resins. 176.110 Section 176... Substances for Use Only as Components of Paper and Paperboard § 176.110 Acrylamide-acrylic acid resins. Acrylamide-acrylic acid resins may be safely used as components of articles intended for use in producing...

ent-Trachylobane diterpenoids from Xylopia langsdorffiana.

PubMed

Tavares, Josean Fechine; Queiroga, Karine F; Silva, Marianna Vieira B; Diniz, Margareth F F M; Filho, José M B; da-Cunha, Emidio V L; de Simone, Carlos Alberto; Júnior, João X de Araújo; Melo, Patrícia S; Haun, Marcela; da Silva, Marcelo Sobral

2006-06-01

Two new diterpenes of the ent-trachylobane type were isolated from the stems of Xylopia langsdorffiana, ent-7alpha-acetoxytrachyloban-18-oic acid (1) and ent-7alpha-hydroxytrachyloban-18-oic acid (2). The structures of these isolates were deduced by spectroscopic data interpretation. X-ray crystallography of 1 was used to confirm its structure. The cytotoxic activity of 1 against V79 fibroblasts and rat hepatocytes was investigated.

Reference Genes for qPCR Analysis in Resin-Tapped Adult Slash Pine As a Tool to Address the Molecular Basis of Commercial Resinosis

PubMed Central

de Lima, Júlio C.; de Costa, Fernanda; Füller, Thanise N.; Rodrigues-Corrêa, Kelly C. da Silva; Kerber, Magnus R.; Lima, Mariano S.; Fett, Janette P.; Fett-Neto, Arthur G.

2016-01-01

Pine oleoresin is a major source of terpenes, consisting of turpentine (mono- and sesquiterpenes) and rosin (diterpenes) fractions. Higher oleoresin yields are of economic interest, since oleoresin derivatives make up a valuable source of materials for chemical industries. Oleoresin can be extracted from living trees, often by the bark streak method, in which bark removal is done periodically, followed by application of stimulant paste containing sulfuric acid and other chemicals on the freshly wounded exposed surface. To better understand the molecular basis of chemically-stimulated and wound induced oleoresin production, we evaluated the stability of 11 putative reference genes for the purpose of normalization in studying Pinus elliottii gene expression during oleoresinosis. Samples for RNA extraction were collected from field-grown adult trees under tapping operations using stimulant pastes with different compositions and at various time points after paste application. Statistical methods established by geNorm, NormFinder, and BestKeeper softwares were consistent in pointing as adequate reference genes HISTO3 and UBI. To confirm expression stability of the candidate reference genes, expression profiles of putative P. elliottii orthologs of resin biosynthesis-related genes encoding Pinus contorta β-pinene synthase [PcTPS-(−)β-pin1], P. contorta levopimaradiene/abietadiene synthase (PcLAS1), Pinus taeda α-pinene synthase [PtTPS-(+)αpin], and P. taeda α-farnesene synthase (PtαFS) were examined following stimulant paste application. Increased oleoresin yields observed in stimulated treatments using phytohormone-based pastes were consistent with higher expression of pinene synthases. Overall, the expression of all genes examined matched the expected profiles of oleoresin-related transcript changes reported for previously examined conifers. PMID:27379135

Reference Genes for qPCR Analysis in Resin-Tapped Adult Slash Pine As a Tool to Address the Molecular Basis of Commercial Resinosis.

PubMed

de Lima, Júlio C; de Costa, Fernanda; Füller, Thanise N; Rodrigues-Corrêa, Kelly C da Silva; Kerber, Magnus R; Lima, Mariano S; Fett, Janette P; Fett-Neto, Arthur G

2016-01-01

Pine oleoresin is a major source of terpenes, consisting of turpentine (mono- and sesquiterpenes) and rosin (diterpenes) fractions. Higher oleoresin yields are of economic interest, since oleoresin derivatives make up a valuable source of materials for chemical industries. Oleoresin can be extracted from living trees, often by the bark streak method, in which bark removal is done periodically, followed by application of stimulant paste containing sulfuric acid and other chemicals on the freshly wounded exposed surface. To better understand the molecular basis of chemically-stimulated and wound induced oleoresin production, we evaluated the stability of 11 putative reference genes for the purpose of normalization in studying Pinus elliottii gene expression during oleoresinosis. Samples for RNA extraction were collected from field-grown adult trees under tapping operations using stimulant pastes with different compositions and at various time points after paste application. Statistical methods established by geNorm, NormFinder, and BestKeeper softwares were consistent in pointing as adequate reference genes HISTO3 and UBI. To confirm expression stability of the candidate reference genes, expression profiles of putative P. elliottii orthologs of resin biosynthesis-related genes encoding Pinus contorta β-pinene synthase [PcTPS-(-)β-pin1], P. contorta levopimaradiene/abietadiene synthase (PcLAS1), Pinus taeda α-pinene synthase [PtTPS-(+)αpin], and P. taeda α-farnesene synthase (PtαFS) were examined following stimulant paste application. Increased oleoresin yields observed in stimulated treatments using phytohormone-based pastes were consistent with higher expression of pinene synthases. Overall, the expression of all genes examined matched the expected profiles of oleoresin-related transcript changes reported for previously examined conifers.

A screening method for cardiovascular active compounds in marine algae.

PubMed

Agatonovic-Kustrin, S; Kustrin, E; Angove, M J; Morton, D W

2018-05-18

The interaction of bioactive compounds from ethanolic extracts of selected marine algae samples, separated on chromatographic plates, with nitric/nitrous acid was investigated. The nature of bioactive compounds in the marine algae extracts was characterised using UV absorption spectra before and after reaction with diluted nitric acid, and from the characteristic colour reaction after derivatization with anisaldehyde. It was found that diterpenes from Dictyota dichotoma, an edible brown algae, and sterols from green algae Caulerpa brachypus, bind nitric oxide and may act as a nitric oxide carrier. Although the carotenoid fucoxanthin, found in all brown marine algae also binds nitric oxide, the bonds between nitrogen and the fucoxanthin molecule are much stronger. Further studies are required to evaluate the effects of diterpenes from Dictyota dichotoma and sterols from green algae Caulerpa brachypus to see if they have beneficial cardiovascular effects. The method reported here should prove useful in screening large numbers of algae species for compounds with cardiovascular activity. Copyright © 2018 Elsevier B.V. All rights reserved.

ent-Copalic acid antibacterial and anti-biofilm properties against Actinomyces naeslundii and Peptostreptococcus anaerobius.

PubMed

Souza, Maria Gorete Mendes de; Leandro, Luís Fernando; Moraes, Thaís da Silva; Abrão, Fariza; Veneziani, Rodrigo Cassio Sola; Ambrosio, Sergio Ricardo; Martins, Carlos Henrique Gomes

2018-05-28

Diterpenes are an important class of plant metabolites that can be used in the search for new antibacterial agents. ent-Copalic acid (CA), the major diterpene in Copaifera species exudates, displays several pharmacological properties. This study evaluates the CA antibacterial potential against the anaerobic bacteria Peptostreptococcus anaerobius and Actinomyces naeslundii. Antimicrobial assays included time-kill and biofilm inhibition and eradication assays. Time-kill assays conducted for CA concentrations between 6.25 and 12.5 μg/mL evidenced bactericidal activity within 72 h. CA combined with chlorhexidine dihydrochloride (CHD) exhibited bactericidal action against P. anaerobius within 6 h of incubation. As for A. naeslundii, the same combination reduced the number of microorganisms by over 3 log10 at 24 h and exerted a bactericidal effect at 48 h of incubation. CA at 500 and 2000 μg/mL inhibited P. anaerobius and A. naeslundii biofilm formation by at least 50%, respectively. CA at 62.5 and 1.000 μg/mL eradicated 99.9% of pre-formed P. anaerobius and A. naeslundii biofilms, respectively. These results indicated that CA presents in vitro antibacterial activity and is a potential biofilm inhibitory agent. This diterpene may play an important role in the search for novel sources of agents that can act against anaerobic bacteria. Copyright © 2018 Elsevier Ltd. All rights reserved.

Biodegradation of resin acid sodium salts

Treesearch

Richard W. Hemingway; H. Greaves

1973-01-01

The sodium salts of resin acids were readily degraded by microflora from two types of river water and from an activated sewage sludge. A lag phase with little or no resin acid salt degradation but rapid bacterial development occurred which was greatly extended by a decrease in incubation temperature. After this initial lag phase, the resin acid salts were rapidly...

Automated protein hydrolysis delivering sample to a solid acid catalyst for amino acid analysis.

PubMed

Masuda, Akiko; Dohmae, Naoshi

2010-11-01

In this study, we developed an automatic protein hydrolysis system using strong cation-exchange resins as solid acid catalysts. Examining several kinds of inorganic solid acids and cation-exchange resins, we found that a few cation-exchange resins worked as acid catalysts for protein hydrolysis when heated in the presence of water. The most efficient resin yielded amounts of amino acids that were over 70% of those recovered after conventional hydrolysis with hydrochloric acid and resulted in amino acid compositions matching the theoretical values. The solid-acid hydrolysis was automated by packing the resin into columns, combining the columns with a high-performance liquid chromatography system, and heating them. The amino acids that constitute a protein can thereby be determined, minimizing contamination from the environment.

Prediction of anticancer activity of diterpenes isolated from the paraiban flora through a PLS model and molecular surfaces.

PubMed

Scotti, Luciana; Scotti, Marcus T; Ishiki, Hamilton; Junior, Francisco J B M; dos, Santos Paula F; Tavares, Josean F; da Silva, Marcelo S

2014-05-01

The aim of this work was to predict the anticancer potential of 3 atisane, and 3 trachylobane diterpene compounds extracted from the roots of Xylopia langsdorffiana. The prediction of anticancer activity as expressed against PC-3 tumor cells was made using a PLS model built with 26 diterpenes in the training set. Significant statistical measures were obtained. The six investigated diterpenes were applied to the model and their activities against PC-3 cells were calculated. All the diterpenes were active, with atisane diterpenes showing the higher pICso values. In human prostate carcinoma PC-3 cells, the apoptosis mechanism is related to an inhibition of IKK/NF-KB. Antioxidant potential implies a greater electronic molecular atmosphere (increased donor electron capacity), which can reduce radical reactivity, and facilitate post donation charge accommodation. Molecular surfaces indicated a much greater electronic cloud over atisane diterpenes.

Scoparic acid A, a beta-glucuronidase inhibitor from Scoparia dulcis.

PubMed

Hayashi, T; Kawasaki, M; Okamura, K; Tamada, Y; Morita, N; Tezuka, Y; Kikuchi, T; Miwa, Y; Taga, T

1992-12-01

The 70% EtOH extract of Scoparia dulcis showed inhibitory activity against beta-glucuronidase from bovine liver. Bioassay-directed fractionation of the active extract led to the isolation of three labdane-type diterpene acids, scoparic acid A [1] [6-benzoyl-12-hydroxy-labda-8(17), 13-dien-18-oic acid], scoparic acid B [2] [6-benzoyl-14,15-dinor-13-oxo-8(17)-labden-18-oic acid], and scoparic acid C [3] [6-benzoyl-15-nor-14-oxo-8(17)-labden-18-oic acid], the structures of which were established by spectral means, including X-ray analysis. Scoparic acid A was found to be a potent beta-glucuronidase inhibitor.

Biota: sediment partitioning of aluminium smelter related PAHs and pulp mill related diterpenes by intertidal clams at Kitimat, British Columbia.

PubMed

Yunker, Mark B; Lachmuth, Cara L; Cretney, Walter J; Fowler, Brian R; Dangerfield, Neil; White, Linda; Ross, Peter S

2011-09-01

The question of polycyclic aromatic hydrocarbon (PAH) bioavailability and its relationship to specific PAH sources with different PAH binding characteristics is an important one, because bioavailability drives PAH accumulation in biota and ultimately the biochemical responses to the PAH contaminants. The industrial harbour at Kitimat (British Columbia, Canada) provides an ideal location to study the bioavailability and bioaccumulation of sediment hydrocarbons to low trophic level biota. Samples of soft shell clams (Mya arenaria) and intertidal sediment collected from multiple sites over six years at various distances from an aluminium smelter and a pulp and paper mill were analysed for 106 PAHs, plant diterpenes and other aromatic fraction hydrocarbons. Interpretation using PAH source ratios and multivariate data analysis reveals six principal hydrocarbon sources: PAHs in coke, pitch and emissions from anode combustion from the aluminium smelter, vascular plant terpenes and aromatised terpenes from the pulp and paper mill, petroleum PAHs from shipping and other anthropogenic activities and PAHs from natural plant detritus. Harbour sediments predominantly contain either pitch or pyrogenic PAHs from the smelter, while clams predominantly contain plant derived PAHs and diterpenes from the adjacent pulp mill. PAHs from the smelter have low bioavailability to clams (Biota-Sediment Accumulation Factors; BSAFs <1 for pitch and coke; <10 for anode combustion, decreasing to ∼0.1 for the mass 300 and 302 PAHs), possibly due to binding to pitch or soot carbon matrices. Decreases in PAH isomer ratios between sediments and clams likely reflect a combination of variation in uptake kinetics of petroleum PAHs and compound specific metabolism, with the importance of petroleum PAHs decreasing with increasing molecular weight. Plant derived compounds exhibit little natural bioaccumulation at reference sites, but unsaturated and aromatised diterpenes released from resins by industrial pulping processes are readily accumulated by the clams (BSAFs >500). Thus while most of the smelter associated PAHs in sediments may not be bioavailable to benthic organisms, the plant terpenes (including retene, totarol, ferruginol, manool, dehydroabietane and other plant terpenes that form the chemical defence mechanism of conifers) released by pulp mills are bioavailable and possess demonstrated toxic properties. The large scale release of plant terpenes by some of the many pulp mills located in British Columbia and elsewhere represents a largely undocumented risk to aquatic biota. Copyright © 2011 Elsevier Ltd. All rights reserved.

40 CFR 414.40 - Applicability; description of the thermoplastic resins subcategory.

Code of Federal Regulations, 2010 CFR

2010-07-01

... *Ethylene-Methacrylic Acid Copolymers *Ethylene-Vinyl Acetate Copolymers *Fatty Acid Resins *Fluorocarbon..., Acrylates (Latex) *PVC Copolymers, Ethylene-Vinyl Chloride *Rosin Derivative Resins *Rosin Modified Resins...

An Unusual Diterpene-Enhygromic Acid and Deoxyenhygrolides from a Marine Myxobacterium, Enhygromyxa sp.

PubMed

Tomura, Tomohiko; Nagashima, Shiori; Yamazaki, Satoshi; Iizuka, Takashi; Fudou, Ryosuke; Ojika, Makoto

2017-04-06

Three new compounds, enhygromic acid ( 1 ) and deoxyenhygrolides A ( 2 ) and B ( 3 ), were isolated from a marine myxobacterium, Enhygromyxa sp. Compound 1 was found to be an acrylic acid derivative with a rare polycyclic carbon skeleton, decahydroacenaphthylene, by spectroscopic analyses. Compounds 2 and 3 were deoxy analogs of the known γ-alkylidenebutenolides, enhygrolides. Compound 1 exhibited cytotoxicity against B16 melanoma cells and anti-bacterial activity against Bacillus subtilis , and enhanced the NGF-induced neurite outgrowth of PC12 cells.

Bifunctional phenyl monophosphonic/sulfonic acid ion exchange resin and process for using the same

DOEpatents

Alexandratos, Spiro; Shelley, Christopher A.; Horwitz, E. Philip; Chiarizia, Renato

2001-01-01

A cross-linked water-insoluble ion exchange resin comprised of polymerized monomers having a phenyl ring is disclosed. A contemplated resin contains (i) polymerized phenyl ring-containing monomers having a phosphonic acid ligand linked to the phenyl ring, (ii) about 2 to about 5 millimoles per gram (mmol/g) of phosphorus as phosphonic acid ligands, and (iii) a sufficient amount of a sulfonic acid ligand such that the ratio of mmol/g of phosphonic acid to mmol/g sulfonic acid is up to 3:1. A process for removing polyvalent metal cations from aqueous solution, and a process for removing iron(III) cations from acidic copper(II) cation-containing solutions that utilize the contemplated resin or other resins are disclosed.

Bifunctional phenyl monophosphonic/sulfonic acid ion exchange resin and process for using the same

DOEpatents

Alexandratos, Spiro; Shelley, Christopher A.; Horwitz, E. Philip; Chiarizia, Renato; Gula, Michael J.; Xue, Sui; Harvey, James T.

2002-01-01

A cross-linked water-insoluble ion exchange resin comprised of polymerized monomers having a phenyl ring is disclosed. A contemplated resin contains (i) polymerized phenyl ring-containing monomers having a phosphonic acid ligand linked to the phenyl ring, (ii) about 2 to about 5 millimoles per gram (mmol/g) of phosphorus as phosphonic acid ligands, and (iii) a sufficient amount of a sulfonic acid ligand such that the ratio of mmol/g of phosphonic acid to mmol/g sulfonic acid is up to 3:1. A process for removing polyvalent metal cations from aqueous solution, and a process for removing iron(III) cations from acidic copper(II) cation-containing solutions that utilize the contemplated resin or other resins are disclosed.

Reaction catalysts of urea-formaldehyde resin, as related to strength properties of southern pine particleboard

Treesearch

C. -Y. Hse

1974-01-01

Twelve resins were formulated with factorial combinations of three alkaline catalysts (i.e., somdium hydroxide, hexamethylenetetramine, and triethanolamine) and four acidic catalysts (i.e., acetic acid, hydrochloric acid, ammonium chloride, and phosphoric acid). The resins were replicated.

Resin–dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding

PubMed Central

Sauro, Salvatore; Toledano, Manuel; Aguilera, Fatima Sánchez; Mannocci, Francesco; Pashley, David H.; Tay, Franklin R.; Watson, Timothy F.; Osorio, Raquel

2013-01-01

Objective To compare resin–dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique. Methods Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H3PO4 (15 s) or 0.1 M EDTA (60 s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20 s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24 h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B. Results The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin. Significance The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H3PO4 acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period. PMID:20074787

Cloning and expression of a CYP720B orthologue involved in the biosynthesis of diterpene resin acids in Pinus brutia.

PubMed

Semiz, Asli; Sen, Alaattin

2015-03-01

Cytochrome P450 monooxygenases mediate a broad range of oxidative reactions involved in the biosynthesis of both primary and secondary metabolites in plants. Until now, only two P450 genes, CYP720B1 from Pinus taeda and CYP720B4 from Picea sitchensis, have been functionally characterised and described in the literature. The purpose of this study was to describe the cloning and expression of CYP720B from Pinus brutia due to its suggested role in the synthesis of bioactive compounds used for chemical defence against insects. A PCR product of the P. brutia CYP720B gene was cloned into the pCR8/GW/TOPO cloning vector. After optimising the sequence for codon usage in yeast, it was transferred into the inducible expression vector pYES-DEST52 and transfected into the S. cerevisiae INVSc1 strain. Sequence analysis showed that the P. brutia CYP720B gene contains an open reading frame of 1,464 nucleotides, which encodes a 53,570 Da putative protein of 487 amino acid residues. The putative protein contains the classic heme-binding sequence motif that is conserved in all P450 enzymes. It shares 99 and 61% identity with the deduced amino acid sequences of CYP720B1 from Pinus taeda and CYP720B4 from Picea sitchensis, respectively. Recombinant CYP720B protein expression was confirmed using western blot analysis. Furthermore, recombinant CYP720B was functionally active, showing a Soret peak at approximately 448 nm in the reduced CO difference spectra. These data suggest that the cloned gene is an orthologue of CYP720B in P. brutia and might be involved in DRA biosynthesis.

Analgesic effects of an ethanol extract of the fruits of Xylopia aethiopica (Dunal) A. Rich (Annonaceae) and the major constituent, xylopic acid in murine models.

PubMed

Woode, Eric; Ameyaw, Elvis O; Boakye-Gyasi, Eric; Abotsi, Wonder K M

2012-10-01

Fruit extracts of Xylopia aethiopica are used traditionally in the management of pain disorders including rheumatism, headache, colic pain, and neuralgia. Little pharmacological data exists in scientific literature of the effect of the fruit extract and its major diterpene, xylopic acid, on pain. The present study evaluated the analgesic properties of the ethanol extract of X. aethiopica (XAE) and xylopic acid (XA), in murine models. XAE and XA were assessed in chemical (acetic acid-induced abdominal writhing and formalin tests), thermal (Tail-flick and Hargreaves thermal hyperalgesia tests), and mechanical (Randall-Selitto paw pressure test) pain models. XAE and XA exhibited significant analgesic activity in all the pain models used. XAE (30-300 mg kg(-1), p.o.) and XA (10-100 mg kg(-1), p.o.) inhibited acetic acid-induced visceral nociception, formalin- induced paw pain (both neurogenic and inflammatory), thermal pain as well as carrageenan-induced mechanical and thermal hyperalgesia in animals. Morphine (1-10 mg kg(-1), i.p.) and diclofenac (1-10 mg kg(-1), i.p.), used as controls, exhibited similar anti-nociceptive activities. XAE and XA did not induce tolerance to their respective anti-nociceptive effects in the formalin test after chronic administration. Morphine tolerance did not also cross-generalize to the analgesic effects of XAE or XA. These findings establish the analgesic properties of the ethanol fruit extract of X. aethiopica and its major diterpene, xylopic acid.

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an...

Environmentally Friendly Bio-Based Vinyl Ester Resins for Military Composite Structures

DTIC Science & Technology

2008-12-01

composites, fatty acid , vinyl ester 9. Distribution $tatement (requr’iedl lsmanuscript subjectto export control? E ruo I yes Circfe appropriate l tter and...resins is to replace some or all of the styrene with fatty acid -based monomers. These fatty acid vinyl ester resins allow for the formulation of high...validation studies have been performed, showing that the fatty acid -based resins have sufficient, modulus, strength, glass transition temperature, and

A UV resonance Raman (UVRR) spectroscopic study on the extractable compounds of Scots pine ( Pinus sylvestris) wood . Part I: Lipophilic compounds

NASA Astrophysics Data System (ADS)

Nuopponen, M.; Willför, S.; Jääskeläinen, A.-S.; Sundberg, A.; Vuorinen, T.

2004-11-01

The wood resin in Scots pine ( Pinus sylvestris) stemwood and branch wood were studied using UV resonance Raman (UVRR) spectroscopy. UVRR spectra of the sapwood and heartwood hexane extracts, solid wood samples and model compounds (six resin acids, three fatty acids, a fatty acid ester, sitosterol and sitosterol acetate) were collected using excitation wavelengths of 229, 244 and 257 nm. In addition, visible Raman spectra of the fatty and resin acids were recorded. Resin compositions of heartwood and sapwood hexane extracts were determined using gas chromatography. Raman signals of both conjugated and isolated double bonds of all the model compounds were resonance enhanced by UV excitation. The oleophilic structures showed strong bands in the region of 1660-1630 cm -1. Distinct structures were enhanced depending on the excitation wavelength. The UVRR spectra of the hexane extracts showed characteristic bands for resin and fatty acids. It was possible to identify certain resin acids from the spectra. UV Raman spectra collected from the solid wood samples containing wood resin showed a band at ˜1650 cm -1 due to unsaturated resin components. The Raman signals from extractives in the resin rich branch wood sample gave even more strongly enhanced signals than the aromatic lignin.

A UV resonance Raman (UVRR) spectroscopic study on the extractable compounds of Scots pine (Pinus sylvestris) wood. Part I: lipophilic compounds.

PubMed

Nuopponen, M; Willför, S; Jääskeläinen, A-S; Sundberg, A; Vuorinen, T

2004-11-01

The wood resin in Scots pine (Pinus sylvestris) stemwood and branch wood were studied using UV resonance Raman (UVRR) spectroscopy. UVRR spectra of the sapwood and heartwood hexane extracts, solid wood samples and model compounds (six resin acids, three fatty acids, a fatty acid ester, sitosterol and sitosterol acetate) were collected using excitation wavelengths of 229, 244 and 257 nm. In addition, visible Raman spectra of the fatty and resin acids were recorded. Resin compositions of heartwood and sapwood hexane extracts were determined using gas chromatography. Raman signals of both conjugated and isolated double bonds of all the model compounds were resonance enhanced by UV excitation. The oleophilic structures showed strong bands in the region of 1660-1630 cm(-1). Distinct structures were enhanced depending on the excitation wavelength. The UVRR spectra of the hexane extracts showed characteristic bands for resin and fatty acids. It was possible to identify certain resin acids from the spectra. UV Raman spectra collected from the solid wood samples containing wood resin showed a band at approximately 1650 cm(-1) due to unsaturated resin components. The Raman signals from extractives in the resin rich branch wood sample gave even more strongly enhanced signals than the aromatic lignin.

Quantitative evaluation of XAD-8 and XAD-4 resins used in tandem for removing organic solutes from water

USGS Publications Warehouse

Malcolm, R.L.; MacCarthy, P.

1992-01-01

The combined XAD-8 and XAD-4 resin procedure for the isolation of dissolved organic solutes from water was found to isolate 85% or more of the organic solutes from Lake Skjervatjern in Norway. Approximately 65% of the dissolved organic carbon (DOC) was first removed on XAD-8 resin, and then an additional 20% of the DOC was removed on XAD-4 resin. Approximately 15% of the DOC solutes (primarily hydrophilic neutrals) were not sorbed or concentrated by the procedure. Of the 65% of the solutes removed on XAD-8 resin, 40% were fulvic acids, 16% were humic acids, and 9% were hydrophobic neutrals. Approximately 20% of the hydrophilic solutes that pass through the XAD-8 resin were sorbed solutes on the second resin, XAD-4 (i.e., they were hydrophobic relative to the XAD-4 resin). The fraction sorbed on XAD-4 resin was called XAD-4 acids because it represented approximately 85-90% of the hydrophilic XAD-8 acid fraction according to the original XAD-8 fractionation procedure. The recovery of hydrophobic acids (fulvic acids and humic acids) and the hydrophobic neutral fraction from XAD-8 resin was essentially quantitative at 96%, 98%, and 86%, respectively. The recovery of XAD-4 acids from the XAD-4 resin was only about 50%. The exact reason for this moderately low recovery is unknown, but could result from ??-?? bonding between these organic solutes and the aromatic matrix of XAD-4. The hydrophobic/hydrophilic solute separation on XAD-8 resin for water from background Side A and Side B of the lake was almost identical at 65 and 67%, respectively. This result suggested that both sides of the lake are similar in organic chemical composition even though the DOC variation from side to side is 20%.

Diterpenes from the Marine Algae of the Genus Dictyota.

PubMed

Chen, Jiayun; Li, Hong; Zhao, Zishuo; Xia, Xue; Li, Bo; Zhang, Jinrong; Yan, Xiaojun

2018-05-11

Species of the brown algae of the genus Dictyota are rich sources of bioactive secondary metabolites with diverse structural features. Excellent progress has been made in the discovery of diterpenes possessing broad chemical defensive activities from this genus. Most of these diterpenes exhibit significant biological activities, such as antiviral, cytotoxic and chemical defensive activities. In the present review, we summarized diterpenes isolated from the brown algae of the genus.

Antimicrobial activity and chemical analysis of Microlicia hatschbachii Wurdack (Melastomataceae) extract.

PubMed

Cassiano, Dayse S A; Pacheco, Alessandra G M; da Costa, Mateus M; Almeida, Jackson R G S; Vieira, Ivo J C; Branco, Alexsandro

2014-01-01

Aerial parts of Microlicia hatschbachii were extracted with hexane, and the extract was evaluated for antimicrobial activity by a broth dilution method. After phytochemical procedures: GC-MS identified aliphatic alkanes, carboxylic acids and methyl esters of long-chain fatty acids; and two diterpenoids [labd-8(17)-en-15-oic acid and labd-8(17),13-dien-15-oic acid] were identified by (1)H and (13)C NMR. The antimicrobial activity of the hexane extract could be attributed to the presence of labdanes. This identification is the first reported occurrence of labdane diterpenes in the Melastomataceae family.

Antimicrobial activity of the diterpenes flexibilide and sinulariolide derived from Sinularia flexibilis Quoy and Gaimard 1833 (Coelenterata: Alcyonacea, Octocorallia).

PubMed

Aceret, T L; Coll, J C; Uchio, Y; Sammarco, P W

1998-07-01

The soft coral Sinularia flexibilis is rarely overgrown by bacteria and algae. Various studies have shown that it contains diterpenes that protect it from competitors and predators. However, of the many diterpenoids isolated from S. flexibilis, only sinulariolide has been studied for antibiotic properties. Samples of soft corals were collected from Orpheus Island and freeze-dried for chemical extraction and isolation of pure diterpenes. Antimicrobial activity of the diterpenes was determined using the disc assay method with antibiotics as controls and the minimum inhibitory concentrations of the diterpenes were determined using the Tube Dilution Technique. Two out of the five diterpenes tested (sinulariolide and flexibilide), showed marked antimicrobial activity and inhibited growth of Gram-positive bacteria. Flexibilide was effective even at concentrations as low as 5 ppm, whereas sinulariolide was effective at concentrations of 10 ppm. These compounds show potential as antibiotics.

Diterpenes from buds of Wikstroemia chamaedaphne showing anti-hepatitis B virus activities.

PubMed

Li, Shi-Fei; Jiao, Ying-Ying; Zhang, Zhi-Qiang; Chao, Jian-Bin; Jia, Jie; Shi, Xun-Long; Zhang, Li-Wei

2018-07-01

Phytochemical study of the buds of Wikstroemia chamaedaphne Meisn. led to the isolation of seven previously undescribed diterpenes, including one tigliane diterpene (wikstchalide A), two daphnane diterpenes (wikstroelides W-X), and four lathyrane diterpenes (laurifoliosides A-B and 2-epi-laurifoliosides A-B), along with four known diterpenes. The structures of these compounds were established by extensive spectroscopic evidence and electronic circular dichroism (ECD) calculations. Wikstchalide A possesses a 5,6-epoxy ring in the tigliane skeleton. Two compounds exhibited potential anti-hepatitis B virus activities, with IC 50 values of 46.5 and 88.3 μg/mL against hepatitis B virus (HBV) surface antigen (HBsAg), and six compounds showed certain inhibitory effects on HBV-DNA replication with the inhibition ratios ranging from 2.0% to 33.0% at the concentrations ranging from 0.39 to 6.25 μg/mL. Copyright © 2018 Elsevier Ltd. All rights reserved.

Efficient in situ separation and production of L-lactic acid by Bacillus coagulans using weak basic anion-exchange resin.

PubMed

Zhang, Yitong; Qian, Zijun; Liu, Peng; Liu, Lei; Zheng, Zhaojuan; Ouyang, Jia

2018-02-01

To get rid of the dependence on lactic acid neutralizer, a simple and economical approach for efficient in situ separation and production of L-lactic acid was established by Bacillus coagulans using weak basic anion-exchange resin. During ten tested resins, the 335 weak basic anion-exchange resins demonstrated the highest adsorption capacity and selectivity for lactic acid recovery. The adsorption study of the 335 resins for lactic acid confirmed that it is an efficient adsorbent under fermentation condition. Langmuir models gave a good fit to the equilibrium data at 50 °C and the maximum adsorption capacity for lactic acid by 335 resins was about 402 mg/g. Adsorption kinetic experiments showed that pseudo-second-order kinetics model gave a good fit to the adsorption rate. When it was used for in situ fermentation, the yield of L-lactic acid by B. coagulans CC17 was close to traditional fermentation and still maintained at about 82% even after reuse by ten times. These results indicated that in situ separation and production of L-lactic acid using the 335 resins were efficient and feasible. This process could greatly reduce the dosage of neutralizing agent and potentially be used in industry.

Phosphonic acid based exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1995-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1994-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene disphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E. Philip; Alexandratos, Spiro D.; Gatrone, Ralph C.; Chiarizia, Ronato

1996-01-01

An ion exchange resin for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene.

Development of melamine modified urea formaldehyde resins based o nstrong acidic pH catalyzed urea formaldehyde polymer

Treesearch

Chung-Yun Hse

2009-01-01

To upgrade the performance of urea-formaldehyde (UF) resin bonded particleboards, melamine modified urea-formaldehyde (MUF) resins based on strong acidic pH catalyzed UF polymers were investigated. The study was conducted in a series of two experiments: 1) formulation of MUF resins based on a UF polymer catalyzed with strong acidic pH and 2) determination of the...

Cardiovascular and diuretic activity of kaurene derivatives of Xylopia aethiopica and Alepidea amatymbica.

PubMed

Somova, L I; Shode, F O; Moodley, K; Govender, Y

2001-10-01

The extractives, crude and pure, of Alepidea amatymbica (AA) and Xylopia aethiopica (XA) were subjected to bioassay-directed phytochemical examination for potential cardiovascular and diuretic activity. All extractives and derivatives (XA/O, AA/1, xylopic acid, AA/3, AA/4, AA/5, AA/6, XA/1, XA/2, XA/3) displayed low toxicity, with LC(50) 0.5-5.0 ng/ml. For the first time, diterpene kaurenoids were reported to have significant systemic hypotensive and coronary vasodilatory effect accompanied with bradycardia. These effects were attributed to calcium antagonistic mechanism. The diuretic and natriuretic effects found were similar to the effects of chlorothiazide, suggesting inhibition of Na+ and K+ reabsorption in the early portion of the distal tubule. Further experiments are needed to elaborate the exact mechanisms of the hypotensive and diuretic effects of diterpene kaurenoids.

Immunomodulatory action of Copaifera spp oleoresins on cytokine production by human monocytes.

PubMed

Santiago, Karina Basso; Conti, Bruno José; Murbach Teles Andrade, Bruna Fernanda; Mangabeira da Silva, Jonas Joaquim; Rogez, Hervé Louis Ghislain; Crevelin, Eduardo José; Beraldo de Moraes, Luiz Alberto; Veneziani, Rodrigo; Ambrósio, Sérgio Ricardo; Bastos, Jairo Kenupp; Sforcin, José Maurício

2015-03-01

Copaifera spp oleoresins have been used in folk medicine for centuries; nevertheless, its immunomodulatory action has not been investigated. Thus, the goal of this study was to characterize different oleoresins and to verify their action on human monocytes regarding pro- and anti-inflammatory cytokine production (TNF-α and IL-10, respectively). The chemical composition of Brazilian Copaifera reticulata, Copaifera duckey and Copaifera multijuga oleoresins was analyzed by HPLC-MS. Cell viability was assessed by MTT method after incubation of cells with Copaifera spp. Noncytotoxic concentrations of oleoresins were incubated with human monocytes from healthy donors, and cytokine production was determined by ELISA. HPLC-MS analysis for terpenes allowed the identification of six diterpene acids and one sesquiterpene acid. Oleoresins exerted no cytotoxic effects on human monocytes. All oleoresins had a similar profile: LPS-induced TNF-α production was maintained by oleoresins, while a significant inhibitory action on IL-10 production was seen. Copaifera oleoresins seemed to exert an activator profile on human monocytes without affecting cell viability. Such effect may be due to the presence of either diterpene or sesquiterpene acids; however, further studies are necessary to determine the involvement of such compounds in Copaifera immunomodulatory effects. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Process for separation of zirconium-88, rubidium-83 and yttrium-88

DOEpatents

Heaton, Richard C.; Jamriska, Sr., David J.; Taylor, Wayne A.

1994-01-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets is provided and includes dissolving the molybdenum target in a hydrogen peroxide solution to form a first ion-containing solution, passing the first ion-containing solution through a first cationic resin whereby ions selected from the group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium and rubidium remain in the first ion-containing solution while ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium and zirconium are selectively adsorbed by the first resin, contacting the first resin with an acid solution capable of stripping adsorbed ions from the first cationic exchange resin whereby the adsorbed ions are removed from the first resin to form a second ion-containing solution, evaporating the second ion-containing solution for time sufficient to remove substantially all of the acid and water from the second ion-containing solution whereby a residue remains, dissolving the residue from the evaporated second-ion containing solution in a dilute acid to form a third ion-containing solution, said third ion-containing solution having an acid molarity adapted to permit said ions to be adsorbed by a cationic exchange resin, passing the third ion-containing solution through a second cationic resin whereby the ions are adsorbed by the second resin, contacting the second resin with a dilute sulfuric acid solution whereby the adsorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, and zirconium are selectively removed from the second resin, and contacting the second resin with a dilute acid solution whereby the adsorbed strontium ions are selectively removed. Zirconium, rubidium, and yttrium radioisotopes can also be recovered with additional steps.

Antimicrobial evaluation of diterpenes from Copaifera langsdorffii oleoresin against periodontal anaerobic bacteria.

PubMed

Souza, Ariana B; de Souza, Maria G M; Moreira, Maísa A; Moreira, Monique R; Furtado, Niege A J C; Martins, Carlos H G; Bastos, Jairo K; dos Santos, Raquel A; Heleno, Vladimir C G; Ambrosio, Sergio Ricardo; Veneziani, Rodrigo C S

2011-11-18

The antimicrobial activity of four labdane-type diterpenes isolated from the oleoresin of Copaifera langsdorffii as well as of two commercially available diterpenes (sclareol and manool) was investigated against a representative panel of microorganisms responsible for periodontitis. Among all the evaluated compounds, (-)-copalic acid (CA) was the most active, displaying a very promising MIC value (3.1 µg mL-1; 10.2 µM) against the key pathogen (Porphyromonas gingivalis) involved in this infectious disease. Moreover, CA did not exhibit cytotoxicity when tested in human fibroblasts. Time-kill curve assays performed with CA against P. gingivalis revealed that this compound only inhibited the growth of the inoculums in the first 12 h (bacteriostatic effect). However, its bactericidal effect was clearly noted thereafter (between 12 and 24 h). It was also possible to verify an additive effect when CA and chlorhexidine dihydrochloride (CHD, positive control) were associated at their MBC values. The time curve profile resulting from this combination showed that this association needed only six hours for the bactericidal effect to be noted. In summary, CA has shown to be an important metabolite for the control of periodontal diseases. Moreover, the use of standardized extracts based on copaiba oleoresin with high CA contents can be an important strategy in the development of novel oral care products.

The Labdane Ent-3-Acetoxy-Labda-8(17), 13-Dien-15-Oic Decreases Blood Pressure In Hypertensive Rats

PubMed Central

Simplicio, Janaina A.; Simão, Marilia R.; Ambrosio, Sergio R.; Tirapelli, Carlos R.

2016-01-01

Background Labdane-type diterpenes induce lower blood pressure via relaxation of vascular smooth muscle; however, there are no studies describing the effects of labdanes in hypertensive rats. Objective The present study was designed to investigate the cardiovascular actions of the labdane-type diterpene ent-3-acetoxy-labda-8(17), 13-dien-15-oic acid (labda-15-oic acid) in two-kidney 1 clip (2K-1C) renal hypertension. Methods Vascular reactivity experiments were performed in aortic rings isolated from 2K-1C and normotensive (2K) male Wistar rats. Nitrate/nitrite (NOx) measurement was performed in aortas by colorimetric assay. Blood pressure measurements were performed in conscious rats. Results Labda-15-oic acid (0.1-300 µmol/l) and forskolin (0.1 nmol/l - 1 µmol/l) relaxed endothelium-intact and endothelium-denuded aortas from both 2K-1C and 2K rats. Labda-15-oic acid was more effective at inducing relaxation in endothelium-intact aortas from 2K pre-contracted with phenylephrine when compared to the endothelium-denuded ones. Forskolin was more potent than labda-15-oic acid at inducing vascular relaxation in arteries from both 2K and 2K-1C rats. Labda-15-oic acid-induced increase in NOx levels was lower in arteries from 2K-1C rats when compared to 2K rats. Intravenous administration of labda-15-oic acid (0.3-3 mg/kg) or forskolin (0.1-1 mg/kg) induced hypotension in conscious 2K-1C and 2K rats. Conclusion The present findings show that labda-15-oic acid induces vascular relaxation and hypotension in hypertensive rats. PMID:27096521

Diterpenes from the Brown Alga Dictyota crenulata.

PubMed

De-Paula, Joel Campos; Bueno, Ludmila Bomeny; Cavalcanti, Diana Negrão; Yoneshigue-Valentin, Yocie; Teixeira, Valéria Laneuville

2008-06-04

The crude extract of the Brazilian brown alga Dictyota crenulata was analyzed by NMR spectroscopy and HRGC-MS techniques. Seven diterpenes were identified: pachydictyol A, dictyodial, 4beta-hydroxydictyodial A, 4beta-acetoxydictyodial A, isopachydictyol A, dictyol C and dictyotadiol. Xeniane diterpenes have previously been found in D. crenulata from the Pacific Ocean. The results characterize D. crenulata as a species that provides prenylated guaiane (group I) and xeniane diterpenes (group III), thus making it a new source of potential antiviral products.

Enrichment and separation of chlorogenic acid from the extract of Eupatorium adenophorum Spreng by macroporous resin.

PubMed

Liu, Boyan; Dong, Beitao; Yuan, Xiaofan; Kuang, Qirong; Zhao, Qingsheng; Yang, Mei; Liu, Jie; Zhao, Bing

2016-01-01

A simple and efficient chromatographic method for separation of chlorogenic acid from Eupatorium adenophorum Spreng extract was developed. The adsorption properties of nine macroporous resins were evaluated. NKA-II resin showed much better adsorption/desorption properties. The adsorption of chlorogenic acid on NKA-II resin at 25°C was well fitted to Langmuir isotherm model and pseudo-second-order kinetic model. The dynamic adsorption and desorption experiments were carried out on columns packed with NKA-II resin to optimize the separation process. The content of chlorogenic acid in the product increased to 22.17%, with a recovery yield of 82.41%. Copyright © 2015 Elsevier B.V. All rights reserved.

Involvement of an ent-copalyl diphosphate synthase in tissue-specific accumulation of specialized diterpenes in Andrographis paniculata.

PubMed

Misra, Rajesh Chandra; Garg, Anchal; Roy, Sudeep; Chanotiya, Chandan Singh; Vasudev, Prema G; Ghosh, Sumit

2015-11-01

Ent-labdane-related diterpene (ent-LRD) specialized (i.e. secondary) metabolites of the medicinal plant kalmegh (Andrographis paniculata) have long been known for several pharmacological activities. However, our understanding of the ent-LRD biosynthetic pathway has remained largely incomplete. Since ent-LRDs accumulate in leaves, we carried out a comparative transcriptional analysis using leaf and root tissues, and identified 389 differentially expressed transcripts, including 223 transcripts that were preferentially expressed in leaf tissue. Analysis of the transcripts revealed various specialized metabolic pathways, including transcripts of the ent-LRD biosynthetic pathway. Two class II diterpene synthases (ApCPS1 and ApCPS2) along with one (ApCPS1') and two (ApCPS2' and ApCPS2″) transcriptional variants that were the outcomes of alternative splicing of the precursor mRNA and alternative transcriptional termination, respectively, were identified. ApCPS1 and ApCPS2 encode for 832- and 817-amino acids proteins, respectively, and are phylogenetically related to the dicotyledons ent-copalyl diphosphate synthases (ent-CPSs). The spatio-temporal patterns of ent-LRD metabolites accumulation and gene expression suggested a likely role for ApCPS1 in general (i.e. primary) metabolism, perhaps by providing precursor for the biosynthesis of phytohormone gibberellin (GA). However, ApCPS2 is potentially involved in tissue-specific accumulation of ent-LRD specialized metabolites. Bacterially expressed recombinant ApCPS2 catalyzed the conversion of (E,E,E)-geranylgeranyl diphosphate (GGPP), the general precursor of diterpenes to ent-copalyl diphosphate (ent-CPP), the precursor of ent-LRDs. Taken together, these results advance our understanding of the tissue-specific accumulation of specialized ent-LRDs of medicinal importance. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Phosphonic acid based exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1995-09-12

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 10 figs.

Resin in bisulfite pulp from Pinus radiata wood and its relationship to pitch troubles

Treesearch

P.J. Nelson; Richard W. Hemingway

1971-01-01

The resin content of bisulfite pulp from Pinus radiata D. Don was determined at various stages in its manufacture and the changes in the composition of the resin studied. About 50% of the resin present in the wood was removed during cooking, an additional 11% by blowpit washing, and a further 8% by screening. Resin acids and fatty acids were...

Analgesic effects of an ethanol extract of the fruits of Xylopia aethiopica (Dunal) A. Rich (Annonaceae) and the major constituent, xylopic acid in murine models

PubMed Central

Woode, Eric; Ameyaw, Elvis O.; Boakye-Gyasi, Eric; Abotsi, Wonder K. M.

2012-01-01

Background: Fruit extracts of Xylopia aethiopica are used traditionally in the management of pain disorders including rheumatism, headache, colic pain, and neuralgia. Little pharmacological data exists in scientific literature of the effect of the fruit extract and its major diterpene, xylopic acid, on pain. The present study evaluated the analgesic properties of the ethanol extract of X. aethiopica (XAE) and xylopic acid (XA), in murine models. Materials and Methods: XAE and XA were assessed in chemical (acetic acid-induced abdominal writhing and formalin tests), thermal (Tail-flick and Hargreaves thermal hyperalgesia tests), and mechanical (Randall-Selitto paw pressure test) pain models. Results: XAE and XA exhibited significant analgesic activity in all the pain models used. XAE (30-300 mg kg-1, p.o.) and XA (10-100 mg kg-1, p.o.) inhibited acetic acid-induced visceral nociception, formalin- induced paw pain (both neurogenic and inflammatory), thermal pain as well as carrageenan-induced mechanical and thermal hyperalgesia in animals. Morphine (1-10 mg kg-1, i.p.) and diclofenac (1-10 mg kg-1, i.p.), used as controls, exhibited similar anti-nociceptive activities. XAE and XA did not induce tolerance to their respective anti-nociceptive effects in the formalin test after chronic administration. Morphine tolerance did not also cross-generalize to the analgesic effects of XAE or XA. Conclusions: These findings establish the analgesic properties of the ethanol fruit extract of X. aethiopica and its major diterpene, xylopic acid. PMID:23248562

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1996-07-23

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 10 figs.

Phosphonic acid based ion exchange resins

DOEpatents

Horwitz, E.P.; Alexandratos, S.D.; Gatrone, R.C.; Chiarizia, R.

1994-01-25

An ion exchange resin is described for extracting metal ions from a liquid waste stream. An ion exchange resin is prepared by copolymerizing a vinylidene diphosphonic acid with styrene, acrylonitrile and divinylbenzene. 9 figures.

Method for digesting spent ion exchange resins and recovering actinides therefrom using microwave radiation

DOEpatents

Maxwell, III, Sherrod L.; Nichols, Sheldon T.

1999-01-01

The present invention relates to methods for digesting diphosphonic acid substituted cation exchange resins that have become loaded with actinides, rare earth metals, or heavy metals, in a way that allows for downstream chromatographic analysis of the adsorbed species without damage to or inadequate elution from the downstream chromatographic resins. The methods of the present invention involve contacting the loaded diphosphonic acid resin with concentrated oxidizing acid in a closed vessel, and irradiating this mixture with microwave radiation. This efficiently increases the temperature of the mixture to a level suitable for digestion of the resin without the use of dehydrating acids that can damage downstream analytical resins. In order to ensure more complete digestion, the irradiated mixture can be mixed with hydrogen peroxide or other oxidant, and reirradiated with microwave radiation.

Alkanes and terpenes in wood and leaves of Pinus jeffreyi and P. sabiniana

Treesearch

Robert P. Adams; Jessica W. Wright

2012-01-01

The wood oils of Pinus jeffreyi and P. sabiniana contain considerable amounts of heptane (76.6%, 92%), on a monoterpene basis. However, when entire wood extractables is considered, the amounts drop considerably (3.4%, 36.8%) with the major portion of the wood oils being diterpene acids. The leaf oil of P. jeffreyi...

Microbial activity in an acid resin deposit: biodegradation potential and ecotoxicology in an extremely acidic hydrocarbon contamination.

PubMed

Kloos, Karin; Schloter, Michael; Meyer, Ortwin

2006-11-01

Acid resins are residues produced in a recycling process for used oils that was in use in the forties and fifties of the last century. The resin-like material is highly contaminated with mineral oil hydrocarbons, extremely acidic and co-contaminated with substituted and aromatic hydrocarbons, and heavy metals. To determine the potential for microbial biodegradation the acid resin deposit and its surroundings were screened for microbial activity by soil respiration measurements. No microbial activity was found in the core deposit. However, biodegradation of hydrocarbons was possible in zones with a lower degree of contamination surrounding the deposit. An extreme acidophilic microbial community was detected close to the core deposit. With a simple ecotoxicological approach it could be shown that the pure acid resin that formed the major part of the core deposit, was toxic to the indigenous microflora due to its extremely low pH of 0-1.

Selection of anion exchangers for detoxification of dilute-acid hydrolysates from spruce.

PubMed

Horváth, Ilona Sárvári; Sjöde, Anders; Nilvebrant, Nils-Olof; Zagorodni, Andrei; Jönsson, Leif J

2004-01-01

Six anion-exchange resins with different properties were compared with respect to detoxification of a dilute-acid hydrolysate of spruce prior to ethanolic fermentation with Saccharomyces cerevisiae. The six resins encompassed strong and weak functional groups as well as styrene-, phenol-, and acrylic-based matrices. In an analytical experimental series, fractions from columns packed with the different resins were analyzed regarding pH, glucose, furfural, hydroxymethylfurfural, phenolic compounds, levulinic acid, acetic acid, formic acid, and sulfate. An initial adsorption of glucose occurred in the strong alkaline environment and led to glucose accumulation at a later stage. Acetic and levulinic acid passed through the column before formic acid, whereas sulfate had the strongest affinity. In a preparative experimental series, one fraction from each of six columns packed with the different resins was collected for assay of the fermentability and analysis of glucose, mannose, and fermentation inhibitors. The fractions collected from strong anion-exchange resins with styrene-based matrices displayed the best fermentability: a sevenfold enhancement of ethanol productivity compared with untreated hydrolysate. Fractions from a strong anion exchanger with acrylic-based matrix and a weak exchanger with phenol-based resin displayed an intermediate improvement in fermentability, a four- to fivefold increase in ethanol productivity. The fractions from two weak exchangers with styrene- and acrylic-based matrices displayed a twofold increase in ethanol productivity. Phenolic compounds were more efficiently removed by resins with styrene- and phenol-based matrices than by resins with acrylic-based matrices.

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an... conditions of time and temperature characterizing the conditions of its intended use, as determined from...

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric acid anhydride to produce a resin having an... conditions of time and temperature characterizing the conditions of its intended use, as determined from...

Emission of volatile aldehydes and ketones from wood pellets under controlled conditions.

PubMed

Arshadi, Mehrdad; Geladi, Paul; Gref, Rolf; Fjällström, Pär

2009-11-01

Different qualities of biofuel pellets were made from pine and spruce sawdust according to an industrial experimental design. The fatty/resin acid compositions were determined by gas chromatography-mass spectrometry for both newly produced pellets and those after 2 and 4 weeks of storage. The aldehydes/ketones compositions were determined by high performance liquid chromatography at 0, 2, and 4 weeks. The designs were analyzed for the response variables: total fatty/resin acids and total aldehydes/ketones. The design showed a strong correlation between the pine fraction in the pellets and the fatty/resin acid content but the influence decreased over storage time. The amount of fatty/resin acids decreased approximately 40% during 4 weeks. The influence of drying temperature on the aldehyde/ketone emission of fresh pellets was also shown. The amounts of emitted aldehydes/ketones generally decreased by 45% during storage as a consequence of fatty/resin acid oxidation. The matrices of individual concentrations were subjected to multivariate data analysis. This showed clustering of the different experimental runs and demonstrated the important mechanism of fatty/resin acid conversion.

Isolation of hydrophilic organic acids from water using nonionic macroporous resins

USGS Publications Warehouse

Aiken, G.R.; McKnight, Diane M.; Thorn, K.A.; Thurman, E.M.

1992-01-01

A method has been developed for the isolation of hydrophilic organic acids from aquatic environments using Amberlite* * Use of trade names in this report is for identification purposes only and does not constitute endorsement by the U.S. Geological Survey. XAD-4 resin. The method uses a two column array of XAD-8 and XAD-4 resins in series. The hydrophobic organic acids, composed primarily of aquatic fulvic acid, are removed from the sample on XAD-8, followed by the isolation of the more hydrophilic organic acids on XAD-4. For samples from a number of diverse environments, more of the dissolved organic carbon was isolated on the XAD-8 resin (23-58%) than on the XAD-4 resin (7-25%). For these samples, the hydrophilic acids have lower carbon and hydrogen contents, higher oxygen and nitrogen contents, and are lower in molecular weight than the corresponding fulvic acids. 13C NMR analyses indicate that the hydrophilic acids have a lower concentration of aromatic carbon and greater heteroaliphatic, ketone and carboxyl content than the fulvic acid. ?? 1992.

Process for strontium-82 separation

DOEpatents

Heaton, Richard C.; Jamriska, Sr., David J.; Taylor, Wayne A.

1992-01-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets comprises dissolving the molybdenum target in a hydrogen peroxide solution to form a first solution containing ions selected from a group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium, rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, and yttrium; passing the solution through a first cationic resin whereby ions selected from a group consisting of zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium a portion of zirconium and a portion of rubidium are selectively absorbed by the first resin; contacting the first resin with an acid solution to strip and remove the absorbed ions from the first cationic exchange resin to form a second solution; evaporating the second solution for a time sufficient to remove substantially all of the acid and water from the solution whereby a residue remains; dissolving the residue in a dilute acid to form a third solution; passing the third solution through a second cationic resin whereby the ions are absorbed by the second resin; contacting the second resin with a dilute sulfuric acid solution whereby the absorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium and zirconium are selectively removed from the second resin; and contacting the second resin with a dilute acid solution whereby the absorbed strontium ions are selectively removed.

Process for strontium-82 separation

DOEpatents

Heaton, R.C.; Jamriska, D.J. Sr.; Taylor, W.A.

1992-12-01

A process for selective separation of strontium-82 and strontium-85 from proton irradiated molybdenum targets comprises dissolving the molybdenum target in a hydrogen peroxide solution to form a first solution containing ions selected from a group consisting of molybdenum, niobium, technetium, selenium, vanadium, arsenic, germanium, zirconium, rubidium, zinc, beryllium, cobalt, iron, manganese, chromium, strontium, and yttrium; passing the solution through a first cationic resin whereby ions selected from a group consisting of zinc, beryllium, cobalt, iron, manganese, chromium, strontium, yttrium a portion of zirconium and a portion of rubidium are selectively absorbed by the first resin; contacting the first resin with an acid solution to strip and remove the absorbed ions from the first cationic exchange resin to form a second solution; evaporating the second solution for a time sufficient to remove substantially all of the acid and water from the solution whereby a residue remains; dissolving the residue in a dilute acid to form a third solution; passing the third solution through a second cationic resin whereby the ions are absorbed by the second resin; contacting the second resin with a dilute sulfuric acid solution whereby the absorbed ions selected from the group consisting of rubidium, zinc, beryllium, cobalt, iron, manganese, chromium and zirconium are selectively removed from the second resin; and contacting the second resin with a dilute acid solution whereby the absorbed strontium ions are selectively removed. 1 fig.

2-Chlorotrityl chloride resin. Studies on anchoring of Fmoc-amino acids and peptide cleavage.

PubMed

Barlos, K; Chatzi, O; Gatos, D; Stavropoulos, G

1991-06-01

The esterification of 2-chlorotrityl chloride resin with Fmoc-amino acids in the presence of DIEA is studied under various conditions. High esterification yields are obtained using 0.6 equiv. Fmoc-amino acid/mmol resin in DCM or DCE, in 25 min, at room temperature. The reaction proceeds without by product formation even in the case of Fmoc-Asn and Fmoc-Gln. The quantitative and easy cleavage of amino acids and peptides from 2-chlorotrityl resin, by using AcOH/TFE/DCM mixtures, is accomplished within 15-60 min at room temperature, while t-butyl type protecting groups remain unaffected. Under these exceptionally mild conditions 2-chlorotrityl cations generated during the cleavage of amino acids and peptides from resin do not attack the nucleophilic side chains of Trp, Met, and Tyr.

Morphological and chemical characterization of the dentin/resin cement interface produced with a self-etching primer.

PubMed

Walker, Mary P; Wang, Yong; Spencer, Paulette

2002-01-01

The purpose of this study was to analyze a resin cement/dentin interface by comparing the diffusion of a resin cement into dentin surfaces pretreated with a self-etching primer with or without pretreatment by conventional acid etching. Dentin surfaces of 8 unerupted human third molars were treated with a self-etch primer (Panavia 21) with or without conventional phosphoric acid pretreatment. Panavia 21 resin cement was applied according to manufacturer's instructions. Dentin/resin cement interface sections from each tooth were examined with scanning electron microscopy and micro-Raman spectroscopy. When the self-etch primer was used following conventional acid pretreatment, the resin cement did not penetrate to the depth of the zone of demineralized dentin, leaving a substantial area of exposed dentin matrix at the dentin/cement interface. In contrast, there was substantial resin cement diffusion throughout the demineralized dentin when the self-etch primer was used without acid etching pretreatment. The in vitro evaluation of resin cement penetration throughout the zone of demineralized dentin is an important step in identifying sites of exposed dentin matrix that may promote postoperative sensitivity and may leave the dentin/resin cement interface vulnerable to premature degradation under clinical conditions. In this study, the self-etch primer used alone produced substantial resin cement penetration and left no exposed dentin matrix at the dentin/resin cement interface.

Clerodane and Ent-kaurane Diterpene Glycosyl and Glycoside Derivatives from the Leaves of Casearia sylvestris

USDA-ARS?s Scientific Manuscript database

Five new clerodane diterpene glycosides caseariasides A-E (1-4) and three new ent-kaurane diterpene glucosides sylvestrisides C-E (6-8) were isolated from the leaves of Casearia sylvestris. Their structures were determined on the basis of chemical and spectroscopic analyses....

Effect of pore structure on the removal of clofibric acid by magnetic anion exchange resin.

PubMed

Tan, Liang; Shuang, Chendong; Wang, Yunshu; Wang, Jun; Su, Yihong; Li, Aimin

2018-01-01

The effect of pore structure of resin on clofibric acid (CA) adsorption behavior was investigated by using magnetic anion exchange resins (ND-1, ND-2, ND-3) with increasing pore diameter by 11.68, 15.37, 24.94 nm. Resin with larger pores showed faster adsorption rates and a higher adsorption capacity because the more opened tunnels provided by larger pores benefit the CA diffusion into the resin matrix. The ion exchange by the electrostatic interactions between Cl-type resin and CA resulted in chloride releasing to the solution, and the ratio of released chloride to CA adsorption amount decreased from 0.90 to 0.65 for ND-1, ND-2 and ND-3, indicating that non-electrostatic interactions obtain a larger proportional part of the adsorption into the pores. Co-existing inorganic anions and organic acids reduced the CA adsorption amounts by the competition effect of electrostatic interaction, whereas resins with more opened pore structures weakened the negative influence on CA adsorption because of the existence of non-electrostatic interactions. 85.2% and 65.1% adsorption amounts decrease are calculated for resin ND-1 and ND-3 by the negative influence of 1 mmol L -1 NaCl. This weaken effect of organic acid is generally depends on its hydrophobicity (Log Kow) for carboxylic acid and its ionization degree (pKb) for sulfonic acid. The resins could be reused with the slightly decreases by 1.9%, 3.2% and 5.4% after 7 cycles of regeneration, respectively for ND-1, ND-2 and ND-3, suggesting the ion exchange resin with larger pores are against its reuse by the brine solution regeneration. Copyright © 2017 Elsevier Ltd. All rights reserved.

METHOD OF SEPARATION

DOEpatents

Boyd, G.E.

1958-08-26

A process is presented fer separating uranium, plutonium, and fission products ions from uranyl nitrate solutions having a pH value between 1 and 3 obtained by dissolving neutron irradiated uranium. The method consists in passing such solutions through a bed of cation exchange resin, which may be a sulfonated phenol formaidehyde type. Following the adsorption step the resin is first treated with a solution of 0.2M to 0.3M sulfuric acid to desorb the uranium. Fission product ions are then desorbed by treating the resin in phosphoric acid and 1M in nitric acid. Lastly, the plutonium may be desorbed by treating the resin with a solution approximately 0.8M in phosphoric acid and 1M in nitric acid.

Separation of aliphatic carboxylic acids and benzenecarboxylic acids by ion-exclusion chromatography with various cation-exchange resin columns and sulfuric acid as eluent.

PubMed

Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae-Jeong; Lee, Kwang-Pill

2003-05-16

The application of various hydrophilic cation-exchange resins for high-performance liquid chromatography (sulfonated silica gel: TSKgel SP-2SW, carboxylated silica gel: TSKgel CM-2SW, sulfonated polymethacrylate resin: TSKgel SP-5PW, carboxylated polymethacrylate resins: TSKgel CM-5PW and TSKgel OA-Pak A) as stationary phases in ion-exclusion chromatography for C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, butyric, isovaleric, valeric, isocaproic, caproic, 2-methylhexanoic and heptanoic acids) and benzenecarboxylic acids (pyromellitic, trimellitic, hemimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic, salicylic acids and phenol) was carried out using diluted sulfuric acid as the eluent. Silica-based cation-exchange resins (TSKgel SP-2SW and TSKgel CM-2SW) were very suitable for the ion-exclusion chromatographic separation of these benzenecarboxylic acids. Excellent simultaneous separation of these benzenecarboxylic acids was achieved on a TSKgel SP-2SW column (150 x 6 mm I.D.) in 17 min using a 2.5 mM sulfuric acid at pH 2.4 as the eluent. Polymethacrylate-based cation-exchange resins (TSKgel SP-5PW, TSKgel CM-5PW and TSKgel OA-Pak A) acted as advanced stationary phases for the ion-exclusion chromatographic separation of these C1-C7 aliphatic carboxylic acids. Excellent simultaneous separation of these C1-C7 acids was achieved on a TSKgel CM-5PW column (150 x 6 mm I.D.) in 32 min using a 0.05 mM sulfuric acid at pH 4.0 as the eluent.

Amino acid analysis

NASA Technical Reports Server (NTRS)

Winitz, M.; Graff, J. (Inventor)

1974-01-01

The process and apparatus for qualitative and quantitative analysis of the amino acid content of a biological sample are presented. The sample is deposited on a cation exchange resin and then is washed with suitable solvents. The amino acids and various cations and organic material with a basic function remain on the resin. The resin is eluted with an acid eluant, and the eluate containing the amino acids is transferred to a reaction vessel where the eluant is removed. Final analysis of the purified acylated amino acid esters is accomplished by gas-liquid chromatographic techniques.

Silencing brassinosteroid receptor BRI1 impairs herbivory-elicited accumulation of jasmonic acid-isoleucine and diterpene glycosides, but not jasmonic acid and trypsin proteinase inhibitors in Nicotiana attenuata.

PubMed

Yang, Da-Hai; Baldwin, Ian T; Wu, Jianqiang

2013-06-01

The brassinosteroid (BR) receptor, BR insensitive 1 (BRI1), plays a critical role in plant development, but whether BRI1-mediated BR signaling is involved in plant defense responses to herbivores was largely unknown. Here, we examined the function of BRI1 in the resistance of Nicotiana attenuata (Solanaceae) to its specialist insect herbivore Manduca sexta. Jasmonic acid (JA) and JA-isoleucine conjugate (JA-Ile) are important hormones that mediate resistance to herbivores and we found that after wounding or simulated herbivory NaBRI1 had little effect on JA levels, but was important for the induction of JA-Ile. Further experiments revealed that decreased JAR (the enzyme for JA-Ile production) activity and availability of Ile in NaBRI1-silenced plants were likely responsible for the low JA-Ile levels. Consistently, M. sexta larvae gained more weight on NaBRI1-silenced plants than on the control plants. Quantification of insect feeding-induced secondary metabolites revealed that silencing NaBRI1 resulted in decreased levels of carbon-rich defensive secondary metabolites (hydroxygeranyllinalool diterpene glycosides, chlorogenic acid, and rutin), but had little effect on the nitrogen-rich ones (nicotine and trypsin proteinase inhibitors). Thus, NaBRI1-mediated BR signaling is likely involved in plant defense responses to M. sexta, including maintaining JA-Ile levels and the accumulation of several carbon-rich defensive secondary metabolites. © 2013 Institute of Botany, Chinese Academy of Sciences.

Fatty Acid-Based Monomers as Styrene Replacements for Liquid Molding Resins

DTIC Science & Technology

2005-05-01

fatty acid length and unsaturation level on resin and polymer properties. Fig. 2. The addition of fatty acids ( oleic acid ) to glycidyl methacylate to...the synthetic route used to form the methacrylated fatty acids (MFA). The carboxylic acid of fatty acids undergoes a simple addition reaction with... form methacrylated fatty acid monomer

High Performance Fatty Acid-Based Vinyl Ester Resin for Liquid Molding

DTIC Science & Technology

2007-07-01

High Performance Fatty Acid -Based Vinyl Ester Resin for Liquid Molding by Xing Geng, John J. La Scala, James M. Sands, and Giuseppe R...it to the originator. Army Research Laboratory Aberdeen Proving Ground, MD 21005-5069 ARL-RP-184 July 2007 High Performance Fatty Acid ...CONTRACT NUMBER 5b. GRANT NUMBER 4. TITLE AND SUBTITLE High Performance Fatty Acid -Based Vinyl Ester Resin for Liquid Molding 5c. PROGRAM

Copper resinate: preparation, characterisation and study of degradation.

PubMed

Colombini, M P; Lanterna, G; Mairani, A; Matteini, M; Modugno, F; Rizzi, M

2001-01-01

This paper describes a method for the synthesis of Copper Resinate, which disappeared from artists' palettes in the eighteenth century. This was carried out by interpreting ancient recipes following a scientific approach. Its characterisation using Fourier Transform-Infrared Spectrometry and Gas Chromatography-Mass Spectrometry demonstrated that it is a mixture containing copper and oxidised abietic acids, mainly dehydroabietic and 7-oxo-dehydroabietic acids, formed during the preparation of the pigment and the curing of the paint layer. The composition of copper resinate paint layers, artificially aged by U.V. irradiation at 365 nm (UV), heating (T), and exposed to atmospheric pollutants (NOX) in a climatic chamber, was investigated. The combination of irradiation and temperature produced a change in colour along with a significant increase in the recovered amount of 7-oxo-dehydroabietic acid. The identification of copper resinate in a sample from an old painting should be related to the presence of the following resin compounds which are stable in the ageing process: dehydroabietic and 7-oxo-dehydroabietic acid pimaradienic acids. Photo-oxidation of the resin acids co-ordinated with copper seem to be the most probable decay mechanism responsible for the colour change in the pigment.

An Efficient Protocol for Preparation of Gallic Acid from Terminalia bellirica (Gaertn.) Roxb by Combination of Macroporous Resin and Preparative High-Performance Liquid Chromatography.

PubMed

Zou, Denglang; Chen, Tao; Chen, Chen; Li, Hongmei; Liu, Yongling; Li, Yulin

2016-08-01

In this article, macroporous resin column chromatography and preparative high-performance liquid chromatography were applied for preparation of gallic acid from Terminalia bellirica (Gaertn.) Roxb. In the first step, six kinds of resins were investigated by adsorption and desorption tests and AB-8 macroporous resin was selected for the enrichment of gallic acid. As a result, 20 g of gallic acid at a purity of 71% could be separated from 100 g of crude extract in which the content of gallic acid was 16.7% and the recovery of gallic acid reached 85.0%. In the second step, preparative high-performance liquid chromatography was selected to purify gallic acid. As a result, 640 mg of gallic acid at a purity of 99.1% was obtained from 1 g of sample in 35 min. The results demonstrated that macroporous resin coupled with preparative high-performance liquid chromatography was suitable for preparation of gallic acid from T. bellirica (Gaertn.) Roxb. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Molecular Signaling Pathways Behind the Biological Effects of Salvia Species Diterpenes in Neuropharmacology and Cardiology.

PubMed

Akaberi, M; Iranshahi, M; Mehri, S

2016-06-01

The genus Salvia, from the Lamiaceae family, has diverse biological properties that are primarily attributable to their diterpene contents. There is no comprehensive review on the molecular signaling pathways of these active components. In this review, we investigated the molecular targets of bioactive Salvia diterpenes responsible for the treatment of nervous and cardiovascular diseases. The effects on different pathways, including apoptosis signaling, oxidative stress phenomena, the accumulation of amyloid beta plaques, and tau phosphorylation, have all been considered to be mechanisms of the anti-Alzheimer properties of Salvia diterpenes. Additionally, effects on the benzodiazepine and kappa opioid receptors and neuroprotective effects are noted as neuropharmacological properties of Salvia diterpenes, including tanshinone IIA, salvinorin A, cryptotanshinone, and miltirone. Tanshinone IIA, as the primary diterpene of Salvia miltiorrhiza, has beneficial activities in heart diseases because of its ability to scavenge free radicals and its effects on transcription factors, such as nuclear transcription factor-kappa B (NF-κB) and the mitogen-activated protein kinases (MAPKs). Additionally, tanshinone IIA has also been proposed to have cardioprotective properties including antiarrhythmic activities and effects on myocardial infarction. With respect to the potential therapeutic effects of Salvia diterpenes, comprehensive clinical trials are warranted to evaluate these valuable molecules as lead compounds. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Divergent synthesis and chemical reactivity of bicyclic lactone fragments of complex rearranged spongian diterpenes.

PubMed

Schnermann, Martin J; Beaudry, Christopher M; Genung, Nathan E; Canham, Stephen M; Untiedt, Nicholas L; Karanikolas, Breanne D W; Sütterlin, Christine; Overman, Larry E

2011-11-02

The synthesis and direct comparison of the chemical reactivity of the two highly oxidized bicyclic lactone fragments found in rearranged spongian diterpenes (8-substituted 6-acetoxy-2,7-dioxabicyclo[3.2.1]octan-3-one and 6-substituted 7-acetoxy-2,8-dioxabicyclo[3.3.0]octan-3-one) are reported. Details of the first synthesis of the 6-acetoxy-2,7-dioxabicyclo[3.2.1]octan-3-one ring system, including an examination of several possibilities for the key bridging cyclization reaction, are described. In addition, the first synthesis of 7-acetoxy-2,8-dioxabicyclo[3.3.0]octanones containing quaternary carbon substituents at C6 is disclosed. Aspects of the chemical reactivity and Golgi-modifying properties of these bicyclic lactone analogs of rearranged spongian diterpenes are also reported. Under both acidic and basic conditions, 8-substituted 2,7-dioxabicyclo[3.2.1]octanones are converted to 6-substituted-2,8-dioxabicyclo[3.3.0]octanones. Moreover, these dioxabicyclic lactones react with primary amines and lysine side chains of lysozyme to form substituted pyrroles, a conjugation that could be responsible for the unique biological properties of these compounds. These studies demonstrate that acetoxylation adjacent to the lactone carbonyl group, in either the bridged or fused series, is required to produce fragmented Golgi membranes in the pericentriolar region that is characteristic of macfarlandin E.

Diterpenes and Their Derivatives as Potential Anticancer Agents.

PubMed

Islam, Muhammad Torequl

2017-05-01

As therapeutic tools, diterpenes and their derivatives have gained much attention of the medicinal scientists nowadays. It is due to their pledging and important biological activities. This review congregates the anticancer diterpenes. For this, a search was made with selected keywords in PubMed, Science Direct, Web of Science, Scopus, The American Chemical Society and miscellaneous databases from January 2012 to January 2017 for the published articles. A total 28, 789 published articles were seen. Among them, 240 were included in this study. More than 250 important anticancer diterpenes and their derivatives were seen in the databases, acting in the different pathways. Some of them are already under clinical trials, while others are in the nonclinical and/or pre-clinical trials. In conclusion, diterpenes may be one of the lead molecules in the treatment of cancer. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Isolation of organic acids from large volumes of water by adsorption on macroporous resins

USGS Publications Warehouse

Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

1987-01-01

Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

Inhibitory effect of resin composite containing S-PRG filler on Streptococcus mutans glucose metabolism.

PubMed

Kitagawa, Haruaki; Miki-Oka, Saeki; Mayanagi, Gen; Abiko, Yuki; Takahashi, Nobuhiro; Imazato, Satoshi

2018-03-01

Resin composites containing surface pre-reacted glass-ionomer (S-PRG) fillers have been reported to inhibit Streptococcus mutans growth on their surfaces, and their inhibitory effects were attributed to BO 3 3- and F - ions. The aim of this study was to evaluate S. mutans acid production through glucose metabolism on resin composite containing S-PRG fillers and assess inhibitory effects of BO 3 3- and F - on S. mutans metabolic activities. The pH change through S. mutans acid production on experimental resin composite was periodically measured after the addition of glucose. Inhibitory effects of BO 3 3- or F - solutions on S. mutans metabolism were evaluated by XTT assays and measurement of the acid production rate. The pH of experimental resin containing S-PRG fillers was significantly higher than that of control resin containing silica fillers (p < 0.05). OD 450 values by XTT assays and S. mutans acid production rates significantly decreased in the presence of BO 3 3- and F - compared with the absence of these ions (p < 0.05). pH reduction by S. mutans acid production was inhibited on resin composite containing S-PRG fillers. Moreover, S. mutans glucose metabolism and acid production were inhibited in the presence of low concentrations of BO 3 3- or F - . BO 3 3- or F - released from resin composite containing S-PRG fillers exhibits inhibitory effects on S. mutans metabolism at concentrations lower than those which inhibit bacterial growth. Copyright © 2017 Elsevier Ltd. All rights reserved.

ADSORPTION PROCEDURE IN PREPARING U$sup 23$$sup 3$

DOEpatents

Stoughton, R.W.

1958-10-14

A process is presented for the separation of protoactinium and thorium from an aqueous nitric acid solution containing these metals. It comprises contacting the solution with a cation exchange phenol-formaldehyde resin containing sulfonic acid groups, and eluting the adsorbed thorium from the resin by means of aqueous nitric acid. Thereafter the adsorbed protoactinium is eluted from the resin by means of an aqueous solution of ammonium fluoride.

Ent-7α-acetoxytrachyloban-18-oic acid and ent-7α-hydroxytrachyloban-18-oic acid from Xylopia langsdorfiana A. St-Hil. & Tul. modulate K(+) and Ca(2+) channels to reduce cytosolic calcium concentration on guinea pig ileum.

PubMed

Santos, Rosimeire F; Martins, Italo R R; Travassos, Rafael A; Tavares, Josean F; Silva, Marcelo S; Paredes-Gamero, Edgar J; Ferreira, Alice T; Nouailhetas, Viviane L A; Aboulafia, Jeannine; Rigoni, Vera L S; da Silva, Bagnólia A

2012-03-05

In this study we investigated the mechanism underlying the spasmolytic action of ent-7α-acetoxytrachyloban-18-oic acid (trachylobane-360) and ent-7α-hydroxytrachyloban-18-oic acid (trachylobane-318), diterpenes obtained from Xylopia langsdorfiana, on guinea pig ileum. Both compounds inhibited histamine-induced cumulative contractions (slope=3.5±0.9 and 4.4±0.7) that suggests a noncompetitive antagonism to histaminergic receptors. CaCl(2)-induced contractions were nonparallelly and concentration-dependently reduced by both diterpenes, indicating blockade of calcium influx through voltage-dependent calcium channels (Ca(v)). The Ca(v) participation was confirmed since both trachylobanes equipotently relaxed ileum pre-contracted with S-(-)-Bay K8644 (EC(50)=3.5±0.7×10-(5) and 1.1±0.2×10-(5)M) and KCl (EC(50)=5.5±0.3×10-(5) and 1.4±0.2×10-(5)M). K(+) channels participation was confirmed since diterpene-induced relaxation curves were significantly shifted to right in the presence of 5mM tetraethylammonium (TEA(+)) (EC(50)=0.5±0.04×10-(4) and 2.0±0.5×10-(5)M). ATP-sensitive K(+) channel (K(ATP)), voltage activated K(+) channels (K(V)), small conductance calcium-activated K(+) channels (SK(Ca)) or big conductance calcium-activated K(+) channels (BK(Ca)) did not seem to participate of trachylobane-360 spasmolytic action. However trachylobane-318 modulated positively K(ATP), K(V) and SK(Ca) (EC(50)=1.1±0.3×10-(5), 0.7±0.2×10-(5) and 0.7±0.2×10-(5)M), but not BK(Ca). A fluorescence analysis technique confirmed the decrease of cytosolic calcium concentration ([Ca(2+)](c)) induced by both trachylobanes in ileal myocytes. In conclusion, trachylobane-360 and trachylobane-318 induced spasmolytic activity by K(+) channel positive modulation and Ca(2+) channel blockade, which results in [Ca(2+)](c) reduction at cellular level leading to smooth muscle relaxation. Copyright © 2011. Published by Elsevier B.V.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Torlakoglu, A.; Gueclue, G.

Waste polyethylene terephthalate (PET) flakes were depolymerized by using propylene glycol (PG) in the presence of zinc acetate as catalyst. Glycolysis reaction products of waste PET obtained by using PET/glycol molar ratio 1/2. Two short oil alkyd resins of high acid values (30-40 mgKOH/g) were prepared from phthalic anhydride (PA), glycerin (G), coconut oil fatty acids (COFA) and glycolyzed products of waste PET (PET-based alkyd resins) or glycols (PG) (reference alkyd resins). These alkyd resins were blended with 30%, 40%, and 50% of a commercial urea-formaldehyde, melamine-formaldehyde and urea-formaldehyde/melamine-formaldehyde mixture (1/1 weight ratio) and heated at 140 deg. C. Themore » physical and chemical properties such as drying time, hardness, abrasion resistance, adhesion strength, water resistance, alkaline resistance, acid resistance, gelation time, and thermal oxidative degradation resistance (with thermogravimetric analysis, TGA) of these alkyd-amino resins were investigated. The properties of the waste PET-based resins were found to be compatible with the properties of the reference resins.« less

Hydrolyzable polyester resins, varnishes and coating compositions containing the same

DOEpatents

Yamamori, Naoki; Yokoi, Junji; Yoshikawa, Motoyoshi

1984-01-01

Preparation of hydrolyzable polyester resin comprising reacting polycarboxylic acid and polyhydric alcohol components, which is characterized by using, as at least part of said polyhydric alcohol component, a metallic salt of hydroxy carboxylic acid of the formula defined and effecting the polycondensation at a temperature which is no more than the decomposition temperature of said metallic salt. The polyester resins are useful as resinous vehicle of varnishes and antifouling paints.

Method development for thermal analyses testing on Reillex HPQ resin using the advanced reactive system screening tool (ARSST)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Best, D.

Reillex™ HPQ resin was developed by Los Alamos Laboratory and Reilly Industries Inc. in an effort to increase safety and process efficiency during the recovery and purification of plutonium. Ionac™ A-641, another strong base macroporous anion exchange resin used in the nuclear industry, was known to undergo a runaway reaction in hot nitric acid solutions. Because of this, an extensive amount of thermal analyses testing on the Reillex™ HPQ resin in SRNL was performed in 1999-2001 prior to use. A report on the thermal stability qualification of the Reillex™ HPQ resin in 8M (35%) and 12M (53%) HNO 3 wasmore » reported in 2000. In 2001, the reactivity of Reillex™ HPQ resin in 14.4M (64%) HNO 3 was evaluated. In January of 2001, thermal stability scoping tests were performed on irradiated Reillex™ HPQ resin in 14.4M (64%) HNO 3 (as a worst case scenario) and the results sent to Fauske and Associates to calculate a rupture disk size for the HB-Line resin column. A technical report by Fauske and Associates was issued in February 2001 recommending a 2.0” vent line with a rupture disk set pressure of 60 psig. This calculation was based on ARSST thermal analyses scoping tests at SRNL in which 4 grams of dried resin and 6.0 grams of 64% nitric acid in a 10 gram test cell, produced a maximum pressure rate (dP/dt) of 720 psi/min (12 psi/sec) and a maximum temperature of 250 °C. In 2015, a new batch of Reillex™ HPQ resin was manufactured by Vertellus Industries. A test sample of the resin was sent to SRNL to perform acceptance and qualification thermal stability testing using the ARSST. During these tests, method development was performed to ensure that a representative resin to acid ratios were used while running the tests in the ARSST. Fauske and Associates recommended to either use a full test cell representative of the HB-Line column or a 10 gram sample in the test cell that was representative of the ratios of resin to nitric acid in the actual HB-Line column. An observation was made during method development testing that the 4 grams of resin to 6 grams of 64% acid ratio used in 2001 to determine the rupture disk size did not entirely wet the resin and was not representative of the actual HB-Line column. The results of this study raised questions as to whether the ratio of 4 grams of resin to 6 grams of 64% nitric acid recommended by Fauske and Associates in 2001 was the correct ratio.« less

Characteristics of Alcian-blue Dye Adsorption of Natural Biofilm Matrix

NASA Astrophysics Data System (ADS)

Kurniawan, A.; Yamamoto, T.; Sukandar; Guntur

2018-01-01

In this study, natural biofilm matrices formed on stones have been used for the adsorption of Alcian blue dye. Alcian blue is a member of polyvalent basic dyes that largely used from laboratory until industrial dying purposes. The adsorption of the dye onto the biofilm matrix has been carried out at different experimental conditions such as adsorption isotherm and kinetic of adsorption. The electric charge properties of biofilm matrix and its changes related to the adsorption of Alcian blue have been also investigated. Moreover, the results of Alcian blue adsorption to the biofilm were compared to those onto the acidic and neutral resin. The kinetics of adsorption result showed that the adsorption of the Alcian blue dye reached to a maximum adsorption amount within 60 minutes. The adsorption amount of Alcian blue to biofilm increased monotonously, and the maximum adsorption amount was greater compared to the resins. On the contrary, Alcian blue did not attach to the neutral resin having no electric charge. It seems that Alcian blue attached to the acidic resins due to electrostatic attractive force, and the same seems to be the case for adsorption of Alcian blue to biofilm. The adsorption of Alcian blue to the biofilm and acidic resins fitted to Langmuir type indicates that the binding of Alcian blue to the biofilm and acidic resins occurred in a monolayer like form. The maximum adsorption amount of Alcian blue on the biofilm (0.24 mmol/dry-g) was greater than those of acidic resin (0.025 mmol/dry-g). This indicates that the biofilm has many more sites for Alcian blue attachment than acidic resins. According to the result of this study, the biofilm matrix can be a good adsorbent for dye such as Alcian blue or other dyes that causing hazards in nature.

Surface Engineering of PAMAM-SDB Chelating Resin with Diglycolamic Acid (DGA) Functional Group for Efficient Sorption of U(VI) and Th(IV) from Aqueous Medium.

PubMed

Ilaiyaraja, P; Deb, A K Singha; Ponraju, D; Ali, Sk Musharaf; Venkatraman, B

2017-04-15

A novel chelating resin obtained via growth of PAMAM dendron on surface of styrene divinyl benzene resin beads, followed by diglycolamic acid functionalization of the dendrimer terminal. Batch experiments were conducted to study the effects of pH, nitric acid concentration, amount of adsorbent, shaking time, initial metal ion concentration and temperature on U(VI) and Th(IV) adsorption efficiency. Diglycolamic acid terminated PAMAM dendrimer functionalized styrene divinylbenzene chelating resin (DGA-PAMAM-SDB) is found to be an efficient candidate for the removal of U(VI) and Th(IV) ions from aqueous (pH >4) and nitric acid media (>3M). The sorption equilibrium could be reached within 60min, and the experimental data fits with pseudo-second-order model. Langmuir sorption isotherm model correlates well with sorption equilibrium data. The maximum U(VI) and Th(IV) sorption capacity onto DGA-PAMAMG 5 -SDB was estimated to be about 682 and 544.2mgg -1 respectively at 25°C. The interaction of actinides and chelating resin is reversible and hence, the resin can be regenerated and reused. DFT calculation on the interaction of U(VI) and Th(IV) ions with chelating resin validates the experimental findings. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of Stevia plants grown from seeds, cuttings and stem-tip cultures for growth and sweet diterpene glucosides.

PubMed

Tamura, Y; Nakamura, S; Fukui, H; Tabata, M

1984-10-01

The growth and sweet diterpene glucosides of Stevia plants propagated by stem-tip cultures were compared with those of the control plants propagated by seeds. There was no significant difference between the two groups both in growth and in chemical composition. As for the contents of sweet diterpene glucosides, however, the clonal plants showed significantly smaller variations than the sexually propagated plants; they were almost as homogeneous as the plants propagated by cuttings. These results suggest that the clonal propagation by stem-tip culture is an effective method of obtaining a population of uniform plants for the production of sweet diterpene glucosides.

Propolis Diterpenes as a Remarkable Bio-Source for Drug Discovery Development: A Review.

PubMed

Aminimoghadamfarouj, Noushin; Nematollahi, Alireza

2017-06-17

Propolis is one of the complex, but valuable, bio-sources for discovering therapeutic compounds. Diterpenes are organic compounds composed of four isoprene units and are known for their biological and pharmacological characteristics, such as antibacterial, anticancer, and anti-inflammatory activities. Recently, advancements have been made in the development of antibacterial and anticancer leads from propolis-isolated diterpenes, and scrutiny of these compounds is being pursued. Thus, this review covers the progress in this arena, with a focus on the chemistry and biological activities of propolis diterpenes. It is anticipated that important information, in a comprehensive and concise manner, will be delivered here for better understanding of natural product drug discovery research.

Propolis Diterpenes as a Remarkable Bio-Source for Drug Discovery Development: A Review

PubMed Central

Aminimoghadamfarouj, Noushin; Nematollahi, Alireza

2017-01-01

Propolis is one of the complex, but valuable, bio-sources for discovering therapeutic compounds. Diterpenes are organic compounds composed of four isoprene units and are known for their biological and pharmacological characteristics, such as antibacterial, anticancer, and anti-inflammatory activities. Recently, advancements have been made in the development of antibacterial and anticancer leads from propolis-isolated diterpenes, and scrutiny of these compounds is being pursued. Thus, this review covers the progress in this arena, with a focus on the chemistry and biological activities of propolis diterpenes. It is anticipated that important information, in a comprehensive and concise manner, will be delivered here for better understanding of natural product drug discovery research. PMID:28629133

21 CFR 175.260 - Partial phosphoric acid esters of polyester resins.

Code of Federal Regulations, 2014 CFR

2014-04-01

... section, partial phosphoric acid esters of polyester resins are prepared by the reaction of trimellitic anhydride with 2,2-dimethyl-1,3-propanediol followed by reaction of the resin thus produced with phosphoric... characterizing the type of food and under the conditions of time and temperature characterizing the conditions of...

Extraction of High Quality DNA from Seized Moroccan Cannabis Resin (Hashish)

PubMed Central

El Alaoui, Moulay Abdelaziz; Melloul, Marouane; Alaoui Amine, Sanaâ; Stambouli, Hamid; El Bouri, Aziz; Soulaymani, Abdelmajid; El Fahime, Elmostafa

2013-01-01

The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish) free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004) adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR) amplification of tetrahydrocannabinolic acid (THCA) synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish) resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances. PMID:24124454

Mass spectrometric methodology for the analysis of highly oxidized diterpenoid acids in Old Master paintings.

PubMed

Berg; Boon; Pastorova; Spetter

2000-04-01

Diterpenoid resins from larch and pine trees and the corresponding fractions in a >100-year-old wax-resin adhesive and varnish and a 200-year-old resin/oil paint sample were analysed with by gas chromatography/mass spectrometry (GC/MS) using several off-line and on-line derivatization methods. The main resin compounds were highly oxidized abietic acids. Important products found are hydroxydehydroabietic acids (OH-DHAs), 7-oxoDHA, di-OH-DHAs and 15-OH-7-oxoDHA. The last two compounds have not been reported to occur in artworks before. Larixyl acetate, an important marker from larch resins, was found to be still present in high amounts in the adhesive. A large number of mass spectra of the different oxidation products and larixol and larixyl acetate are presented and their fragmentation behaviour under electron impact conditions is discussed. An index for the degree of oxidation (IDOX) of the abietic acids is presented as an indicator of the degree of oxidation of the matrix in which the resin is present. The IDOX was 0.10, 0.67, 0.81 and 0.76 for the fresh resins, the dark-aged adhesive, the aged varnish and the resin/oil paint, respectively (measured with pyrolysis (Py)-tetramethylammonium hydroxide (TMAH)-GC/MS). Py-TMAH-GC/MS and direct temperature-resolved mass spectrometry are reliable, valuable and fast techniques for the assessment of the presence and degree of oxidation of diterpenoid resins. Copyright 2000 John Wiley & Sons, Ltd.

[The qualitative analysis and quantitative analysis of purification of salvianolic acids by macroreticular resin].

PubMed

Fang, Xin-sheng; Tan, Xiao-mei

2005-09-01

To purify salvianolic acids by macroreticular resin,then mensurate the contents of salvianolic acids and analyse the chromatogram with HPLC. Make salvianolic acids with macroreticular resin; mensurate the content of Salvianolic acids with UV spestrophotometry: the control compound is protocaechuic aldehyde, and the wavelength is 281 nm. Analysis the chromatogram with HPLC, and compare the chromatogram in different technics: zorbax ODS column (4.6 mm x 250 mm, 5 microm), mobilephase: 1% aceticacid-water and methanol in different proportions, the wavelength is 281 nm. The contents of salvianolic acids is 53.8%; HPLC chromatogram indicate that the method is reasonable to make salvianolic acids. Determination of contents and HPLC chromatogram can control the quality of Salvianolic acids more accurately.

Molecular Cloning and Functional Analysis of Gene Clusters for the Biosynthesis of Indole-Diterpenes in Penicillium crustosum and P. janthinellum

PubMed Central

Nicholson, Matthew J.; Eaton, Carla J.; Stärkel, Cornelia; Tapper, Brian A.; Cox, Murray P.; Scott, Barry

2015-01-01

The penitremane and janthitremane families of indole-diterpenes are abundant natural products synthesized by Penicillium crustosum and P. janthinellum. Using a combination of PCR, cosmid library screening, and Illumina sequencing we have identified gene clusters encoding enzymes for the synthesis of these compounds. Targeted deletion of penP in P. crustosum abolished the synthesis of penitrems A, B, D, E, and F, and led to accumulation of paspaline, a key intermediate for paxilline biosynthesis in P. paxilli. Similarly, deletion of janP and janD in P. janthinellum abolished the synthesis of prenyl-elaborated indole-diterpenes, and led to accumulation in the latter of 13-desoxypaxilline, a key intermediate for the synthesis of the structurally related aflatremanes synthesized by Aspergillus flavus. This study helps resolve the genetic basis for the complexity of indole-diterpene natural products found within the Penicillium and Aspergillus species. All indole-diterpene gene clusters identified to date have a core set of genes for the synthesis of paspaline and a suite of genes encoding multi-functional cytochrome P450 monooxygenases, FAD dependent monooxygenases, and prenyl transferases that catalyse various regio- and stereo- specific oxidations that give rise to the diversity of indole-diterpene products synthesized by this group of fungi. PMID:26213965

Cytotoxic Effects of Sarcophyton sp. Soft Corals—Is There a Correlation to Their NMR Fingerprints?

PubMed Central

Farag, Mohamed A.; Fekry, Mostafa I.; Al-Hammady, Montasser A.; Khalil, Mohamed N.; El-Seedi, Hesham R.; Meyer, Achim; Westphal, Hildegard; Wessjohann, Ludger A.

2017-01-01

Sarcophyton sp. soft corals are rich in cembranoid diterpenes, which represent the main chemical defense of corals against their natural predators in addition to their myriad biological effects in humans. Quantitative NMR (qNMR) was applied for assessing the diterpene variation in 16 soft coral specimens in the context of their genotype, origin, and growing habitat. qNMR revealed high diterpene levels in Sarcophyton sp. compared to Sinularia and Lobophyton, with (ent)sarcophines as major components (17–100 µg/mg) of the coral tissues. Multivariate data analysis was employed to classify samples based on the quantified level of diterpenes, and compared to the untargeted NMR approach. Results revealed that qNMR provided a stronger classification model of Sarcophyton sp. than untargeted NMR fingerprinting. Additionally, cytotoxicity of soft coral crude extracts was assessed against androgen-dependent prostate cancer cell lines (PC3) and androgen-independent colon cancer cell lines (HT-29), with IC50 values ranging from 10–60 µg/mL. No obvious correlation between the extracts’ IC50 values and their diterpene levels was found using either Spearman or Pearson correlations. This suggests that this type of bioactivity may not be easily predicted by NMR metabolomics in soft corals, or is not strongly correlated to measured diterpene levels. PMID:28677625

Cytotoxic Effects of Sarcophyton sp. Soft Corals-Is There a Correlation to Their NMR Fingerprints?

PubMed

Farag, Mohamed A; Fekry, Mostafa I; Al-Hammady, Montasser A; Khalil, Mohamed N; El-Seedi, Hesham R; Meyer, Achim; Porzel, Andrea; Westphal, Hildegard; Wessjohann, Ludger A

2017-07-04

Sarcophyton sp. soft corals are rich in cembranoid diterpenes, which represent the main chemical defense of corals against their natural predators in addition to their myriad biological effects in humans. Quantitative NMR (qNMR) was applied for assessing the diterpene variation in 16 soft coral specimens in the context of their genotype, origin, and growing habitat. qNMR revealed high diterpene levels in Sarcophyton sp. compared to Sinularia and Lobophyton , with (ent)sarcophines as major components (17-100 µg/mg) of the coral tissues. Multivariate data analysis was employed to classify samples based on the quantified level of diterpenes, and compared to the untargeted NMR approach. Results revealed that qNMR provided a stronger classification model of Sarcophyton sp. than untargeted NMR fingerprinting. Additionally, cytotoxicity of soft coral crude extracts was assessed against androgen-dependent prostate cancer cell lines (PC3) and androgen-independent colon cancer cell lines (HT-29), with IC 50 values ranging from 10-60 µg/mL. No obvious correlation between the extracts' IC 50 values and their diterpene levels was found using either Spearman or Pearson correlations. This suggests that this type of bioactivity may not be easily predicted by NMR metabolomics in soft corals, or is not strongly correlated to measured diterpene levels.

Labdane diterpenes protect against anoxia/reperfusion injury in cardiomyocytes: involvement of AKT activation

PubMed Central

Cuadrado, I; Fernández-Velasco, M; Boscá, L; de las Heras, B

2011-01-01

Several labdane diterpenes exert anti-inflammatory and cytoprotective actions; therefore, we have investigated whether these molecules protect cardiomyocytes in an anoxia/reperfusion (A/R) model, establishing the molecular mechanisms involved in the process. The cardioprotective activity of three diterpenes (T1, T2 and T3) was studied in the H9c2 cell line and in isolated rat cardiomyocyte subjected to A/R injury. In both cases, treatment with diterpenes T1 and T2 protected from A/R-induced apoptosis, as deduced by a decrease in the percentage of apoptotic and caspase-3 active positive cells, a decrease in the Bcl-2/Bax ratio and an increase in the expression of antiapoptotic proteins. Analysis of cell survival signaling pathways showed that diterpenes T1 and T2 added after A/R increased phospho-AKT and phospho-ERK 1/2 levels. These cardioprotective effects were lost when AKT activity was pharmacologically inhibited. Moreover, the labdane-induced cardioprotection involves activation of AMPK, suggesting a role for energy homeostasis in their mechanism of action. Labdane diterpenes (T1 and T2) also exerted cardioprotective effects against A/R-induced injury in isolated cardiomyocytes and the mechanisms involved activation of specific survival signals (PI3K/AKT pathways, ERK1/2 and AMPK) and inhibition of apoptosis. PMID:22071634

Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

PubMed

Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

2015-09-01

A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

Proteomic Analysis of the Endosperm Ontogeny of Jatropha curcas L. Seeds.

PubMed

Shah, Mohibullah; Soares, Emanoella L; Carvalho, Paulo C; Soares, Arlete A; Domont, Gilberto B; Nogueira, Fábio C S; Campos, Francisco A P

2015-06-05

Seeds of Jatropha curcas L. represent a potential source of raw material for the production of biodiesel. However, this use is hampered by the lack of basic information on the biosynthetic pathways associated with synthesis of toxic diterpenes, fatty acids, and triacylglycerols, as well as the pattern of deposition of storage proteins during seed development. In this study, we performed an in-depth proteome analysis of the endosperm isolated from five developmental stages which resulted in the identification of 1517, 1256, 1033, 752, and 307 proteins, respectively, summing up 1760 different proteins. Proteins with similar label free quantitation expression pattern were grouped into five clusters. The biological significance of these identifications is discussed with special focus on the analysis of seed storage proteins, proteins involved in the metabolism of fatty acids, carbohydrates, toxic components and proteolytic processing. Although several enzymes belonging to the biosynthesis of diterpenoid precursors were identified, we were unable to find any terpene synthase/cyclase, indicating that the synthesis of phorbol esters, the main toxic diterpenes, does not occur in seeds. The strategy used enabled us to provide a first in depth proteome analysis of the developing endosperm of this biodiesel plant, providing an important glimpse into the enzymatic machinery devoted to the production of C and N sources to sustain seed development.

Influence of phosphoproteins' biomimetic analogs on remineralization of mineral-depleted resin-dentin interfaces created with ion-releasing resin-based systems.

PubMed

Sauro, Salvatore; Osorio, Raquel; Watson, Timothy F; Toledano, Manuel

2015-07-01

The study aimed at evaluating the remineralization of acid-etched dentin pre-treated with primers containing biomimetic analogs and bonded using an ion-releasing light-curable resin-based material. An experimental etch-and-rinse adhesive system filled with Ca(2+), PO4(3-)-releasing Ca-Silicate micro-fillers was created along with two experimental primers containing biomimetic analogs such as sodium trimetaphosphate (TMP) and/or polyaspartic acid (PLA). Dentin specimens etched with 37% H3PO4 were pre-treated with two different aqueous primers containing the polyanionic biomimetic analogs or deionized water and subsequently bonded using the experimental resin-based materials. The specimens were sectioned and analyzed by AFM/nanoindentation to evaluate changes in the modulus of elasticity (Ei) across the resin-dentin interface at different AS storage periods (up to 90 days). Raman cluster analysis was also performed to evaluate the chemical changes along the interface. The phosphate uptake by the acid-etched dentin was evaluated using the ATR-FTIR. Additional resin-dentin specimens were tested for microtensile bond strength. SEM examination was performed after de-bonding, while confocal laser microscopy was used to evaluate the interfaces ultramorphology and micropermeability. Both biomimetic primers induced phosphate uptake by acid-etched dentin. Specimens created with the ion-releasing resin in combination with the pre-treatment primers containing either PLA and TMA showed the greatest recovery of the Ei of the hybrid layer, with no decrease in μTBS (p>0.05) after 3-month AS storage. The ion-releasing resin applied after use of the biomimetic primers showed the greatest reduction in micropermeability due to mineral precipitation; these results were confirmed using SEM. The use of the ion-releasing resin-based system applied to acid-etched dentin pre-treated with biomimetic primers containing analogs of phosphoproteins such as poly-l-aspartic acid and/or sodium trimetaphosphate provides a suitable bonding approach for biomimetic remineralization of resin-dentin interfaces. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Method of purifying neutral organophosphorus extractants

DOEpatents

Horwitz, E. Philip; Gatrone, Ralph C.; Chiarizia, Renato

1988-01-01

A method for removing acidic contaminants from neutral mono and bifunctional organophosphorous extractants by contacting the extractant with a macroporous cation exchange resin in the H.sup.+ state followed by contact with a macroporous anion exchange resin in the OH.sup.- state, whereupon the resins take up the acidic contaminants from the extractant, purifying the extractant and improving its extraction capability.

Influence of a peracetic acid-based immersion on indirect composite resin.

PubMed

Samuel, Susana Maria Werner; Fracaro, Gisele Baggio; Collares, Fabrício Mezzomo; Leitune, Vicente Castelo Branco; Campregher, Ulisses Bastos

2011-06-01

The aim of this study was to evaluate the influence of immersion in a 0.2% peracetic acid-based disinfectant on the three-point flexural strength, water sorption and water solubility of an indirect composite resin. Specimens were produced according to ISO 4049:2000 specifications and were divided in two groups: Control group, with no disinfection and Disinfected group, with three 10 min immersions in the peracetic acid intercalated with 10 min immersions in sterile distilled water. All evaluations were conducted in compliance with ISO specifications. Three-point flexural strength, water sorption and solubility of indirect composite resin before and after immersion showed no statistical significant differences (p > 0.05) and met ISO standard requirements. Immersion in peracetic acid solution showed no influence in indirect composite resin tested properties.

METHOD OF SEPARATING RARE EARTHS BY ION EXCHANGE

DOEpatents

Spedding, F.H.; Powell, J.E.

1960-10-18

A process is given for separating yttrium and rare earth values having atomic numbers of from 57 through 60 and 68 through 71 from an aqueous solution whose pH value can range from 1 to 9. All rare earths and yttrium are first adsorbed on a cation exchange resin, and they are then eluted with a solution of N-hydroxyethylethylenediaminetriacetic acid (HEDTA) in the order of decreasing atomic number, yttrium behaving like element 61; the effluents are collected in fractions. The HEDTA is recovered by elution with ammonia solution and the resin is regenerated with sulfuric acid. Rare earths are precipitated from the various effluents with oxalic acid, and each supernatant is passed over cation exchange resin for adsorption of HEDTA and nonprecipitated rare earths: the oxalic acid is not retained by the resin.

Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column.

PubMed

Novaes, Fábio Junior Moreira; Kulsing, Chadin; Bizzo, Humberto Ribeiro; de Aquino Neto, Francisco Radler; Rezende, Claudia Moraes; Marriott, Philip John

2018-02-09

Comprehensive two-dimensional gas chromatography (GC×GC) approaches with cryogenic modulation were developed for the qualitative analysis of selected low volatility compounds in raw coffee bean extracts, without derivatisation. The approaches employed short first ( 1 D) and second ( 2 D) dimension columns, specifically a 1 D 65% phenyl methyl siloxane column (11m) and a 2 D 5% phenyl methyl siloxane column (1m), which allowed elution of high molar mass compounds (e.g.>600Da). Solutes included hydrocarbons, fatty acids, diterpenes, tocopherols, sterols, diterpene esters, and di- and triacylglycerides. An oven temperature program up to 370°C was employed. The effects of experimental conditions were investigated, revealing that the GC×GC results strongly depended on the cryogenic trap T, and oven T program. An appropriate condition was selected and further applied for group type analysis of low volatility compounds in green Arabica coffee beans. Retention indices were compiled for 1D GC analysis and were similar for the composite column data in GC×GC. The elution of some compounds was confirmed by use of authentic standards. The approach allowed direct analysis of coffee extract in ethyl acetate solution, with improved analyte peak capacity (approximately 200 compounds were detected) without prior fractionation or pre-treatment of the sample. This avoided potential hydrolysis of high molar mass conjugate esters as well as degradation of thermally labile compounds such as the derivatives of the diterpenes cafestol and kahweol. Copyright © 2017 Elsevier B.V. All rights reserved.

Recovery of lactic acid from the pretreated fermentation broth based on a novel hyper-cross-linked meso-micropore resin: Modeling.

PubMed

Song, Mingkai; Jiao, Pengfei; Qin, Taotao; Jiang, Kangkang; Zhou, Jingwei; Zhuang, Wei; Chen, Yong; Liu, Dong; Zhu, Chenjie; Chen, Xiaochun; Ying, Hanjie; Wu, Jinglan

2017-10-01

An innovative benign process for recovery lactic acid from its fermentation broth is proposed using a novel hyper-cross-linked meso-micropore resin and water as eluent. This work focuses on modeling the competitive adsorption behaviors of glucose, lactic acid and acetic acid ternary mixture and explosion of the adsorption mechanism. The characterization results showed the resin had a large BET surface area and specific pore structure with hydrophobic properties. By analysis of the physicochemical properties of the solutes and the resin, the mechanism of the separation is proposed as hydrophobic effect and size-exclusion. Subsequently three chromatographic models were applied to predict the competitive breakthrough curves of the ternary mixture under different operating conditions. The pore diffusion was the major limiting factor for the adsorption process, which was consistent with the BET results. The novel HD-06 resin can be a good potential adsorbent for the future SMB continuous separation process. Copyright © 2017 Elsevier Ltd. All rights reserved.

Biological activity of some naturally occurring resins, gums and pigments against in vitro LDL oxidation.

PubMed

Andrikopoulos, Nikolaos K; Kaliora, Andriana C; Assimopoulou, Andreana N; Papapeorgiou, Vassilios P

2003-05-01

Naturally occurring gums and resins with beneficial pharmaceutical and nutraceutical properties were tested for their possible protective effect against copper-induced LDL oxidation in vitro. Chiosmastic gum (CMG) (Pistacia lentiscus var. Chia resin) was the most effective in protecting human LDL from oxidation. The minimum and maximum doses for the saturation phenomena of inhibition of LDL oxidation were 2.5 mg and 50 mg CMG (75.3% and 99.9%, respectively). The methanol/water extract of CMG was the most effective compared with other solvent combinations. CMG when fractionated in order to determine a structure-activity relationship showed that the total mastic essential oil, collofonium-like residue and acidic fractions of CMG exhibited a high protective activity ranging from 65.0% to 77.8%. The other natural gums and resins (CMG resin 'liquid collection', P. terebinthus var. Chia resin, dammar resin, acacia gum, tragacanth gum, storax gum) also tested as above, showed 27.0%-78.8% of the maximum LDL protection. The other naturally occurring substances, i.e. triterpenes (amyrin, oleanolic acid, ursolic acid, lupeol, 18-a-glycyrrhetinic acid) and hydroxynaphthoquinones (naphthazarin, shikonin and alkannin) showed 53.5%-78.8% and 27.0%-64.1% LDL protective activity, respectively. The combination effects (68.7%-76.2% LDL protection) of ursolic-, oleanolic- and ursodeoxycholic- acids were almost equal to the effect (75.3%) of the CMG extract in comparable doses. Copyright 2003 John Wiley & Sons, Ltd.

Novel aqueous oil-in-water emulsions containing extracts of natural coniferous resins are strongly antimicrobial against enterobacteria, staphylococci and yeasts, as well as on bacterial biofilms.

PubMed

Haapakorva, E; Holmbom, T; von Wright, A

2018-01-01

The aim of this study was to examine the antimicrobial properties of novel aqueous natural rapeseed oil/saline emulsions containing different soluble components of spruce resin. The composition of aqueous resin emulsions was analysed by GC-MS and their antimicrobial properties were studied with challenge tests and with turbidometric assays. The emulsions were strongly antimicrobial against common Gram-positive and Gram-negative bacteria (including MRSA) as well as common yeasts. Furthermore, they inhibited the biofilm formation and eradicated the microbial biofilms on tested microbes. Characteristic for the emulsions was the presence of oxidized resin acids. Other main components present in emulsions, such as lignans and coumaric acids, were not antimicrobial, when tested separately. The results indicated that the oxidized resin acids were the antimicrobial components in the emulsions. Also, there appears to be a stoichiometric relationship between the number of resin acid molecules and the number microbe cells in the antimicrobial action. The fact that these solutions do not contain abietic acid, which is the main allergenic compound in resins, suggests that these solutions would be suitable, well-tolerated antimicrobials for various medical applications. The aqueous formulation will also allow the expansion of the use of these emulsions in from medical applications to the food preservatives and disinfectants. © 2017 The Authors. Journal of Applied Microbiology published by John Wiley & Sons Ltd on behalf of the Society for Applied Microbiology.

Significance of wood extractives for wood bonding.

PubMed

Roffael, Edmone

2016-02-01

Wood contains primary extractives, which are present in all woods, and secondary extractives, which are confined in certain wood species. Extractives in wood play a major role in wood-bonding processes, as they can contribute to or determine the bonding relevant properties of wood such as acidity and wettability. Therefore, extractives play an immanent role in bonding of wood chips and wood fibres with common synthetic adhesives such as urea-formaldehyde-resins (UF-resins) and phenol-formaldehyde-resins (PF-resins). Extractives of high acidity accelerate the curing of acid curing UF-resins and decelerate bonding with alkaline hardening PF-resins. Water-soluble extractives like free sugars are detrimental for bonding of wood with cement. Polyphenolic extractives (tannins) can be used as a binder in the wood-based industry. Additionally, extractives in wood can react with formaldehyde and reduce the formaldehyde emission of wood-based panels. Moreover, some wood extractives are volatile organic compounds (VOC) and insofar also relevant to the emission of VOC from wood and wood-based panels.

Quantitative analysis of PMR-15 polyimide resin by HPLC

NASA Technical Reports Server (NTRS)

Roberts, Gary D.; Lauver, Richard W.

1987-01-01

The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

Structural Characterization of the Degradation Products of a Minor Natural Sweet Diterpene Glycoside Rebaudioside M under Acidic Conditions

PubMed Central

Prakash, Indra; Chaturvedula, Venkata Sai Prakash; Markosyan, Avetik

2014-01-01

Degradation of rebaudioside M, a minor sweet component of Stevia rebaudiana Bertoni, under conditions that simulated extreme pH and temperature conditions has been studied. Thus, rebaudioside M was treated with 0.1 M phosphoric acid solution (pH 2.0) and 80 °C temperature for 24 h. Experimental results indicated that rebaudioside M under low pH and higher temperature yielded three minor degradation compounds, whose structural characterization was performed on the basis of 1D (1H-, 13C-) & 2D (COSY, HSQC, HMBC) NMR, HRMS, MS/MS spectral data as well as enzymatic and acid hydrolysis studies. PMID:24424316

Constituents of the root of Anemone tomentosa.

PubMed

Hu, Hao-Bin; Zheng, Xu-Dong; Jian, Yu-Feng; Liu, Jian-Xin; Zhu, Ji-Hua

2011-07-01

A new diterpene glycoside, tomentoside I (1), along with eleven known compounds, including the four coumarins, 4,5-dimethoxyl-7-methylcoumarin (2), 4,7-dimethoxyl-5-methylcoumarin (3), isofraxidin (4) and fraxidin (5) as well as the seven triterpenoids, oleanolic acid (6), oleanolic acid 3-O-α-L-arabinopyranoside (7), oleanolic acid 3-O-β-D-galactopyranosyl-(1→3)-β-D-glucopyranoside (8), hederagenin 3-O-α-L-arabinopyranoside (9), betulinic acid (10), 18-hydroxyursolic acid (11) and 2α,3β,23-trihydroxyurs-12-en-28-oic acid (12) were isolated from the ethanolic extract of the root of Anemone tomentosa and their chemical structures were elucidated by spectroscopic methods. The antimicrobial activities of compounds 1-12 were measured using the agar disc-diffusion method. Also, their antioxidant activities against 1,1-diphenyl-2-picrylhydrazyl (DPPH) were evaluated.

7 CFR 160.3 - Rosin defined.

Code of Federal Regulations, 2010 CFR

2010-01-01

...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

7 CFR 160.3 - Rosin defined.

Code of Federal Regulations, 2011 CFR

2011-01-01

...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

Using Sr Resin with mixed acid matrices

DOE PAGES

McLain, Derek R.; Liu, Christine; Sudowe, Ralf

2018-03-02

Here, the quantification of radioactive material dispersed following the release of 90Sr, whether accidental or intentional, would be of high importance. Depending on the circumstances, it is possible that the contaminated materials would need to be completely digested prior to quantification. Many sample matrices require a mixture of different acids be employed to achieve total dissolution. Unfortunately, one the most common approaches for the separation of strontium, extraction chromatography with Sr Resin, has only been fully characterized in pure mineral acid solutions. This work shows that Sr Resin can be used effectively with high concentration mixtures of nitric and hydrochloricmore » acids in the presence or absence of hydrofluoric acid, thereby potentially negating the need for conversion to a pure mineral acid matrix.« less

Using Sr Resin with mixed acid matrices

DOE Office of Scientific and Technical Information (OSTI.GOV)

McLain, Derek R.; Liu, Christine; Sudowe, Ralf

Here, the quantification of radioactive material dispersed following the release of 90Sr, whether accidental or intentional, would be of high importance. Depending on the circumstances, it is possible that the contaminated materials would need to be completely digested prior to quantification. Many sample matrices require a mixture of different acids be employed to achieve total dissolution. Unfortunately, one the most common approaches for the separation of strontium, extraction chromatography with Sr Resin, has only been fully characterized in pure mineral acid solutions. This work shows that Sr Resin can be used effectively with high concentration mixtures of nitric and hydrochloricmore » acids in the presence or absence of hydrofluoric acid, thereby potentially negating the need for conversion to a pure mineral acid matrix.« less

Changes in properties of polyacid-modified composite resins (compomers) following storage in acidic solutions.

PubMed

Nicholson, J W; Gjorgievska, E; Bajraktarova, B; McKenzie, M A

2003-06-01

The interaction of three polyacid-modified composite resins (compomers) with various acidic storage solutions, and also water, over periods of time up to 6 months has been studied and compared with those of a glass-ionomer and a composite resin. This interaction has been shown to vary in a complex way with length of storage and nature of the acid, and citric acid was found to be the most aggressive storage medium for glass-ionomer cement, and also for the compomers. The pure composite resin, by contrast, was relatively unaffected by all of the acid solutions examined. In all acids, the compomers showed a distinct buffering effect, i.e. they increased the pH towards neutral, as did the glass-ionomer. The extent of this also varied with duration of storage and nature of the acid. The biaxial flexure strength was determined and found to be essentially unaffected by the complex chemical interactions with acidic storage solutions. Values obtained for the compomers were lower than those of the composite resin, but above those of the glass-ionomer. Fourier-transform infrared (FT-IR) spectroscopy was employed to study the changes in the compomers following storage in the aqueous media, but bands were broad and no detailed assignments could be made. There were changes in the region of the spectra associated with metal carboxylates however, and this indicates that the secondary acid-base reaction had occurred following water uptake.

Theoretical research into anticancer activity of diterpenes isolated from the paraiban flora.

PubMed

Ishiki, Hamilton; Junior, Francisco J B Mendonça; Santos, Paula F; Tavares, Josean F; Tavares, Josean F; Silva, Marcelo S; Scotti, Marcus T

2014-07-01

Many studies of the scientific literature discuss the anticancer activity of diterpenes inhibiting the Akt/IKK/NF-kappaB pro-survival signaling cascade, mainly by the activation of serine/threonine phosphatase PP2A. The aim of this work was to evaluate and compare the anticancer potential of three atisane, three kaurane and three trachylobane diterpenes extracted from the roots of Xylopia langsdorffiana. Thus, we investigated the reactivity (H-L(GAP) parameter), HOMO atmosphere favorable to neutralize the radical reactivity, and the docking of compounds with PP2A. With all approaches, this theoretical study showed that atisane diterpenes have favorable characteristics for antitumor activity, like electron donating ability and greater hydrophilic interactions with the enzyme, by inhibition of Akt/IKK/NF-kappaB, and activation of PP2A.

Phytochemical and pharmacological investigation of Spiraea chamaedryfolia: a contribution to the chemotaxonomy of Spiraea genus.

PubMed

Kiss, Tivadar; Cank, Kristóf Bence; Orbán-Gyapai, Orsolya; Liktor-Busa, Erika; Zomborszki, Zoltán Péter; Rutkovska, Santa; Pučka, Irēna; Németh, Anikó; Csupor, Dezső

2017-12-21

Diterpene alkaloids are secondary plant metabolites and chemotaxonomical markers with a strong biological activity. These compounds are characteristic for the Ranunculaceae family, while their occurrence in other taxa is rare. Several species of the Spiraea genus (Rosaceae) are examples of this rarity. Screening Spiraea species for alkaloid content is a chemotaxonomical approach to clarify the classification and phylogeny of the genus. Novel pharmacological findings make further investigations of Spiraea diterpene alkaloids promising. Seven Spiraea species were screened for diterpene alkaloids. Phytochemical and pharmacological investigations were performed on Spiraea chamaedryfolia, the species found to contain diterpene alkaloids. Its alkaloid-rich fractions were found to exert a remarkable xanthine-oxidase inhibitory activity and a moderate antibacterial activity. The alkaloid distribution within the root was clarified by microscopic techniques.

Photosensitive filler minimizes internal stresses in epoxy resins

NASA Technical Reports Server (NTRS)

Dillon, J. N.

1967-01-01

Photosensitive filler is added to curable epoxy resins to minimize stress from internal shrinkage during curing or polymerization. Cinnamic acid resins and cinnamal ketones may be added in the amount of 1 to 3 percent by weight of the resin mixture.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); Saintclair, Anne K. (Inventor)

1989-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solution of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4'-benzo phenone tetracarboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'oxydianiline (4,4'-ODA). By utilizing the interrelationship between coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

1991-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solutions of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4' benzophenonetetra carboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'-oxydianiline (4,4'-ODA). By utilizing the relationship among coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Effects of the peracetic acid and sodium hypochlorite on the colour stability and surface roughness of the denture base acrylic resins polymerised by microwave and water bath methods.

PubMed

Fernandes, Flavio H C N; Orsi, Iara A; Villabona, Camilo A

2013-03-01

This study evaluated the surface roughness (Ra) and color stability of acrylic resin colors (Lucitone 550, QC-20 and Vipi-Wave) used for fabricating bases for complete, removable dentures, overdentures and prosthetic protocol after immersion in chemical disinfectants (1% sodium hypochlorite and 2% peracetic acid) for 30 and 60 minutes. Sixty specimens were made of each commercial brand of resin composite, and divided into 2 groups according to the chemical disinfectants. Specimens had undergone the finishing and polishing procedures, the initial color and roughness measurements were taken (t=0), and after this, ten test specimens of each commercial brand of resin composite were immersed in sodium hypochlorite and ten in peracetic acid, for 30 and 60 minutes, with measurements being taken after each immersion period. These data were submitted to statistical analysis. There was evidence of an increase in Ra after 30 minutes immersion in the disinfectants in all the resins, with QC-20 presenting the highest Ra values, and Vipi-Wave the lowest. After 60 minutes immersion in the disinfectants all the resins presented statistically significant color alteration. Disinfection with 1% sodium hypochlorite and peracetic acid altered the properties of roughness and color of the resins. © 2012 The Gerodontology Society and John Wiley & Sons A/S.

Adsorptive separation in bioprocess engineering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, E.W.Y.

1987-01-01

The invention and development of an energy-efficient separation technique for recovery of desired chemicals from biomass conversion would greatly enhance the economic viability of this bioprocess. Adsorptive separation of several chemicals from aqueous solution was studied in this thesis. The desired species were recovered from the dilute aqueous solution by using crosslinked polyvinylpyridine resin to effect selective sorption. The sorbed chemicals were then removed from the resin by either thermal regeneration or elution with some appropriate desorbents. The effects of temperature, pH value, and solute concentration on resin swelling were investigated. The adsorption equilibrium isotherms, resin capacities and resin selectivitiesmore » of methanol, ethanol, 1-propanol, isopropanol, glycerol, acetone, 1-butanol, tert-butanol, and 2,3-butanediol were determined to study the homologies. Furthermore, acetic acid, butyric acid, hydrochloric acid, lactic acid, and sulfuric acid were recovered from very dilute aqueous solutions. The concentration of the sorbed chemical in the stationary phase can be many times higher than in the mobile phase for some acids. Finally, different types of equilibrium isotherms were used to fit the experimental data. A mathematical model was developed by using the theory of interference to predict the breakthrough curves and the process efficiency to provide information for large-scale process design and development.« less

Resin-dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding. Part II: Effects of mechanical cycling load on microtensile bond strengths.

PubMed

Sauro, Salvatore; Toledano, Manuel; Aguilera, Fatima Sánchez; Mannocci, Francesco; Pashley, David H; Tay, Franklin R; Watson, Timothy F; Osorio, Raquel

2011-06-01

To compare microtensile bond strengths (MTBS) subsequent to load cycling of resin bonded acid-etched or EDTA-treated dentin using a modified ethanol wet-bonding technique. Flat dentin surfaces were obtained from extracted human molars and conditioned using 37% H(3)PO(4) (PA) (15s) or 0.1M EDTA (60s). Five experimental adhesives and one commercial bonding agent were applied to the dentin and light-cured. Solvated experimental resins (50% ethanol/50% comonomers) were used as primers and their respective neat resins were used as the adhesives. The resin-bonded teeth were stored in distilled water (24h) or submitted to 5000 loading cycles of 90N. The bonded teeth were then sectioned in beams for MTBS. Modes of failure were examined by scanning electron microscopy. The most hydrophobic resin 1 gave the lowest bond strength values to both acid and EDTA-treated dentin. The hydrophobic resin 2 applied to EDTA-treated dentin showed lower bond strengths after cycling load but this did not occur when it was bonded to PA-etched dentin. Resins 3 and 4, which contained hydrophilic monomers, gave higher bond strengths to both EDTA-treated or acid-etched dentin and showed no significant difference after load cycling. The most hydrophilic resin 5 showed no significant difference in bond strengths after cycling loading when bonded to EDTA or phosphoric acid treated dentin but exhibited low bond strengths. The presence of different functional monomers influences the MTBS of the adhesive systems when submitted to cyclic loads. Adhesives containing hydrophilic comonomers are not affected by cycling load challenge especially when applied on EDTA-treated dentin followed by ethanol wet bonding. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Energy value of paraquat-treated and resin-soaked lobolly pine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kossuth, S.V.; Roberts, D.R.; Huffman, J.B.

1984-07-01

With a basal injector, loblolly pines were treated with 5% paraquat cation (weight/weight basis) and harvested after 18 months. The resin acid, turpentine, moisture content (MC) and energy value were measured in three bolts of the stem. In bolt 1, the first 152 cm above the injection site, the increase in resin acids was 392% and in turpentine, 564%. Within the whole stem (the first two 152 cm bolts and the third bolt to a 7.6 cm inside-bark diameter) resin acids and turpentine increased 203 and 296% respectively. Moisture content was reduced 9%, 8%, and 8% in bolts 1, 2more » and 3, respectively. Turpentine from treated and untreated trees had an average heating value of 19,369 cal/g. When weighted for volume, net energy content was 7.8% greater for treated than control trees because of the increase in resin, including turpentine and the lowered MC.« less

Labdane Diterpenes from the Fruits of Sinopodophyllum emodi.

PubMed

Sun, Yan-Jun; Gao, Mei-Ling; Zhang, Yan-Li; Wang, Jun-Min; Wu, Ya; Wang, Yu; Liu, Tao

2016-03-31

Two new labdane diterpenes, sinoditerpene A (1) and B (2), were isolated from the fruits of Sinopodophyllum emodi, along with two known analogues 3 and 4. Their structures were established on the basis of extensive spectroscopic analysis. The isolation of compounds 1-4 represents the first report of diterpenes from the genus Sinopodophyllum. The cytotoxic activities of all isolated compounds were evaluated in comparison with 5-fluorouracil against the MCF-7 and HepG2 cell lines, towards which 3 showed more potent cytotoxicity.

Antiproliferative activity of Greek propolis.

PubMed

Pratsinis, Harris; Kletsas, Dimitris; Melliou, Eleni; Chinou, Ioanna

2010-04-01

The butanolic extract and the isolated chemical constituents, mainly diterpenes and flavonoids, from Greek propolis have been tested for their cytostatic activities against human malignant and normal cell strains. The extract and the diterpenes were found to be the most active against HT-29 human colon adenocarcinoma cells, without affecting normal human cells. Manool, a diterpene isolated for the first time from Greek propolis, was the most active compound, arresting the cancer cells at the G(2)/M phase of the cell cycle.

Analytical method for dissolved-organic carbon fractionation

USGS Publications Warehouse

Leenheer, Jerry A.; Huffman, Edward W. D.

1979-01-01

A standard procedure for analytical-scale dissolved organic carbon fractionation is presented, whereby dissolved organic carbon in water is first fractionated by a nonionic macroreticular resin into acid, base, and neutral hydrophobic organic solute fractions, and next fractionated by ion-exchange resins into acid, base, and neutral hydrophilic solute fractions. The hydrophobic solutes are defined as those sorbed on a nonionic, acrylic-ester macroreticular resin and are differentiated into acid, base, and nautral fractions by sorption/desorption controlled by pH adjustment. The hydrophilic bases are next sorbed on strong-acid ion-exchange resin, followed by sorption of hydrophilic acids on a strong-base ion-exchange resin. Hydrophilic neutrals are not sorbed and remain dissolved in the deionized water at the end of the fractionation procedure. The complete fractionation can be performed on a 200-milliliter filtered water sample, whose dissolved organic carbon content is 5-25 mg/L and whose specific conductance is less than 2,000 μmhos/cm at 25°C. The applications of dissolved organic carbon fractionation analysis range from field studies of changes of organic solute composition with synthetic fossil fuel production, to fundamental studies of the nature of sorption processes.

Production of sodium-22 from proton irradiated aluminum

DOEpatents

Taylor, Wayne A.; Heaton, Richard C.; Jamriska, David J.

1996-01-01

A process for selective separation of sodium-22 from a proton irradiated minum target including dissolving a proton irradiated aluminum target in hydrochloric acid to form a first solution including aluminum ions and sodium ions, separating a portion of the aluminum ions from the first solution by crystallization of an aluminum salt, contacting the remaining first solution with an anion exchange resin whereby ions selected from the group consisting of iron and copper are selectively absorbed by the anion exchange resin while aluminum ions and sodium ions remain in solution, contacting the solution with an cation exchange resin whereby aluminum ions and sodium ions are adsorbed by the cation exchange resin, and, contacting the cation exchange resin with an acid solution capable of selectively separating the adsorbed sodium ions from the cation exchange resin while aluminum ions remain adsorbed on the cation exchange resin is disclosed.

Acid etching of titanium for bonding with veneering composite resins.

PubMed

Ban, Seiji; Taniki, Toshio; Sato, Hideo; Kono, Hiroshi; Iwaya, Yukari; Miyamoto, Motoharu

2006-06-01

Commercially pure titanium (cpTi) was etched using three concentrated acids: 18% HCl, 43% H3PO4, and 48% H2SO4. The bond strengths between five types of veneering composite resin and eight cpTi treatments (involving combinations of sandblasting, acid etching in 48% H2SO4, and vacuum firing) were determined before and after 10,000 and 20,000 thermal cycles. There were no significant differences in the bond strength of resin to cpTi after etching in 48% H2SO4 at 90 degrees C for 15 minutes, at 60 degrees C for 15, 30, or 60 minutes, and after sandblasting with and without vacuum firing (p > 0.05); moreover, these treatments yielded the highest values. As for vacuum firing, it had no significant effect on resin bond strength to cpTi before or after 10,000 and 20,000 thermal cycles. We therefore concluded that acid etching in concentrated H2SO4 is a simple and effective surface modification method of titanium for bonding to veneering composite resins.

Reusable chelating resins concentrate metal ions from highly dilute solutions

NASA Technical Reports Server (NTRS)

Bauman, A. J.; Weetal, H. H.; Weliky, N.

1966-01-01

Column chromatographic method uses new metal chelating resins for recovering heavy-metal ions from highly dilute solutions. The absorbed heavy-metal cations may be removed from the chelating resins by acid or base washes. The resins are reusable after the washes are completed.

Development of solvent-free offset ink using vegetable oil esters and high molecular-weight resin.

PubMed

Park, Jung Min; Kim, Young Han; Kim, Sung Bin

2013-01-01

In the development of solvent-free offset ink, the roles of resin molecular weight and used solvent on the ink performance were evaluated by examining the relationship between the various properties of resin and solvent and print quality. To find the best performing resin, the soy-oil fatty acid methyl ester (FAME) was applied to the five modified-phenolic resins having different molecular weights. It is found from the experimental results that the ink made of higher molecular weight and better solubility resin gives better printability and print quality. It is because larger molecular weight resin with better solubility gives higher rate of ink transfer. From the ink application of different esters to high molecular weight resin, the best printing performance was yielded from the soy-oil fatty acid butyl ester (FABE). It is due to its high kinematic viscosity resulting in the smallest change of ink transfer weight upon multiple number of printing, which improves the stability of ink quality.

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2013 CFR

2013-04-01

... polyester resins are produced by the condensation of one or more of the acids listed in paragraph (a)(1) of.... Reinforcements: Asbestos Glass fiber Polyester fiber produced by the condensation of one or more of the acids...

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2012 CFR

2012-04-01

... polyester resins are produced by the condensation of one or more of the acids listed in paragraph (a)(1) of.... Reinforcements: Asbestos Glass fiber Polyester fiber produced by the condensation of one or more of the acids...

Andrographis paniculata transcriptome provides molecular insights into tissue-specific accumulation of medicinal diterpenes.

PubMed

Garg, Anchal; Agrawal, Lalit; Misra, Rajesh Chandra; Sharma, Shubha; Ghosh, Sumit

2015-09-02

Kalmegh (Andrographis paniculata) has been widely exploited in traditional medicine for the treatment of infectious diseases and health disorders. Ent-labdane-related diterpene (ent-LRD) specialized (i.e., secondary) metabolites of kalmegh such as andrographolide, neoandrographolide and 14-deoxy-11,12-didehydroandrographolide, are known for variety of pharmacological activities. However, due to the lack of genomic and transcriptomic information, underlying molecular basis of ent-LRDs biosynthesis has remained largely unknown. To identify candidate genes of the ent-LRD biosynthetic pathway, we performed comparative transcriptome analysis using leaf and root tissues that differentially accumulate ent-LRDs. De novo assembly of Illumina HiSeq2000 platform-generated paired-end sequencing reads resulted into 69,011 leaf and 64,244 root transcripts which were assembled into a total of 84,628 unique transcripts. Annotation of these transcripts to the Uniprot, Kyoto Encyclopedia of Genes and Genomes (KEGG) and Carbohydrate-Active Enzymes (CAZy) databases identified candidate transcripts of the ent-LRD biosynthetic pathway. These included transcripts that encode enzymes of the plastidial 2C-methyl-D-erythritol-4-phosphate pathway which provides C5 isoprenoid precursors for the ent-LRDs biosynthesis, geranylgeranyl diphosphate synthase, class II diterpene synthase (diTPS), cytochrome P450 monooxygenase and glycosyltransferase. Three class II diTPSs (ApCPS1, ApCPS2 and ApCPS3) that showed distinct tissue-specific expression profiles and are phylogenetically related to the dicotyledon ent-copalyl diphosphate synthases, are identified. ApCPS1, ApCPS2 and ApCPS3 encode for 832-, 817- and 797- amino acids proteins of 55-63 % identity, respectively. Spatio-temporal patterns of transcripts and ent-LRDs accumulation are consistent with the involvement of ApCPS1 in general (i.e., primary) metabolism for the biosynthesis of phytohormone gibberellin, ApCPS2 in leaf specialized ent-LRDs biosynthesis and ApCPS3 in root diterpene biosynthesis. Moreover, simple sequence repeats (SSRs) that might assist in genotyping and developing specific chemotypes were identified in transcripts of the specialized metabolic pathways, including ent-LRDs. Comparative analysis of root and leaf transcriptomes disclosed novel genes of the ent-LRD biosynthetic pathway, including three class II diTPSs that showed discrete spatio-temporal expression patterns; thus, suggesting their participation into distinct diterpene metabolic pathways of kalmegh. Overall, these results will be useful in understanding molecular basis of the medicinal ent-LRDs biosynthesis and developing breeding strategies for improving their yields.

Tall oil precursors of Douglas fir

Treesearch

Daniel O. Foster; Duane F. Zinkel; Anthony H. Conner

1980-01-01

The sapwood and heartwood extractives of Douglas fir [Pseudotsuga menziesii (Mirb.) Franco] and the tall oil in the kraft black liquor were characterized. On pulping, isomerization and conversion of conjugated resin acids to dehydroabietic acid was observed. Recovery of both fatty and resin acids from pulping was lower than predicted from the extractive composition....

Paraquat-induced lightwood in two European conifers - Scotch pine and Norway spruce

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wroblewska, H.; Conner, A.H.; Rowe, J.W.

1978-04-01

Paraquat treatment induced oleoresin-soaked lightwood in Scotch pine; borehole and ax-frill treatment methods were equally effective. Paraquat treatment of Norway spruce induced limited lightwood formation accompanied by heavy external oleoresin exudation. Thus paraquat treatment of Scotch pine and possibly Norway spruce could be commercially advantageous for increasing naval stores production from these species. Analysis of tall oil precursors (nonvolatile ether extractives) for resin acids, fatty acids, and nonsaponifiables showed that the increase from paraquat treatment was mainly from an increased resin acid content. The chemical composition of the resin acids from the lightwood and control wood areas was similar andmore » consisted of the usual pimaric and abietic type resin acids found in conifers. The fatty acids were predominately unsaturated C/sub 18/ isomers. Turpentine of both species consisted mainly of ..cap alpha..-pinene, ..beta..-pinene, and 3-carene. The composition of the turpentine from the Scotch pine lightwood did not differ from that of the control wood. However, turpentine from the Norway spruce lightwood had an increased 3-carene content compared to that from the control.« less

Separation of organic ion exchange resins from sludge -- engineering study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duncan, J.B.

1998-08-25

This engineering study evaluates the use of physical separation technologies to separate organic ion exchange resin from KE Basin sludge prior to nitric acid dissolution. This separation is necessitate to prevent nitration of the organics in the acid dissolver. The technologies under consideration are: screening, sedimentation, elutriation. The recommended approach is to first screen the Sludge and resin 300 microns then subject the 300 microns plus material to elutriation.

Diterpenes as lead molecules against neglected tropical diseases.

PubMed

Barros de Alencar, Marcus Vinícius Oliveira; de Castro E Sousa, João Marcelo; Rolim, Hercília Maria Lins; de Medeiros, Maria das Graças Freire; Cerqueira, Gilberto Santos; de Castro Almeida, Fernanda Regina; Citó, Antônia Maria das Graças Lopes; Ferreira, Paulo Michel Pinheiro; Lopes, José Arimatéia Dantas; de Carvalho Melo-Cavalcante, Ana Amélia; Islam, Md Torequl

2017-02-01

Nowadays, neglected tropical diseases (NTDs) are reported to be present everywhere. Poor and developing areas in the world have received great attention to NTDs. Drug resistance, safety profile, and various challenges stimulate the search for alternative medications. Plant-based drugs are viewed with great interest, as they are believed to be devoid of side effects. Diterpenes, a family of essential oils, have showed attractive biological effects. A systematic review of the literature was carried out to summarize available evidences of diterpenes against NTDs. For this, databases were searched using specific search terms. Among the 2338 collected reports, a total of 181 articles were included in this review. Of them, 148 dealt with investigations using single organisms, and 33 used multiple organisms. No mechanisms of action were reported in the case of 164 reports. A total of 93.92% were related to nonclinical studies, and 4.42% and 1.66% dealt with preclinical and clinical studies, respectively. The review displays that many diterpenes are effective upon Chagas disease, chikungunya, echinococcosis, dengue, leishmaniasis, leprosy, lymphatic filariasis, malaria, schistosomiasis, and tuberculosis. Indeed, diterpenes are amazing drug candidates against NTDs. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Molecular docking and inhibition kinetics of α-glucosidase activity by labdane diterpenes isolated from tora seeds (Alpinia nigra B.L. Burtt.).

PubMed

Ghosh, Sudipta; Rangan, Latha

2015-02-01

Current approach against type 2 diabetes involves α-glucosidase inhibitors like acarbose associated with many side effects. Therefore, as an alternative to the existing drug, many natural products mainly from plant sources have been investigated which inhibit α-glucosidase. Here, we have selected medicinally important Alpinia nigra to explore its α-glucosidase inhibitory activity. Organic extracts of seeds and two purified natural diterpenes I: (E)-labda-8(17), 12-diene-15, 16-dial and II: (E)-8β, 17-epoxylabd-12-ene-15, 16-dial from A. nigra were investigated towards inhibition of α-glucosidase activity. Dose-dependent inhibition pattern were observed for seed extracts and both the compounds. Further, inhibition kinetics studies of the diterpenes indicated a non-competitive type of inhibition against α-glucosidase. Docking studies were carried out which revealed that both the diterpenes interacted within the active site of N-terminal and C-terminal domain of human maltase-glucoamylase enzyme, respectively. This is the first report of α-glucosidase inhibitory activity of these isolated diterpenes and their higher inhibitory potential than any terpenoids studied till date against α-glucosidase.

SEPARATION OF PLUTONIUM FROM AQUEOUS SOLUTIONS BY ION-EXCHANGE

DOEpatents

Schubert, J.

1958-06-01

A process is described for the separation of plutonium from an aqueous solution of a plutonium salt, which comprises adding to the solution an acid of the group consisting of sulfuric acid, phosphoric acid, and oxalic acid, and mixtures thereof to provide an acid concentration between 0.0001 and 1 M, contacting the resultant solution with a synthetic organic anion exchange resin, and separating the aqueous phase and the resin which contains the plutonium.

A Cocatalytic Effect between Meldrum's Acid and Benzoxazine Compounds in Preparation of High Performance Thermosetting Resins.

PubMed

Chen, Yi; Lin, Liang-Kai; Chiang, Shu-Jen; Liu, Ying-Ling

2017-02-01

In this work, a cocatalytic effect between Meldrum's acid (MA) and benzoxazine (Bz) compounds has been explored to build up a self-promoting curing system. Consequently, the MA/Bz reactive blend exhibits a relatively low reaction temperature compared to the required temperatures for the cross-linking reactions of the pure MA and Bz components. This feature is attractive for energy-saving processing issues. Moreover, the thermosetting resins based on the MA/Bz reactive blends have been prepared. The MA component can generate additional free volume in the resulting resins, so as to trap air in the resin matrix and consequently to bring low dielectric constants to the resins. The MA-containing agent is an effective modifier for benzoxazine resins to reduce their dielectric constants. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design and synthesis of bio-based UV curable PU acrylate resin from itaconic acid for coating applications

PubMed Central

Patil, Deepak M.; Phalak, Ganesh A.; Mhaske, S. T.

2017-01-01

Abstract UV curable PUA resin was successfully synthesized from polyol based on sustainable resource originated from itaconic acid (IA), isophorone diisocyanate (IPDI) and 2-hydroxyethyl methacrylate (HEMA). A polyol was synthesized by condensation reaction of IA with 16-hexanediol in the presence of p-Toluenesulfonic acid (pTSA). The synthesized PUA resin was characterized for its structural elucidation by using Fourier Transform Infrared Spectrophotometer (FTIR), 1H and 13C NMR spectroscopy. The synthesized UV curable PUA resin was incorporated in varying concentrations in conventional PUA coating system. The effects of varying concentration of synthesized UV curable PUA resin on rheology, crystallinity, thermal and coating properties were evaluated. The rheological behavior of the resins were evaluated at variable stress and result showed decrease in viscosity of resin as concentration of synthesized UV curable PUA resin increases in conventional PUA resin. The cured coatings have been evaluated for glass transition temperature (T g) and thermal behavior by differential scanning calorimeter and thermogravimetric analysis respectively. The degree of crystallinity of the coatings was determined from X-ray diffraction patterns using the PFM program. It was found that increase in the mass proportion of IA based PUA in coatings, the coating becomes more rigid and crystalline. The synthesized UV curable PUA coatings showed interesting mechanical, chemical, solvent and thermal properties as compared to the conventional PUA. Further, cured coatings were also evaluated for gel content and water absorption. PMID:29491798

Effect of sulfuric acid etching of polyetheretherketone on the shear bond strength to resin cements.

PubMed

Sproesser, Oliver; Schmidlin, Patrick R; Uhrenbacher, Julia; Roos, Malgorzata; Gernet, Wolfgang; Stawarczyk, Bogna

2014-10-01

To examine the influence of etching duration on the bond strength of PEEK substrate in combination with different resin composite cements. In total, 448 PEEK specimens were fabricated, etched with sulfuric acid for 5, 15, 30, 60, 90, 120, and 300 s and then luted with two conventional resin cements (RelyX ARC and Variolink II) and one self-adhesive resin cement (Clearfil SA Cement) (n = 18/subgroup). Non-etched specimens served as the control group. Specimens were stored in distilled water for 28 days at 37°C and shear bond strengths were measured. Data were analyzed nonparametrically using Kruskal-Wallis-H (p < 0.05). Non-etched PEEK demonstrated no bond strength to resin composite cements. The optimal etching duration varied with the type of resin composite: 60 s for RelyX ARC (15.3 ± 7.2 MPa), 90 s for Variolink II (15.2 ± 7.2 MPa), and 120 s for Clearfil SA Cement (6.4 ± 5.9 MPa). Regardless of etching duration, however, the self-etching resin composite cement showed significantly lower shear bond strength values when compared to groups luted with the conventional resin composites. Although sulfuric acid seems to be suitable and effective for PEEK surface pre-treatment, further investigations are required to examine the effect of other adhesive systems and cements.

Effect of acid and laser etching on shear bond strength of conventional and resin-modified glass-ionomer cements to composite resin.

PubMed

Navimipour, Elmira Jafari; Oskoee, Siavash Savadi; Oskoee, Parnian Alizadeh; Bahari, Mahmoud; Rikhtegaran, Sahand; Ghojazadeh, Morteza

2012-03-01

Success in sandwich technique procedures can be achieved through an acceptable bond between the materials. The aim of this study was to compare the effect of 35% phosphoric acid and Er,Cr:YSGG laser on shear bond strength of conventional glass-ionomer cement (GIC) and resin-modified glass-ionomer cement (RMGIC) to composite resin in sandwich technique. Sixty-six specimens were prepared from each type of glass-ionomer cements and divided into three treatment groups as follows: without pretreatment, acid etching by 35% phosphoric acid for 15 s, and 1-W Er,Cr:YSGG laser treatment for 15 s with a 600-μm-diameter tip aligned perpendicular to the target area at a distance of 1 mm from the surface. Energy density of laser irradiation was 17.7 J/cm(2). Two specimens in each group were prepared for evaluation under a scanning electron microscope (SEM) after surface treatment and the remainder underwent bonding procedure with a bonding agent and composite resin. Then the shear bond strength was measured at a crosshead speed of 0.5 mm/min. Two-factor analysis of variance and post-hoc Tukey test showed that the cement type, surface treatment method, and the interaction of these two factors significantly affect the shear bond strength between glass-ionomer cements and composite resin (p < 0.05). Surface treatment with phosphoric acid or Er,Cr:YSGG laser increased the shear bond strength of GIC to composite resin; however, in RMGIC only laser etching resulted in significantly higher bond strength. These findings were supported by SEM results. The fracture mode was evaluated under a stereomicroscope at ×20.

Modelling of the acid-base properties of natural and synthetic adsorbent materials used for heavy metal removal from aqueous solutions.

PubMed

Pagnanelli, Francesca; Vegliò, Francesco; Toro, Luigi

2004-02-01

In this paper a comparison about kinetic behaviour, acid-base properties and copper removal capacities was carried out between two different adsorbent materials used for heavy metal removal from aqueous solutions: an aminodiacetic chelating resin as commercial product (Lewatit TP207) and a lyophilised bacterial biomass of Sphaerotilus natans. The acid-base properties of a S. natans cell suspension were well described by simplified mechanistic models without electrostatic corrections considering two kinds of weakly acidic active sites. In particular the introduction of two-peak distribution function for the proton affinity constants allows a better representation of the experimental data reproducing the site heterogeneity. A priori knowledge about resin functional groups (aminodiacetic groups) is the base for preliminary simulations of titration curve assuming a Donnan gel structure for the resin phase considered as a concentrated aqueous solution of aminodiacetic acid (ADA). Departures from experimental and simulated data can be interpreted by considering the heterogeneity of the functional groups and the effect of ionic concentration in the resin phase. Two-site continuous model describes adequately the experimental data. Moreover the values of apparent protonation constants (as adjustable parameters found by non-linear regression) are very near to the apparent constants evaluated by a Donnan model assuming the intrinsic constants in resin phase equal to the equilibrium constants in aqueous solution of ADA and considering the amphoteric nature of active sites for the evaluation of counter-ion concentration in the resin phase. Copper removal outlined the strong affinity of the active groups of the resin for this ion in solution compared to the S. natans biomass according to the complexation constants between aminodiacetic and mono-carboxylic groups and copper ions.

Anti-inflammatory and anti-angiogenic activities in vitro of eight diterpenes from Daphne genkwa based on hierarchical cluster and principal component analysis.

PubMed

Wang, Ling; Lan, Xin-Yi; Ji, Jun; Zhang, Chun-Feng; Li, Fei; Wang, Chong-Zhi; Yuan, Chun-Su

2018-06-01

Rheumatoid arthritis (RA) is one of the most prevalent chronic inflammatory and angiogenic diseases. The aim of this study was to evaluate the anti-inflammatory and anti-angiogenic activities in vitro of eight diterpenoids isolated from Daphne genkwa. LC-MS was used to identify diterpenes isolated from D. genkwa. The anti-inflammatory and anti-angiogenic activities of eight diterpenoids were evaluated on LPS-induced macrophage RAW264.7 cells and TNF-α-stimulated human umbilical vein endothelial cells (HUVECs) using hierarchical cluster analysis (HCA) and principal component analysis (PCA). The eight diterpenes isolated from D. genkwa were identified as yuanhuaphnin, isoyuanhuacine, 12-O-(2'E,4'E-decadienoyl)-4-hydroxyphorbol-13-acetyl, yuanhuagine, isoyuanhuadine, yuanhuadine, yuanhuaoate C and yuanhuacine. All the eight diterpenes significantly down-regulated the excessive secretion of TNF-α, IL-6, IL-1β and NO in LPS-induced RAW264.7 macrophages. However, only 12-O-(2'E,4'E-decadienoyl)-4-hydroxyphorbol-13-acetyl markedly reduced production of VEGF, MMP-3, ICAM and VCAM in TNF-α-stimulated HUVECs. HCA obtained 4 clusters, containing 12-O-(2'E,4'E-decadienoyl)-4-hydroxyphorbol-13-acetyl, isoyuanhuacine, isoyuanhuadine and five other compounds. PCA showed that the ranking of diterpenes sorted by efficacy from highest to lowest was 12-O-(2'E,4'E-decadienoyl)-4-hydroxyphorbol-13-acetyl, yuanhuaphnin, isoyuanhuacine, yuanhuacine, yuanhuaoate C, yuanhuagine, isoyuanhuadine, yuanhuadine. In conclusion, eight diterpenes isolated from D. genkwa showed different levels of activity in LPS-induced RAW264.7 cells and TNF-α-stimulated HUVECs. The comprehensive evaluation of activity by HCA and PCA indicated that of the eight diterpenes, 12-O-(2'E,4'E-decadienoyl)-4-hydroxyphorbol-13-acetyl was the best, and can be developed as a new drug for RA therapy.

Sand consolidation method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Young, B.M.

1965-10-05

This is a new and improved sand consolidation method wherein an in-situ curing of a resinous fluid is undertaken. This method does not require that the resinous fluids be catalyzed at the surface of the well or well bore as is the case in previous methods. This method consists of, first, pumping an acid-curable consolidating fluid into the unconsolidated sand or earth formation and, secondly, pumping an oil overflush solution containing a halogenated organic or other organic acid or delayed acid-producing chemical. A small quantity of diesel oilspacer may be used between the plastic catalyst solution. The overflush functions tomore » remove permeability, and its acid or acid producing component promotes subsequent hardening of the remaining film of consolidating fluid. Trichloroacetic acid and benzotrichloride are satisfactory to add to the overflush solution for curing the resins. (17 claims)« less

Unveiling the mode of action of antibacterial labdane diterpenes from Alpinia nigra (Gaertn.) B. L. Burtt seeds.

PubMed

Ghosh, Sudipta; Indukuri, Kiran; Bondalapati, Somasekhar; Saikia, Anil K; Rangan, Latha

2013-08-01

The labdane diterpene, (E)-labda-8(17), 12-diene-15, 16-dial (compound A) and its epoxide analogue, (E)-8β, 17-Epoxylabd-12-ene-15, 16-dial (compound B) were isolated from the seeds of Alpinia nigra for the first time. The antibacterial activities of both compounds were evaluated against three Gram-positive and four Gram-negative bacteria, and flow cytometric analysis revealed that these compounds caused significant damage to the bacterial cell membranes. Further, field emission scanning electron microscope imaging and cell leakage analysis confirmed that the labdane diterpenes were responsible for bacterial cell membrane damage and disintegration. Our findings provide new insight into the broad-spectrum effects of two natural labdane diterpenes that may be useful in the future development of herbal antibiotic products. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Determination of airborne, volatile amines from polyurethane foams by sorption onto a high-capacity cation-exchange resin based on poly(succinic acid).

PubMed

Seeber, G; Buchmeiser, M R; Bonn, G K; Bertsch, T

1998-06-05

A high-capacity carboxylic acid-functionalized resin prepared by ring-opening metathesis polymerization based on cross-linked endo,endo-poly(norborn-2-ene-5,6-dicarboxylic acid) was used for the sampling of volatile, airborne amines from polyurethane (PU) foams. Six tertiary amines which represent commonly used promotors for the formation of PUs from diisocyanates and polyols, namely pentamethyldiethylenetriamine, diazabicyclooctane, N-methylmorpholine, N-ethylmorphine, 1,4-dimethylpiperazine and N,N-dimethylethanolamine, were sorbed onto the new resin. The sorption behavior of the new material was investigated in terms of loading capacities, the influence of concentration, flow-rate as well as of the amount of resin. Breakthrough curves were recorded from each single component as well as of mixtures thereof. Finally, the resin was used for the sampling of amines evaporating from PU foams applied in buildings. Further information about time dependent concentration profiles were obtained using a combination of GC-MS and Fourier transform IR spectroscopy.

Application of 2-chlorotrityl resin in solid phase synthesis of (Leu15)-gastrin I and unsulfated cholecystokinin octapeptide. Selective O-deprotection of tyrosine.

PubMed

Barlos, K; Gatos, D; Kapolos, S; Poulos, C; Schäfer, W; Yao, W Q

1991-12-01

The carboxyl terminal dipeptide amide, Fmoc-Asp-Phe-NH2, of gastrin and cholecystokinin (CCK) has been attached in high yield through its free side chain carboxyl group to the acid labile 2-chlorotrityl resin. The obtained peptide resin ester has been applied in the solid phase synthesis of partially protected (Leu15)-gastrin I utilising Fmoc-amino acids. Quantitative cleavage of this peptide from resin, with the t-butyl type side chain protection intact is achieved using mixtures of acetic acid/trifluoroethanol/dichloromethane. Under the same conditions complete detritylation of the tyrosine phenoxy function occurs simultaneously. Thus, the solid-phase synthesis of peptides selectively deprotected at the side chain of tyrosine is rendered possible by the use of 2-chlorotrityl resin and Fmoc-Tyr(Trt)-OH. The efficiency of this approach has been proved by the subsequent high-yield synthesis of three model peptides and the CCK-octapeptide.

Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

PubMed

Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

2011-01-01

We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

Humic Acid Isolations from Lignite by Ion Exchange Method

NASA Astrophysics Data System (ADS)

Kurniati, E.; Muljani, S.; Virgani, D. G.; Neno, B. P.

2018-01-01

The humic liquid is produced from lignite extraction using alkali solution. Conventional humic acid is obtained by acidifying a humic solution using HCl. The purpose of this research is the formation of solid humic acid from lignite by ion exchange method using cation resin. The results showed that the addition of cation resin was able to reduce the pH from 14 to pH 2 as well as the addition of acid (HCl), indicating the exchange of Na + ions with H + ions. The reduction of pH in the humic solution is influenced by the concentration of sodium ions in the humic solution, the weight of the cation resin, and the ion exchange time. The IR spectra results are in good agreement for humic acid from lignite characterization.

Analysis of diterpenoic compounds in natural resins applied as binders in museum objects by capillary electrophoresis.

PubMed

Findeisen, Anna; Kolivoska, Viliam; Kaml, Isabella; Baatz, Wolfgang; Kenndler, Ernst

2007-07-20

The exudates of conifers consist mainly of diterpenoic acids of the abietane and pimarane type (abietic, neoabietic, dehydroabietic, palustric, pimaric, isopimaric, levopimaric and sandaracopimaric acid) and larixol acetate. These natural resins were used as adhesives, coatings, varnishes or plasticizers in artistic and historic works since ancient times. For the purpose of conservation and restoration and for art historic examination of such museum objects the identification of the binding media used is undoubtedly of paramount importance. In the present paper, the characterization of these resins based on the pattern of their diterpenoid constituents is carried out by capillary electrophoresis. For separation a background electrolyte which has been initially introduced for the analysis of chlorinated and natural resin acids in waste water was modified and the experimental conditions were adjusted in terms of resolution and analysis time. Separation was carried out in borate buffer at pH 9.25 (ionic strength 20 mmol L(-1)) with methyl-beta-cyclodextrin and sulfobutylether-beta-cyclodextrin as additives to increase selectivity and enhance the solubility of the analytes. With this electrophoretic system the resin acids of interest and larixol acetate--all as anionic cyclodextrin complexes--were separated within 5 min and detected at 200, 250 and 270 nm with a diode array detector. The electrophoretic patterns served for the characterisation of the relevant diterpenoic resins, balsams and copals. Sample pre-treatment was limited to sonication in methanol at 55 degrees C for 30 min. This enables the identification of the resins in mixtures with other binders like plant gums, animal glues or drying oils, even when these media are present in excess. Colophony was identified as resinous constituent of a modelling mass for gilded frames originating from the 19th century.

Antiviral agents of plant origin. III. Scopadulin, a novel tetracyclic diterpene from Scoparia dulcis L.

PubMed

Hayashi, T; Kawasaki, M; Miwa, Y; Taga, T; Morita, N

1990-04-01

The structure and stereochemistry of scopadulin, a novel aphidicolane-type diterpene isolated from Scoparia dulcis L. have been established from spectral data and single-crystal X-ray analysis of its acetone solvate.

Discovery and functional characterization of two diterpene synthases for sclareol biosynthesis in Salvia sclarea (L.) and their relevance for perfume manufacture

PubMed Central

2012-01-01

Background Sclareol is a diterpene natural product of high value for the fragrance industry. Its labdane carbon skeleton and its two hydroxyl groups also make it a valued starting material for semisynthesis of numerous commercial substances, including production of Ambrox® and related ambergris substitutes used in the formulation of high end perfumes. Most of the commercially-produced sclareol is derived from cultivated clary sage (Salvia sclarea) and extraction of the plant material. In clary sage, sclareol mainly accumulates in essential oil-producing trichomes that densely cover flower calices. Manool also is a minor diterpene of this species and the main diterpene of related Salvia species. Results Based on previous general knowledge of diterpene biosynthesis in angiosperms, and based on mining of our recently published transcriptome database obtained by deep 454-sequencing of cDNA from clary sage calices, we cloned and functionally characterized two new diterpene synthase (diTPS) enzymes for the complete biosynthesis of sclareol in clary sage. A class II diTPS (SsLPPS) produced labda-13-en-8-ol diphosphate as major product from geranylgeranyl diphosphate (GGPP) with some minor quantities of its non-hydroxylated analogue, (9 S, 10 S)-copalyl diphosphate. A class I diTPS (SsSS) then transformed these intermediates into sclareol and manool, respectively. The production of sclareol was reconstructed in vitro by combining the two recombinant diTPS enzymes with the GGPP starting substrate and in vivo by co-expression of the two proteins in yeast (Saccharomyces cerevisiae). Tobacco-based transient expression assays of green fluorescent protein-fusion constructs revealed that both enzymes possess an N-terminal signal sequence that actively targets SsLPPS and SsSS to the chloroplast, a major site of GGPP and diterpene production in plants. Conclusions SsLPPS and SsSS are two monofunctional diTPSs which, together, produce the diterpenoid specialized metabolite sclareol in a two-step process. They represent two of the first characterized hydroxylating diTPSs in angiosperms and generate the dihydroxylated labdane sclareol without requirement for additional enzymatic oxidation by activities such as cytochrome P450 monoxygenases. Yeast-based production of sclareol by co-expresssion of SsLPPS and SsSS was efficient enough to warrant the development and use of such technology for the biotechnological production of scareol and other oxygenated diterpenes. PMID:22834731

Discovery and functional characterization of two diterpene synthases for sclareol biosynthesis in Salvia sclarea (L.) and their relevance for perfume manufacture.

PubMed

Caniard, Anne; Zerbe, Philipp; Legrand, Sylvain; Cohade, Allison; Valot, Nadine; Magnard, Jean-Louis; Bohlmann, Jörg; Legendre, Laurent

2012-07-26

Sclareol is a diterpene natural product of high value for the fragrance industry. Its labdane carbon skeleton and its two hydroxyl groups also make it a valued starting material for semisynthesis of numerous commercial substances, including production of Ambrox® and related ambergris substitutes used in the formulation of high end perfumes. Most of the commercially-produced sclareol is derived from cultivated clary sage (Salvia sclarea) and extraction of the plant material. In clary sage, sclareol mainly accumulates in essential oil-producing trichomes that densely cover flower calices. Manool also is a minor diterpene of this species and the main diterpene of related Salvia species. Based on previous general knowledge of diterpene biosynthesis in angiosperms, and based on mining of our recently published transcriptome database obtained by deep 454-sequencing of cDNA from clary sage calices, we cloned and functionally characterized two new diterpene synthase (diTPS) enzymes for the complete biosynthesis of sclareol in clary sage. A class II diTPS (SsLPPS) produced labda-13-en-8-ol diphosphate as major product from geranylgeranyl diphosphate (GGPP) with some minor quantities of its non-hydroxylated analogue, (9 S, 10 S)-copalyl diphosphate. A class I diTPS (SsSS) then transformed these intermediates into sclareol and manool, respectively. The production of sclareol was reconstructed in vitro by combining the two recombinant diTPS enzymes with the GGPP starting substrate and in vivo by co-expression of the two proteins in yeast (Saccharomyces cerevisiae). Tobacco-based transient expression assays of green fluorescent protein-fusion constructs revealed that both enzymes possess an N-terminal signal sequence that actively targets SsLPPS and SsSS to the chloroplast, a major site of GGPP and diterpene production in plants. SsLPPS and SsSS are two monofunctional diTPSs which, together, produce the diterpenoid specialized metabolite sclareol in a two-step process. They represent two of the first characterized hydroxylating diTPSs in angiosperms and generate the dihydroxylated labdane sclareol without requirement for additional enzymatic oxidation by activities such as cytochrome P450 monoxygenases. Yeast-based production of sclareol by co-expresssion of SsLPPS and SsSS was efficient enough to warrant the development and use of such technology for the biotechnological production of scareol and other oxygenated diterpenes.

Chemical Characterization of Beer Aging Products Derived from Hard Resin Components in Hops (Humulus lupulus L.).

PubMed

Taniguchi, Yoshimasa; Yamada, Makiko; Taniguchi, Harumi; Matsukura, Yasuko; Shindo, Kazutoshi

2015-11-25

The bitter taste of beer originates from resins in hops (Humulus lupulus L.), which are classified into two subtypes (soft and hard). Whereas the nature and reactivity of soft-resin-derived compounds, such as α-, β-, and iso-α-acids, are well studied, there is only a little information on the compounds in hard resin. For this work, hard resin was prepared from stored hops and investigated for its compositional changes in an experimental model of beer aging. The hard resin contained a series of α-acid oxides. Among them, 4'-hydroxyallohumulinones were unstable under beer storage conditions, and their transformation induced primary compositional changes of the hard resin during beer aging. The chemical structures of the products, including novel polycyclic compounds scorpiohumulinols A and B and dicyclohumulinols A and B, were determined by HRMS and NMR analyses. These compounds were proposed to be produced via proton-catalyzed cyclization reactions of 4'-hydroxyallohumulinones. Furthermore, they were more stable than their precursor 4'-hydroxyallohumulinones during prolonged storage periods.

Automated Desalting Apparatus

NASA Technical Reports Server (NTRS)

Spencer, Maegan K.; Liu, De-Ling; Kanik, Isik; Beegle, Luther

2010-01-01

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

Synthesis and characterization of an N-(2-hydroxyethyl)-ethylenediaminetriacetic acid resin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lai, Yuet Fan

1977-10-01

A chelating ion-exchange resin with N-(2-hydroxyethyl)ethylene-diaminetriacetic acid (HEDTA) used as the ligand chemically bonded to XAD-4 by an ester linkage, HEDTA-4, was synthesized. It is stable under normal experimental conditions with the liquid chromatograph. The structure of the resin was confirmed by an infrared spectrum, and by potentiometric titrations. The capacity of the resin was also obtained by potentiometric titration and by a nitrogen analysis. The resin was used to pack a column of 5 mm internal diameter and 5 cm long. The effect of pH on the retention of different metal ions on the resin was studied. It wasmore » found that the resin was most selective for chromium(III), copper(II), lead(II), mercury(II), uranium(VI), zirconium(IV) and zinc(II) at a pH of less than 3. Furthermore, the resin proves to be functioning with a chelating mechanism rather than ion-exchange, and it can concentrate trace metal ions in the presence of a large excess of calcium and magnesium. This makes the resin potentially useful for purifying and analyzing drinking water.« less

Regeneration of strong-base anion-exchange resins by sequential chemical displacement

DOEpatents

Brown, Gilbert M.; Gu, Baohua; Moyer, Bruce A.; Bonnesen, Peter V.

2002-01-01

A method for regenerating strong-base anion exchange resins utilizing a sequential chemical displacement technique with new regenerant formulation. The new first regenerant solution is composed of a mixture of ferric chloride, a water-miscible organic solvent, hydrochloric acid, and water in which tetrachloroferrate anion is formed and used to displace the target anions on the resin. The second regenerant is composed of a dilute hydrochloric acid and is used to decompose tetrachloroferrate and elute ferric ions, thereby regenerating the resin. Alternative chemical displacement methods include: (1) displacement of target anions with fluoroborate followed by nitrate or salicylate and (2) displacement of target anions with salicylate followed by dilute hydrochloric acid. The methodology offers an improved regeneration efficiency, recovery, and waste minimization over the conventional displacement technique using sodium chloride (or a brine) or alkali metal hydroxide.

SEPARATION OF BARIUM VALUES FROM URANYL NITRATE SOLUTIONS

DOEpatents

Tompkins, E.R.

1959-02-24

The separation of radioactive barium values from a uranyl nitrate solution of neutron-irradiated uranium is described. The 10 to 20% uranyl nitrate solution is passed through a flrst column of a cation exchange resin under conditions favoring the adsorption of barium and certain other cations. The loaded resin is first washed with dilute sulfuric acid to remove a portion of the other cations, and then wash with a citric acid solution at pH of 5 to 7 to recover the barium along with a lesser amount of the other cations. The PH of the resulting eluate is adjusted to about 2.3 to 3.5 and diluted prior to passing through a smaller second column of exchange resin. The loaded resin is first washed with a citric acid solution at a pH of 3 to elute undesired cations and then with citric acid solution at a pH of 6 to eluts the barium, which is substantially free of undesired cations.

The cholesterol-raising factor from coffee beans.

PubMed Central

Urgert, R; Katan, M B

1996-01-01

Coffee beans and some types of coffee brew-not the regular types of coffee prepared with a paper filter or with soluble coffee granules-contain the diterpenes cafestol and kahweol. Cafestol and kahweol raise the serum concentration of cholesterol and triglycerides in humans, and they also appear mildly to affect the integrity of liver cells. Both effects are transient after withdrawal of the diterpenes, and it is as yet unsure whether these effects are associated. Patients at increased risk of heart disease who drink large amounts of coffee should be advised to select brews low in diterpenes. PMID:9135590

Phytotoxic clerodane diterpenes from Salvia miniata Fernald (Lamiaceae).

PubMed

Bisio, Angela; Damonte, Gianluca; Fraternale, Daniele; Giacomelli, Emanuela; Salis, Annalisa; Romussi, Giovanni; Cafaggi, Sergio; Ricci, Donata; De Tommasi, Nunziatina

2011-02-01

Our ongoing research to identify natural growth inhibitors with diterpene and triterpene skeletons exuding from the surface of the aerial parts of Salvia species led us to study Salvia miniata Fernald. Ten clerodane diterpenoids were found, along with three known diterpenes. Most of the isolated compounds from S. miniata inhibited the germination of Papaver rhoeas L. and Avena sativa L. in Petri dish experiments. Parallel results have been obtained in experiments carried out to evaluate the subsequent growth of the seedlings of the target species in the presence of the tested compounds. Copyright © 2010 Elsevier Ltd. All rights reserved.

Chelating resin immobilizing carboxymethylated polyethyleneimine for selective solid-phase extraction of trace elements: Effect of the molecular weight of polyethyleneimine and its carboxymethylation rate.

PubMed

Kagaya, Shigehiro; Kajiwara, Takehiro; Gemmei-Ide, Makoto; Kamichatani, Waka; Inoue, Yoshinori

2016-01-15

The effect of the molecular weight of polyethyleneimine (PEI), defined as a compound having two or more ethyleneamine units, and of its carboxymethylation rate (CM/N), represented by the ratio of ion-exchange capacity to the amount of N on the resin, on the selective solid-phase extraction ability of the chelating resin immobilizing carboxymethylated (CM) PEI was investigated. The chelating resins (24 types) were prepared by immobilization of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, PEI300 (MW=ca. 300), and PEI600 (MW=ca. 600) on methacrylate resins, followed by carboxymethylation with various amounts of sodium monochloroacetate. When resins with approximately the same CM/N ratio (0.242-0.271) were used, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, Zn, and alkaline earth elements increased with increasing the molecular weight of PEIs under acidic and weakly acidic conditions; however, the extraction behavior of Mo and V was only slightly affected. This was probably due to the increase in N content of the resin, resulting in an increase in carboxylic acid groups; the difference in the molecular weight of PEIs immobilized on the resin exerts an insignificant influence on the selective extraction ability. The CM/N ratio considerably affected the extraction behavior for various elements. Under acidic and neutral conditions, the recovery of Cd, Co, Cu, Fe, Ni, Pb, Ti, and Zn increased with increasing CM/N values. However, under these conditions, the recovery of alkaline earth elements was considerably low when a resin with low CM/N ratio was used. This is presumably attributed to the different stability constants of the complexes of these elements with aminocarboxylic acids and amines, and to the electrostatic repulsion between the elements and the protonated amino groups in the CM-PEI. The recovery of Mo and V decreased or varied with increasing CM/N values, suggesting that the extraction of these elements occurred mainly by the anion-exchange reaction. For the separation and preconcentration of trace elements in samples containing large amounts of alkali and alkaline earth elements, the CM-PEI600 resin with CM/N=0.131 (Cu(II) extraction capacity, 0.37mmol g(-)(1)) was found to be the most suitable because it scarcely extracts alkali and alkaline earth elements under acidic and neutral conditions. This resin proved to be convenient for separating and preconcentrating Cd, Co, Cu, Fe, Mn, Mo, Ni, Pb, V, and Zn in the certified reference materials (EnviroMAT EU-L-1 wastewater and ES-L-1 ground water) and commercially available table salt. Copyright © 2015 Elsevier B.V. All rights reserved.

Bonding efficacy of new self-etching, self-adhesive dual-curing resin cements to dental enamel.

PubMed

Benetti, Paula; Fernandes, Virgílio Vilas; Torres, Carlos Rocha; Pagani, Clovis

2011-06-01

This study evaluated the efficacy of the union between two new self-etching self-adhesive resin cements and enamel using the microtensile bond strength test. Buccal enamel of 80 bovine teeth was submitted to finishing and polishing with metallographic paper to a refinement of #600, in order to obtain a 5-mm2 flat area. Blocks (2 x 4 x 4 mm) of laboratory composite resin were cemented to enamel according to different protocols: (1) untreated enamel + RelyX Unicem cement (RX group); (2) untreated enamel + Bifix SE cement (BF group); (3) enamel acid etching and application of resin adhesive Single Bond + RelyX Unicem (RXA group); (4) enamel acid etching and application of resin adhesive Solobond M + Bifix SE (BFA group). After 7 days of storage in distillated water at 37°C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm2 (n = 120). Specimens were submitted to the microtensile bond strength test at a crosshead speed of 0.5 mm/min. The results (in MPa) were analyzed statistically by ANOVA and Tukey's test. Enamel pre-treatment with phosphoric acid and resin adhesive (27.9 and 30.3 for RXA and BFA groups) significantly improved (p ≤ 0.05) the adhesion of both cements to enamel compared to the union achieved with as-polished enamel (9.9 and 6.0 for RX and BF). Enamel pre-treatment with acid etching and the application of resin adhesive significantly improved the bond efficacy of both luting agents compared to the union achieved with as-polished enamel.

Ion-exclusion chromatography with conductimetric detection of aliphatic carboxylic acids on a weakly acidic cation-exchange resin by elution with benzoic acid-beta-cyclodextrin.

PubMed

Tanaka, Kazuhiko; Mori, Masanobu; Xu, Qun; Helaleh, Murad I H; Ikedo, Mikaru; Taoda, Hiroshi; Hu, Wenzhi; Hasebe, Kiyoshi; Fritz, James S; Haddad, Paul R

2003-05-16

In this study, an aqueous solution consisting of benzoic acid with low background conductivity and beta-cyclodextrin (beta-CD) of hydrophilic nature and the inclusion effect to benzoic acid were used as eluent for the ion-exclusion chromatographic separation of aliphatic carboxylic acids with different pKa values and hydrophobicity on a polymethacrylate-based weakly acidic cation-exchange resin in the H+ form. With increasing concentration of beta-cyclodextrin in the eluent, the retention times of the carboxylic acids decreased due to the increased hydrophilicity of the polymethacrylate-based cation-exchange resin surface from the adsorption of OH groups of beta-cyclodextrin. Moreover, the eluent background conductivity decreased with increasing concentration of beta-cyclodextrin in 1 mM benzoic acid, which could result in higher sensitivity for conductimetric detection. The ion-exclusion chromatographic separation of carboxylic acids with high resolution and sensitivity was accomplished successfully by elution with a 1 mM benzoic acid-10 mM cyclodextrin solution without chemical suppression.

Synthesis and properties of hydroxy acrylic resin with high solid content

NASA Astrophysics Data System (ADS)

Yu, Zhen; Hu, Mingguang; Cui, Han; Xiao, Jijun

2017-10-01

Manufacturers of automotive repair finishes are tending to reduce more and more the level of volatile organic compounds in their paints in order to comply with increasingly strict environmental legislation. A high solid hydroxy acrylic resin was synthesised using CARDURA E10 and a type of hydroxyacrylic acid resin, its' acid value, hydroxylvalue, viscosity, structure, morphology was measured and film-forming properties after curing were characterised. The results show that the addition of CARDURA E10 in the copolymer composition significantly reduced the viscosity of the polymer system, improved the solid content of the resin and the physical properties of the coating. The hydroxyl acrylate resin with solid content of 90% and excellent comprehensive performance were successfully prepared by controlling the initiator dosage, polymerization temperature and monomer ratio.

Method for the purification of bis (2-ethyl-hexyl)phosphoric acid

DOEpatents

Schulz, W.W.

1974-02-19

Foreign products including the neutral organophosphorous compounds and the iron salts normally present in commercial bis(2ethyl-hexyl) phosphoric acid(HDEHP), and the radiolytic degradation products of HDEHP on exposure of HDEHP to beta and gamma irradiation are removed from HDEHP containing one or more of such products by contacting the said foreign product containing HDEHP with a macroreticular anion exchange resin in base form whereby the DEHP- ion of HDEHP exchanges with the anion of the resin and is thus adsorbed on the resin and the said foreign products are not adsorbed and will pass through a bed of particles of the resin. The adsorbed DEHP- ion is then eluted from the resin and acidified to form and recover the purified HDEHP. (auth)

SURFACE DEGRADATION OF COMPOSITE RESINS BY ACIDIC MEDICINES AND pH-CYCLING

PubMed Central

Valinoti, Ana Carolina; Neves, Beatriz Gonçalves; da Silva, Eduardo Moreira; Maia, Lucianne Cople

2008-01-01

This study evaluated the effects of acidic medicines (Dimetapp® and Claritin®), under pH-cycling conditions, on the surface degradation of four composite resins (microhybrid: TPH, Concept, Opallis and Nanofilled: Supreme). Thirty disc-shaped specimens (Ø = 5.0 mm / thickness = 2.0 mm) of each composite were randomly assigned to 3 groups (n = 10): a control and two experimental groups, according to the acidic medicines evaluated. The specimens were finished and polished with aluminum oxide discs, and the surface roughness was measured by using a profilometer. After the specimens were submitted to a pH-cycling regimen and immersion in acidic medicines for 12 days, the surface roughness was measured again. Two specimens for each material and group were analyzed by scanning electron microscopy (SEM) before and after pH-cycling. Data were analyzed by the Student's-t test, ANOVA, Duncan's multiple range test and paired t-test (α=0.05). Significant increase in roughness was found only for TPH in the control group and TPH and Supreme immersed in Claritin® (p<0.05). SEM analyses showed that the 4 composite resins underwent erosion and surface degradation after being subjected to the experimental conditions. In conclusion, although the roughness was slightly affected, the pH-cycling and acidic medicines caused surface degradation of the composite resins evaluated. Titratable acidity seemed to play a more crucial role on surface degradation of composite resins than pH. PMID:19089257

ELUTION OF URANIUM VALUES FROM ION EXCHANGE RESINS

DOEpatents

Kennedy, R.H.

1959-11-24

A process is described for eluting complex uranium ions absorbed on ion exchange resins. The resin is subjected to the action of an aqueous eluting solution contuining sulfuric acid and an alkali metal, ammonium, or magnesium chloride or nitrate, the elution being carried out until the desired amount of the uranium is removed from the resin.

Preventive effect of fluoridated orthodontic resins subjected to high cariogenic challenges.

PubMed

Passalini, Paula; Fidalgo, Tatiana Kelly da Silva; Caldeira, Erika Machado; Gleiser, Rogerio; Nojima, Matilde da Cunha Gonçalves; Maia, Lucianne Cople

2010-01-01

The aim of the present study was to evaluate the in vitro caries preventive effect of fluoridated orthodontic resins under pH cycling with two types of acid demineralizing saliva. Brackets were bonded to 60 bovine incisors, using either Transbond Plus Color Change (n=30) or Orthodontic Fill Magic (n=30) orthodontic resins. Each group of resin was divided into 3 subgroups (n=10): immersion in remineralizing artificial saliva for 14 days, pH cycling with high cariogenic challenge in acid saliva with pH 5.5, and acid saliva with pH 4.5. After 14 days of pH cycling, the caries preventive effect on the development of white spot lesion was evaluated considering the presence of inhibition zones to white spot lesions using two scores: 0= absence and 1= presence. Kruskal Wallis and Mann-Whitney tests (a=0.05) were used. Formation of white spot lesions was observed only under pH cycling using acid saliva with pH 4.5; with Transbond Plus Color Change being significantly more effective (p<0.05) in preventing the appearance of white spot lesions effect than Orthodontic Fill Magic. The acidity of the demineralizing solution influenced the formation of white spot lesions around orthodontic brackets under highly cariogenic conditions. Transbond Plus Color Change resin presented higher caries preventive effect than Orthodontic Fill Magic.

QSAR studies of macrocyclic diterpenes with P-glycoprotein inhibitory activity.

PubMed

Sousa, Inês J; Ferreira, Maria-José U; Molnár, Joseph; Fernandes, Miguel X

2013-02-14

Multidrug resistance (MDR) represents a major limitation for cancer chemotherapy. There are several mechanisms of MDR but the most important is associated with P-glycoprotein (P-gp) overexpression. The development of modulators of P-gp that are able to re-establish drug sensitivity of resistant cells has been considered a promising approach for overcoming MDR. Macrocyclic lathyrane and jatrophane-type diterpenes from Euphorbia species were found to be strong MDR reversing agents. In this study we applied quantitative structure-activity relationship (QSAR) methodology in order to identify the most relevant molecular features of macrocyclic diterpenes with P-gp inhibitory activity and to determine which structural modifications can be performed to improve their activity. Using experimental biological data at two concentrations (4 and 40 μg/ml), we developed a QSAR model for a set of 51 bioactive diterpenic compounds which includes lathyrane and jatrophane-type diterpenes and another model just for jatrophanes. The cross-validation correlation values for all diterpenes QSAR models developed for biological activities at compound concentrations of 4 and 40 μg/ml were 0.758 and 0.729, respectively. Regarding the prediction ability, we get R²(pred) values of 0.765 and 0.534 for biological activities at compound concentrations of 4 and 40 μg/ml, respectively. Applying the cross-validation test to jatrophanes QSAR models, we obtained 0.680 and 0.787 for biological activities at compound concentrations of 4 and 40 μg/ml concentrations, respectively. For the same concentrations, the obtained R²(pred) values for jatrophanes models were 0.541 and 0.534, respectively. The obtained models were statistically valid and showed high prediction ability. Copyright © 2012 Elsevier B.V. All rights reserved.

Ion exchange treatment of rinse water generated in the galvanizing process.

PubMed

Marañón, Elena; Fernández, Yolanda; Castrillón, Leonor

2005-01-01

A study was conducted of the viability of using the cationic exchange resins Amberlite IR-120 and Lewatit SP-112 to treat rinse water generated in the galvanizing process as well as acidic wastewater containing zinc (Zn) and iron (Fe). Solutions containing either 100 mg/L of Zn at pH 5.6 (rinse water) or Fe and Zn at concentrations of 320 and 200 mg/L at pH 1.5 (acidic water), respectively, were percolated through packed beds until the resins were exhausted. Breakthrough capacities obtained ranged between 1.1 and 1.5 meq metal/mL resin. The elution of metal and the regeneration of resins were performed with hydrochloric acid. The influence of the flowrate used during the loading stage was also studied, with 0.5 bed volumes/min (3.2 cm/min) found to be the optimum flowrate.

Rhizovarins A-F, Indole-Diterpenes from the Mangrove-Derived Endophytic Fungus Mucor irregularis QEN-189.

PubMed

Gao, Shu-Shan; Li, Xiao-Ming; Williams, Katherine; Proksch, Peter; Ji, Nai-Yun; Wang, Bin-Gui

2016-08-26

Genome mining of the fungus Mucor irregularis (formerly known as Rhizomucor variabilis) revealed the presence of various gene clusters for secondary metabolite biosynthesis, including several terpene-based clusters. Investigation into the chemical diversity of M. irregularis QEN-189, an endophytic fungus isolated from the fresh inner tissue of the marine mangrove plant Rhizophora stylosa, resulted in the discovery of 20 structurally diverse indole-diterpenes including six new compounds, namely, rhizovarins A-F (1-6). Among them, compounds 1-3 represent the most complex members of the reported indole-diterpenes. The presence of an unusual acetal linked to a hemiketal (1) or a ketal (2 and 3) in an unprecedented 4,6,6,8,5,6,6,6,6-fused indole-diterpene ring system makes them chemically unique. Their structures and absolute configurations were elucidated by spectroscopic analysis, modified Mosher's method, and chemical calculations. Each of the isolated compounds was evaluated for antitumor activity against HL-60 and A-549 cell lines.

A Novel Diterpene Glycoside with Nine Glucose Units from Stevia rebaudiana Bertoni

PubMed Central

Prakash, Indra; Ma, Gil; Bunders, Cynthia; Charan, Romila D.; Ramirez, Catherine; Devkota, Krishna P.; Snyder, Tara M.

2017-01-01

Following our interest in new diterpene glycosides with better taste profiles than that of Rebaudioside M, we have recently isolated and characterized Rebaudioside IX—a novel steviol glycoside—from a commercially-supplied extract of Stevia rebaudiana Bertoni. This molecule contains a hexasaccharide group attached at C-13 of the central diterpene core, and contains three additional glucose units when compared with Rebaudioside M. Here we report the complete structure elucidation—based on extensive Nuclear Magnetic Resonance (NMR) analysis (1H, 13C, Correlation Spectroscopy (COSY), Heteronuclear Single Quantum Coherence-Distortionless Enhancement Polarization Transfer (HSQC-DEPT), Heteronuclear Multiple Bond Correlation (HMBC), 1D Total Correlation Spectroscopy (TOCSY), Nuclear Overhauser Effect Spectroscopy (NOESY)) and mass spectral data—of this novel diterpene glycoside with nine sugar moieties and containing a relatively rare 1→6 α-linked glycoside. A steviol glycoside bearing nine glucose units is unprecedented in the literature, and could have an impact on the natural sweetener catalog. PMID:28146121

A Novel Diterpene Glycoside with Nine Glucose Units from Stevia rebaudiana Bertoni.

PubMed

Prakash, Indra; Ma, Gil; Bunders, Cynthia; Charan, Romila D; Ramirez, Catherine; Devkota, Krishna P; Snyder, Tara M

2017-01-31

Following our interest in new diterpene glycosides with better taste profiles than that of Rebaudioside M, we have recently isolated and characterized Rebaudioside IX-a novel steviol glycoside-from a commercially-supplied extract of Stevia rebaudiana Bertoni. This molecule contains a hexasaccharide group attached at C-13 of the central diterpene core, and contains three additional glucose units when compared with Rebaudioside M. Here we report the complete structure elucidation-based on extensive Nuclear Magnetic Resonance (NMR) analysis (1H, 13C, Correlation Spectroscopy (COSY), Heteronuclear Single Quantum Coherence-Distortionless Enhancement Polarization Transfer (HSQC-DEPT), Heteronuclear Multiple Bond Correlation (HMBC), 1D Total Correlation Spectroscopy (TOCSY), Nuclear Overhauser Effect Spectroscopy (NOESY)) and mass spectral data-of this novel diterpene glycoside with nine sugar moieties and containing a relatively rare 16 α-linked glycoside. A steviol glycoside bearing nine glucose units is unprecedented in the literature, and could have an impact on the natural sweetener catalog.

Effect of Silanization on Microtensile Bond Strength of Different Resin Cements to a Lithium Disilicate Glass Ceramic.

PubMed

Gré, Cristina Parise; de Ré Silveira, Renan C; Shibata, Shizuma; Lago, Carlo Tr; Vieira, Luiz Cc

2016-02-01

This study evaluated the influence of a silane-coupling agent on the bond strength of a self-adhesive cement and a conventional resin cement to a lithium disilicate glass ceramic. A total of eight ceramic blocks were fabricated and divided into four groups (n = 2). In groups 1 and 3, ceramic surfaces were etched with hydrofluoric acid 10% for 20 seconds, rinsed for 30 seconds, and air-dried. One layer of a silane agent was applied onto all ceramic specimens and air-dried for 30 seconds. In groups 2 and 4, ceramic surfaces were etched with hydrofluoric acid, rinsed, and air-dried without application of the silane-coupling agent. The ceramic blocks were bonded to a block of composite with a self-adhesive resin cement or with a conventional resin cement, according to the manufacturer's instructions. After 24 hours in distilled water at 37°C, the specimens were sectioned perpendicular to the bonding interface area to obtain beams with a bonding area of 0.8 mm(2) and submitted to a microtensile bond strength test at a crosshead speed of 0.5 mm/min. Data were statistically analyzed with one-way analysis of variance and the Games-Howell post hoc test (p = 0.05). Fractured specimens were examined under optical microscopy at 40x magnification. Silanization resulted in higher microtensile bond strength compared to groups without silane. No significant differences were found between the conventional resin cement and the self-adhesive resin cement with silane agent (p = 0.983), and without silane agent (p = 0.877). Silanization appears to be crucial for resin bonding to a lithium disilicate-based ceramic, regardless of the resin cement used. The self-adhesive resin cement performed as well as the conventional resin cement. Applying one layer of a silane-coupling agent after etching the ceramic surface with hydrofluoric acid 10% enhanced the bond strength between resin cements and a glass ceramic.

Improving the sensory and oxidative stability of cooked and chill-stored lamb using dietary rosemary diterpenes.

PubMed

Serrano, Rafael; Ortuño, Jordi; Bañón, Sancho

2014-09-01

Two dietary rosemary extracts (DREs) containing diterpenes (carnosic acid and carnosol at 1:1 and 2:1 w:w) were tested in fattening lambs to stabilize the sensory quality of cooked and chill-stored patties. A total of 63 lambs were fed freely for 80 ± 5 d with a basal diet supplemented or not with DRE. Minced leg meat from each lamb was used to make patty batches. The patties were cooked at 72 ºC for 2 min, aerobically packed, kept at 2 ºC for up to 4 d and then reheated. Sensory traits (color, odor, flavor, and texture), CIELab color, and lipid oxidation (assessed as TBARS) were determined. In a first experiment, the lamb diet was supplemented with 600 mg of 1:1-DRE or 2:1-DRE kg(-1) feed. The 1:1-DRE diet delayed discoloration, flavor deterioration, and rancidity, while the 2:1-DRE diet was ineffective in this respect. In a second experiment, 4 supplementation levels of 1:1-DRE (0, 200, 400, and 600 mg kg(-1) feed) were compared. Flavor deterioration was delayed when the lamb diet was supplemented with at least 400 mg 1:1-DRE kg(-1) feed. The effects of the diet on the odor, flavor, and color were corroborated by differences in TBARS and CIELab. The results obtained suggest that rosemary diterpenes and/or their active secondary compounds deposited in muscle can act as endogenous antioxidants in cooked lamb. The carnosol intake seems crucial in the antioxidant actions achieved through DRE. The use of rosemary antioxidants in animal feeding would allow meat-based dishes to be preserved longer without adding preservatives. © 2014 Institute of Food Technologists®

Study on the removal of iron impurities in methanesulfonic acid tin plating bath

NASA Astrophysics Data System (ADS)

Hou-li, LIU; Jian-Jun, CHEN; Hong-Liang, PAN

2018-03-01

This thesis investigated the the influence of sodium sulfite as reducing agent on the recovery rate of tin ion. The approach is that HZ016 type cation exchange resin was used to adsorb Sn2+ and Fe2+ in electroplated tin solution first. After adsorption, the resin was removed by sulfuric acid, which was added with NaOH to adjust pH value to form precipitation and separate tin. X-ray diffraction (XRD) and energy spectrum (EDS) method were used to analyze the composition of the precipitates adjusted by pH. The results show that when the mass ratio of resin to bath is 1:2, the adsorption efficiency of resin reaches 98.3% and 97.1% respectively, and the elution efficiency of tin and iron reaches 95.1% and 94% respectively when the mass ratio of resin to eluent sulfuric acid is 1:4. Sodium sulfite was added to increase the efficiency of tin recovery by 8.1%. EDS and XRD atlas showed that after pH regulation, the main composition of the filtration precipitation was the hydroxides of tin.

NtPDR3, an iron-deficiency inducible ABC transporter in Nicotiana tabacum.

PubMed

Ducos, Eric; Fraysse, Staffan; Boutry, Marc

2005-12-19

In plants, the ABC transporter PDR (pleiotropic drug resistance) subfamily is composed of approximately 15 genes, few of which have been analyzed. We have identified NtPDR3, a Nicotiana tabacum PDR gene belonging to a cluster for which no functional data was previously available. NtPDR3 was found to be induced in suspension cells treated with methyl jasmonate, salicylic acid, 1-naphthalene acetic acid, or cembrene, a macrocyclic diterpene. In agreement with the identification of a putative iron deficiency element in the NtPDR3 transcription promoter region, we found that iron deficiency in the culture medium induced NtPDR3 expression, thus suggesting a new function of the PDR transporter family.

Affinity resins as new tools for identifying target proteins of ascorbic acid.

PubMed

Iwaoka, Yuji; Nishino, Kohei; Ishikawa, Takahiro; Ito, Hideyuki; Sawa, Yoshihiro; Tai, Akihiro

2018-02-12

l-Ascorbic acid (AA) has diverse physiological functions, but little is known about the functional mechanisms of AA. In this study, we synthesized two types of affinity resin on which AA is immobilized in a stable form to identify new AA-targeted proteins, which can provide important clues for elucidating unknown functional mechanisms of AA. To our knowledge, an affinity resin on which AA as a ligand is immobilized has not been prepared, because AA is very unstable and rapidly degraded in an aqueous solution. By using the affinity resins, cytochrome c (cyt c) was identified as an AA-targeted protein, and we showed that oxidized cyt c exhibits specific affinity for AA. These results suggest that two kinds of AA-affinity resin can be powerful tools to identify new target proteins of AA.

Affinity purification of the voltage-sensitive sodium channel from electroplax with resins selective for sialic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

James, W.M.; Emerick, M.C.; Agnew, W.S.

1989-07-11

The voltage-sensitive sodium channel present in the eel (Electrophorus electricus) has an unusually high content of sialic acid, including {alpha}-(2{yields}8)-linked polysialic acid, not found in other electroplax membrane glycopeptides. Lectins from Limax flavus (LFA) and wheat germ (WGA) proved the most effective of 11 lectin resins tried. The most selective resin was prepared from IgM antibodies against Neisseria meningitidis {alpha}-(2{yields}8)-polysialic acid which were affinity purified and coupled to Sepharose 4B. The sodium channel was found to bind to WGA, LFA, and IgM resins and was readily eluted with the appropriate soluble carbohydrates. Experiments with LFA and IgM resins demonstrated bindingmore » and unbinding rates and displacement kinetics, which suggest highly specific binding at multiple sites on the sodium channel protein. In preparative-scale purification of protein previously fractionated by anion-exchange chromatography, without stabilizing TTX, high yields were reproducibly obtained. Further, when detergent extracts were prepared from electroplax membranes fractionated by low-speed sedimentation, a single step over the IgM resin provided a 70-fold purification, yielding specific activities of 3,200 pmol of ({sup 3}H)TTX-binding sites/mg of protein and a single polypeptide of {approximately}285,000 Da on SDS-acrylamide gels. No small peptides were observed after this 5-h isolation. The authors describe a cation-dependent stabilization with millimolar levels of monovalent and micromolar levels of divalent species.« less

Comparison of total phenolic content, scavenging activity and HPLC-ESI-MS/MS profiles of both young and mature leaves and stems of Andrographis paniculata.

PubMed

Chua, Lee Suan; Yap, Ken Choy; Jaganath, Indu Bala

2013-12-01

The total phenolic content and radical scavenging activity of Andrographis paniculata has been investigated to estimate the amount of phenolic compounds and diterpene lactones, respectively in the plant extracts. The stem extracts exhibited higher total phenolic content and scavenging activity than those of the leaf extracts from both young and mature plants. A range of 19.6-47.8 mg extract of A. paniculata from different parts of the plant is equivalent to the scavenging activity exhibited by one mg of standard Trolox. HPLC-ESI-MS/MS was also used to identify simultaneously the phytochemicals from the leaves and stems of both young and mature plant samples. Of the identified compounds, seven of the sixteen diterpene lactones, three of the six flavonoids, five of the six phenolic acids and two cyclic acids are reported here for the first time for this species. Multivariate statistical approaches such as Hierarchiral Component Analysis (HCA) and Principle Component Analysis (PCA) have clustered the plant extracts into the leaf and stem groups, regardless of plant age. Further classification based on the phytochemical profiles revealed that mostly phenolic acids and flavonoids were from the young leaf extracts, and diterpenoids and their glycosides from the mature leaf extracts. However, the phytochemical profiles for the stems of both young and mature plants were not significantly different as presented in the dendrogram of HCA and the score plot of PCA. The marker for mature plants might be the m/z 557 ion (dihydroxyl dimethyl 19-[(beta-D-glucopyranosyl)oxy]-19-oxo-ent-labda-8(17),13-dien-16,15-olide), whereas the m/z 521 ion (propyl neoandrographolide) could be the marker for leaf extracts.

Zinc incorporation improves biological activity of beta-tricalcium silicate resin-based cement.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Tim F; Toledano, Manuel

2014-11-01

Matrix metalloproteinase (MMP) inhibition may improve endodontic treatment prognosis. The purpose of this study was to determine if zinc incorporation into experimental resin cements containing bioactive fillers may modulate MMP-mediated collagen degradation of dentin. Human dentin samples untreated and demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (OSspray, London, UK), (3) resin with beta-tricalcium silicate particles (βTCS), (4) resin with zinc-doped Bioglass 45S5, and (5) resin with zinc-doped βTCS particles. The specimens were stored in artificial saliva (for 24 hours, 1 week, and 4 weeks) and submitted to radioimmunoassay to quantify C-terminal telopeptide. Scanning electron microscopy analysis was also undertaken on dentin samples after 4 weeks of storage. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced MMP activity in demineralized dentin. Resin containing Bioglass 45S5 particles exerted higher and stable protection of collagen. The presence of zinc in βTCS particles increases MMP inhibition. Different mineral precipitation was attained in dentin infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced after resin infiltration of dentin. Zinc incorporation in βTCS particles exerted an additional protection against MMP-mediated collagen degradation. However, it did not occur in resin containing Bioglass 45S5 particles, probably because of the formation of phosphate-zinc compounds. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Pahangensin A and B, two new antibacterial diterpenes from the rhizomes of Alpinia pahangensis Ridley.

PubMed

Sivasothy, Yasodha; Ibrahim, Halijah; Paliany, Audra Shaleena; Alias, Siti Aisyah; Awang, Khalijah

2013-12-01

The rhizomes of Alpinia pahangensis Ridley yielded a new bis-labdanic diterpene for which the name pahangensin A (1) was proposed along with a new labdane diterpene, pahangensin B (2). Their structures were elucidated by spectroscopic methods including, 1D and 2D NMR techniques and LCMS-IT-TOF analysis. Pahangensin A (1) was found to be an antibacterial agent against Staphylococcus aureus, Bacillus cereus and Bacillus subtilis with MIC values less than 100 μg/mL, respectively. Pahangensin B (2) exhibited antibacterial activity (MIC <100 μg/mL) against B. cereus. Copyright © 2013 Elsevier Ltd. All rights reserved.

Three new cyathane diterpenes with neurotrophic activity from the liquid cultures of Hericium erinaceus.

PubMed

Zhang, Yuting; Liu, Li; Bao, Li; Yang, Yanlong; Ma, Ke; Liu, Hongwei

2018-05-21

Three new cyathane diterpenes erinacines T-V (1-3), and two known cyathane diterpenes erinacine A (4) and erinacine P (5) were isolated from the liquid cultures of Hericium erinaceus. The structures of 1-3 were determined by extensive spectroscopic analysis. All isolated compounds were evaluated for the cytotoxicity, and neurite-promoting activities using PC12 cell line. Compounds 1-3, and 5 exhibited pronounced neurite outgrowth-promoting effects on PC12 cells in the range of 2.5-10 μM. Compound 4 showed weak cytotoxicity against PC12 cells with IC 50 of 73.7 μM.

Tensile bond strength of an aged resin composite repaired with different protocols.

PubMed

Celik, Esra Uzer; Ergücü, Zeynep; Türkün, L Sebnem; Ercan, Utku Kürșat

2011-08-01

To evaluate the effect of different surface treatments and bonding procedures on the tensile bond strength (TBS) of resin composites repaired 6 months after polymerization. Resin composite sticks were aged in distilled water at 37°C for 6 months. They were divided into 12 groups (n = 10) according to the combination of surface treatment/bonding procedures [none, only bur treatment, XP Bond (XPB/Dentsply/DeTrey) with/without bur, AdheSE (A-SE/Ivoclar/Vivadent) with/without bur, Composite Primer (CP/GC) with/without bur, CP after bur and acid-etching, XPB after acid etching and CP with bur, A-SE after bur and CP]. The ultimate tensile bond strength (UTS) of the resin composites was tested in intact but aged specimens. Tensile bond strengths were tested with a universal testing machine (Shimadzu). Data were analyzed using one-way ANOVA and Duncan Multiple Comparisons tests (p < 0.05). All repaired groups showed significantly higher TBS than the group without any sureface treatment (p < 0.05). Four groups resulted in TBS similar to those of intact resin composite UTS: A-SE, A-SE with bur, A-SE after CP with bur, and XPB after acid etching+CP with bur. Bur treatment, silane primer or etch-and-rinse adhesive application alone were not successful in the repair process of aged resin composite, whereas self-etching adhesive alone showed similar performance to the intact specimens. Combined procedures generally showed better performance: A-SE with bur, A-SE after CP with bur, and XPB after acid etching +CP with bur showed TBS similar to those of the intact specimens. It was concluded that bur roughening of the surfaces and rebonding procedures were essential for repairing aged resin composites.

Diterpenoids from Casearia sylvestris

USDA-ARS?s Scientific Manuscript database

Two highly oxygenated clerodane diterpenes casearins U (1) and V (2) and two ent-kaurane diterpene glucosides sylvestrisides A (3) and B (4) were isolated from the leaves of Casearia sylvestris, together with 13 known compounds. Their structures were established on the basis of 1D and 2D NMR spectro...

Low dielectric polyimide fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

1994-01-01

A high temperature resistant polyimide fiber that has a dielectric constant of less than 3 is presented. The fiber was prepared by first reacting 2,2-bis (4-(4aminophenoxy)phenyl) hexafluoropropane with 2,2-bis (3,4-dicarboxyphenyl) hexafluoropropane dianhydride in an aprotic solvent to form a polyamic acid resin solution. The polyamic acid resin solution is then extruded into a coagulation medium to form polyamic acid fibers. The fibers are thermally cured to their polyimide form. Alternatively, 2,2-bis(4-(4-aminophenoxy)phenyl) hexafluoropropane is reacted with 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride to form a polyamic acid, and the polyamic acid is chemically converted to its polyimide form. The polyimide is then dissolved in a solvent to form a polyimide resin solution, and the polyimide resin is extruded into a coagulation medium to form a polyimide wet gel filament. In order to obtain polyimide fibers of increased tensile properties, the polyimide wet gel filaments are stretched at elevated temperatures. The tensile properties of the fibers were measured and found to be in the range of standard textile fibers. Polyimide fibers obtained by either method will have a dielectric constant similar to that of the corresponding polymer, viz., less than 3 at 10 GHz.

Versatile On-Resin Synthesis of High Mannose Glycosylated Asparagine with Functional Handles

PubMed Central

Chen, Rui; Pawlicki, Mark A.; Tolbert, Thomas J.

2013-01-01

Here we present a synthetic route for solid phase synthesis of N-linked glycoconjugates containing high mannose oligosaccharides which allows the incorporation of useful functional handles on the N-terminus of asparagine. In this strategy, the C-terminus of an Fmoc protected aspartic acid residue is first attached to a solid phase support. The side chain of aspartic acid is protected by a 2-phenylisopropyl protecting group, which allows selective deprotection for the introduction of glycosylation. By using a convergent on-resin glycosylamine coupling strategy, an N-glycosidic linkage is successfully formed on the free side chain of the resin bound aspartic acid with a large high mannose oligosaccharide, Man8GlcNAc2, to yield N-linked high mannose glycosylated asparagine. The use of on-resin glycosylamine coupling provides excellent glycosylation yield, can be applied to couple other types of oligosaccharides, and also makes it possible to recover excess oligosaccharides conveniently after the on-resin coupling reaction. Useful functional handles including an alkene (p-vinylbenzoic acid), an alkyne (4-pentynoic acid), biotin, and 5-carboxyfluorescein are then conjugated onto the N-terminal amine of asparagine on-resin after the removal of the Fmoc protecting group. In this way, useful functional handles are introduced onto the glycosylated asparagine while maintaining the structural integrity of the reducing end of the oligosaccharide. The asparagine side chain also serves as a linker between the glycan and the functional group and preserves the native presentation of N-linked glycan which may aid in biochemical and structural studies. As an example of a biochemical study using functionalized high mannose glycosylated asparagine, a fluorescence polarization assay has been utilized to study the binding of the lectin Concanavalin A (ConA) using 5-carboxyfluorescein labeled high mannose glycosylated asparagine. PMID:24326091

Comparison of microleakage of three acid-base luting cements versus one resin-bonded cement for Class V direct composite inlays.

PubMed

Piemjai, Morakot; Miyasaka, Kumiko; Iwasaki, Yasuhiko; Nakabayashi, Nobuo

2002-12-01

Demineralized dentin beneath set cement may adversely affect microleakage under fixed restorations. Microleakage of direct composite inlays cemented with acid-base cements and a methyl methacrylate resin cement were evaluated to determine their effect on the integrity of the underlying hybridized dentin. Sixty Class V box preparations (3 mm x 3 mm x 1.5 mm) were precisely prepared in previously frozen bovine teeth with one margin in enamel and another margin in dentin. Direct composite inlays (EPIC-TMPT) for each preparation were divided into 4 groups of 15 specimens each and cemented with 3 acid-base cements (control group): Elite, Ketac-Cem, Hy-Bond Carbo-Cem, and 1 adhesive resin cement: C&B Metabond. All specimens were stored in distilled water for 24 hours at 37 degrees C before immersion in 0.5% basic fuchsin for 24 hours. The dye penetration was measured on the sectioned specimens at the tooth-cement interface of enamel and cementum margins and recorded with graded criteria under light microscopy (Olympus Vanox-T) at original magnification x 50, 100, and 200. A Kruskal-Wallis and the Mann-Whitney test at P<.05 were used to analyze leakage score. All cementum margins of the 3 acid-base cements tested demonstrated significantly higher leakage scores than cementum margins for inlays cemented with the resin cement tested(P<.01). No leakage along the tooth-cement interface was found for inlays retained with the adhesive resin cement. Within the limitations of this study, the 3 acid-base cements tested exhibited greater microleakage at the cementum margins than did the adhesive resin cement that was tested.

The first structure of a bacterial diterpene cyclase: CotB2.

PubMed

Janke, Ronja; Görner, Christian; Hirte, Max; Brück, Thomas; Loll, Bernhard

2014-06-01

Sesquiterpenes and diterpenes are a diverse class of secondary metabolites that are predominantly derived from plants and some prokaryotes. The properties of these natural products encompass antitumor, antibiotic and even insecticidal activities. Therefore, they are interesting commercial targets for the chemical and pharmaceutical industries. Owing to their structural complexity, these compounds are more efficiently accessed by metabolic engineering of microbial systems than by chemical synthesis. This work presents the first crystal structure of a bacterial diterpene cyclase, CotB2 from the soil bacterium Streptomyces melanosporofaciens, at 1.64 Å resolution. CotB2 is a diterpene cyclase that catalyzes the cyclization of the linear geranylgeranyl diphosphate to the tricyclic cyclooctat-9-en-7-ol. The subsequent oxidation of cyclooctat-9-en-7-ol by two cytochrome P450 monooxygenases leads to bioactive cyclooctatin. Plasticity residues that decorate the active site of CotB2 have been mutated, resulting in alternative monocyclic, dicyclic and tricyclic compounds that show bioactivity. These new compounds shed new light on diterpene cyclase reaction mechanisms. Furthermore, the product of mutant CotB2(W288G) produced the new antibiotic compound (1R,3E,7E,11S,12S)-3,7,18-dolabellatriene, which acts specifically against multidrug-resistant Staphylococcus aureus. This opens a sustainable route for the industrial-scale production of this bioactive compound.

Anti-allodynic and Anti-hyperalgesic effects of an ethanolic extract and xylopic acid from the fruits of Xylopia aethiopica in murine models of neuropathic pain

PubMed Central

Ameyaw, Elvis O.; Woode, Eric; Boakye-Gyasi, Eric; Abotsi, Wonder K.M.; Kyekyeku, James Oppong; Adosraku, Reimmel K.

2014-01-01

Background: Fruit extracts of Xylopia aethiopica are used traditionally in the management of pain disorders including headache and neuralgia. An animal model of vincristine-induced sensory neuropathy was developed after repeated intraperitoneal injection in rats and used in the present work to study the effects of the ethanolic extract of X. aethiopica (XAE) and its diterpene xylopic acid (XA) in vincristine-induced neuropathic pain. Materials and Methods: Vincristine (0.1 mg kg-1 day-1) was administered during two cycles of five consecutive days to induce chemotherapy-induced neuropathic pain. Static tactile anti-allodynic, anti-hyperalgesic, and cold anti-allodynic effects of XAE (30-300 mg kg-1) and XA (10-100 mg kg-1) were assessed using Von Frey filaments of bending forces of 4, 8, and 15 g, the Randall-Selitto paw pressure test, and cold water (4.5°C), respectively. Results: Administration of vincristine caused the development of allodynia and hyperalgesia with no significant motor deficit, spontaneous pain, and foot deformity. XAE (30-300 mg kg-1) and XA (10-100 mg kg-1) exhibited anti-hyperalgesic, tactile, and cold anti-allodynic properties with XA exhibiting greater potency than XAE. Pregabalin (10-100 mg kg-1) used as control produced similar effect. Conclusion: These findings establish the anti-allodynic and anti-hyperalgesic effects of the ethanolic fruit XAE and its major diterpene XA in vincristine-induced neuropathtic pain. PMID:24761123

Anti-allodynic and Anti-hyperalgesic effects of an ethanolic extract and xylopic acid from the fruits of Xylopia aethiopica in murine models of neuropathic pain.

PubMed

Ameyaw, Elvis O; Woode, Eric; Boakye-Gyasi, Eric; Abotsi, Wonder K M; Kyekyeku, James Oppong; Adosraku, Reimmel K

2014-04-01

Fruit extracts of Xylopia aethiopica are used traditionally in the management of pain disorders including headache and neuralgia. An animal model of vincristine-induced sensory neuropathy was developed after repeated intraperitoneal injection in rats and used in the present work to study the effects of the ethanolic extract of X. aethiopica (XAE) and its diterpene xylopic acid (XA) in vincristine-induced neuropathic pain. Vincristine (0.1 mg kg(-1) day(-1)) was administered during two cycles of five consecutive days to induce chemotherapy-induced neuropathic pain. Static tactile anti-allodynic, anti-hyperalgesic, and cold anti-allodynic effects of XAE (30-300 mg kg(-1)) and XA (10-100 mg kg(-1)) were assessed using Von Frey filaments of bending forces of 4, 8, and 15 g, the Randall-Selitto paw pressure test, and cold water (4.5°C), respectively. Administration of vincristine caused the development of allodynia and hyperalgesia with no significant motor deficit, spontaneous pain, and foot deformity. XAE (30-300 mg kg(-1)) and XA (10-100 mg kg(-1)) exhibited anti-hyperalgesic, tactile, and cold anti-allodynic properties with XA exhibiting greater potency than XAE. Pregabalin (10-100 mg kg(-1)) used as control produced similar effect. These findings establish the anti-allodynic and anti-hyperalgesic effects of the ethanolic fruit XAE and its major diterpene XA in vincristine-induced neuropathtic pain.

A Convenient Approach to Synthesizing Peptide C-Terminal N-Alkyl Amides

PubMed Central

Fang, Wei-Jie; Yakovleva, Tatyana; Aldrich, Jane V.

2014-01-01

Peptide C-terminal N-alkyl amides have gained more attention over the past decade due to their biological properties, including improved pharmacokinetic and pharmacodynamic profiles. However, the synthesis of this type of peptide on solid phase by current available methods can be challenging. Here we report a convenient method to synthesize peptide C-terminal N-alkyl amides using the well-known Fukuyama N-alkylation reaction on a standard resin commonly used for the synthesis of peptide C-terminal primary amides, the PAL-PEG-PS (Peptide Amide Linker-polyethylene glycol-polystyrene) resin. The alkylation and oNBS deprotection were conducted under basic conditions and were therefore compatible with this acid labile resin. The alkylation reaction was very efficient on this resin with a number of different alkyl iodides or bromides, and the synthesis of model enkephalin N-alkyl amide analogs using this method gave consistently high yields and purities, demonstrating the applicability of this methodology. The synthesis of N-alkyl amides was more difficult on a Rink amide resin, especially the coupling of the first amino acid to the N-alkyl amine, resulting in lower yields for loading the first amino acid onto the resin. This method can be widely applied in the synthesis of peptide N-alkyl amides. PMID:22252422

Sampling and analysis of airborne resin acids and solvent-soluble material derived from heated colophony (rosin) flux: a method to quantify exposure to sensitizing compounds liberated during electronics soldering.

PubMed

Smith, P A; Son, P S; Callaghan, P M; Jederberg, W W; Kuhlmann, K; Still, K R

1996-07-17

Components of colophony (rosin) resin acids are sensitizers through dermal and pulmonary exposure to heated and unheated material. Significant work in the literature identifies specific resin acids and their oxidation products as sensitizers. Pulmonary exposure to colophony sensitizers has been estimated indirectly through formaldehyde exposure. To assess pulmonary sensitization from airborne resin acids, direct measurement is desired, as the degree to which aldehyde exposure correlates with that of resin acids during colophony heating is undefined. Any analytical method proposed should be applicable to a range of compounds and should also identify specific compounds present in a breathing zone sample. This work adapts OSHA Sampling and Analytical Method 58, which is designed to provide airborne concentration data for coal tar pitch volatile solids by air filtration through a glass fiber filter, solvent extraction of the filter, and gravimetric analysis of the non-volatile extract residue. In addition to data regarding total soluble material captured, a portion of the extract may be subjected to compound-specific analysis. Levels of soluble solids found during personal breathing zone sampling during electronics soldering in a Naval Aviation Depot ranged from below the "reliable quantitation limit" reported in the method to 7.98 mg/m3. Colophony-spiked filters analyzed in accordance with the method (modified) produced a limit of detection for total solvent-soluble colophony solids of 10 micrograms/filter. High performance liquid chromatography was used to identify abietic acid present in a breathing zone sample.

The effect of storage conditions, contamination modes and cleaning procedures on the resin bond strength to lithium disilicate ceramic.

PubMed

Klosa, Karsten; Wolfart, Stefan; Lehmann, Frank; Wenz, Hans-Jürgen; Kern, Matthias

2009-04-01

The purpose of this in-vitro study was to evaluate the resin bond strength to pre-etched lithium disilicate ceramic using different cleaning methods after two contamination modes (saliva or saliva and silicone). Plexiglas tubes filled with composite resin (MultiCore Flow) were bonded to etched and silanized ceramic disks made of lithium disilicate ceramic (IPS e.max Press) using a luting resin (Multilink Automix). Either etched or unetched ceramic surfaces were contaminated with saliva or with saliva followed by a disclosing silicone. Groups of 16 specimens each were bonded after pretreatment using 4 surface cleaning agents (37% phosphoric acid, 5% hydrofluoric acid, 96% isopropanol, air polishing device with sodium bicarbonate) in different combinations. Before measuring tensile bond strength, specimens were stored for 3 or 150 days with thermocycling. After 150 days of storage, etching of saliva-contaminated surfaces with 5% hydrofluoric acid and/or 37% phosphoric acid provided statistically significantly higher bond strengths (37.9 to 49.5 MPa) than the other cleaning methods (1.7 to 15.5 MPa). After saliva and silicone contamination, etching with 5% hydrofluoric acid provided statistically significantly higher bond strengths (44.5 to 50.3 MPa) than all other cleaning methods (0.3 to 13.5 MPa). Ceramic cleaning methods after try-in procedures have a significant influence on the resin bond strength and are dependent on the type of contamination. Re-etching lithium disilicate ceramic with 5% hydrofluoric acid is most effective in removing contamination with saliva and/or a silicone disclosing medium.

A method for the production of weakly acidic cation exchange resins

NASA Astrophysics Data System (ADS)

Heller, H.; Werner, F.; Mitschker, A.; Diehl, H. V.; Schaefer, A.

1991-12-01

The invention relates to a nonpolluting method for the production of weakly acidic cation exchange resins by saponification of cross-linked acrylonitrile bead polymers, with an alkaline saponification agent at elevated temperature, according to which method the bead polymer and alkaline saponification agent are jointly added only at elevated temperature.

Identification of indole diterpenes in Ipomoea asarifolia and Ipomoea muelleri, plants tremorgenic to livestock

USDA-ARS?s Scientific Manuscript database

Ipomoea asarifolia has been associated with a tremorgenic syndrome in livestock in Brazil and was recently reported to contain tremorgenic indole diterpenes. Ipomoea muelleri has been reported to cause a similar tremorgenic syndrome in livestock in Australia. Ipomoea asarifolia and I. muelleri were ...

ANION EXCHANGE METHOD FOR SEPARATION OF METAL VALUES

DOEpatents

Hyde, E.K.; Raby, B.A.

1959-02-10

A method is described for selectively separating radium, bismuth, poloniums and lead values from a metallic mixture of thc same. The mixture is dissolved in aqueous hydrochloric acid and the acidity is adjusted to between 1 to 2M in hydrochloric acid to form the anionic polychloro complexes of polonium and bismuth. The solution is contacted with a first anion exchange resin such as strong base quaternary ammonia type to selectively absorb the polonium and bismuth leaving the radium and lead in the effluent. The effluent, after treatment in hydrochloric acid to increase the hydrochloric acid concentration to 6M is contacted with a second anion exchange iesin of the same type as the above to selectively adsorb the lead leaving the radium in the effluent. Radium is separately recovered from the effluent from the second exchange column. Lead is stripped from the loaded resin of the second column by treatment with 3M hydrochloric acid solution. The loaded resin of the first column is washed with 8M hydrochloric acid solution to recover bismuth and then treated with strong nitric acid solution to recover polonium.

Spasmolytic activity of trachylobanes ent-7α-acetoxytrachyloban-18-oic acid and ent-7α-hydroxytrachyloban-18-oic acid isolated from Xylopia langsdorfiana A. St-Hil. & Tul. (Annonaceae).

PubMed

Santos, Rosimeire F; Martins, Italo R R; Monteiro, Fabio de S; Travassos, Rafael de A; Janebro, Daniele I; Tavares, Josean F; Silva, Marcelo S; da Silva, Bagnólia A

2012-01-01

We aimed to investigate the possible spasmolytic activity of ent-7α-acetoxytrachyloban-18-oic acid (1) and ent-7α-hydroxytrachyloban-18-oic acid (2) on smooth muscle models. In male rat aorta and rat uterus, both diterpenes were unable to trigger spasmolytic action. However, 2 relaxed guinea-pig trachea: Compounds 1 and 2 antagonised, significantly and concentration-dependently, carbachol- and histamine-induced phasic contractions in guinea-pig ileum. Moreover, they induced a significant and concentration-dependent relaxation in pre-contracted (KCl, carbachol or histamine) guinea-pig ileum, with 2 being 15 times more potent than 1 in histamine-contracted ileum. These dissimilar results may be due to chemical differences between them. Thus, we demonstrated that 1 and 2 seem to be promising spasmolytic agents, although further studies are required to elucidate the spasmolytic action mechanism.

Natural derivatives of diphenolic acid as substitutes for bisphenol-A

NASA Astrophysics Data System (ADS)

Ertl, Johanna; Cerri, Elisa; Rizzuto, Matteo; Caretti, Daniele

2014-05-01

Diphenolic acid had been originally used in the first epoxy resins and was later on forgotten as it was substituted by the cheaper bisphenol A. But in the recent years major health concerns have been raised as bisphenol A has a pseudo-hormonal effect on the body, playing the role of estrogen it can cause a severe impact on the organism, especially in males. Moreover it is produced from acetone and phenol, both from fossil, and thus limited resources. On the contrary, diphenolic acid is synthesized from levulinic acid and phenol. Levulinic acid being directly produced by hydrolysis of biomass. By substituting the fossil phenol with natural phenols from lignin or plant extraction we are able to synthesize a fully renewable substitute for bisphenol A. The reactions to yield an epoxy resin have been examined and the reactivity with epichlorohydrin is satisfying. Moreover, some of the derivatives of diphenolic acid have interesting curing properties and preliminary results show excellent properties of the cured resin, including thermal stability and pencil hardness.

Strategies for improving production performance of probiotic Pediococcus acidilactici viable cell by overcoming lactic acid inhibition.

PubMed

Othman, Majdiah; Ariff, Arbakariya B; Wasoh, Helmi; Kapri, Mohd Rizal; Halim, Murni

2017-11-27

Lactic acid bacteria are industrially important microorganisms recognized for fermentative ability mostly in their probiotic benefits as well as lactic acid production for various applications. Fermentation conditions such as concentration of initial glucose in the culture, concentration of lactic acid accumulated in the culture, types of pH control strategy, types of aeration mode and different agitation speed had influenced the cultivation performance of batch fermentation of Pediococcus acidilactici. The maximum viable cell concentration obtained in constant fed-batch fermentation at a feeding rate of 0.015 L/h was 6.1 times higher with 1.6 times reduction in lactic acid accumulation compared to batch fermentation. Anion exchange resin, IRA 67 was found to have the highest selectivity towards lactic acid compared to other components studied. Fed-batch fermentation of P. acidilactici coupled with lactic acid removal system using IRA 67 resin showed 55.5 and 9.1 times of improvement in maximum viable cell concentration compared to fermentation without resin for batch and fed-batch mode respectively. The improvement of the P. acidilactici growth in the constant fed-batch fermentation indicated the use of minimal and simple process control equipment is an effective approach for reducing by-product inhibition. Further improvement in the cultivation performance of P. acidilactici in fed-bath fermentation with in situ addition of anion-exchange resin significantly helped to enhance the growth of P. acidilactici by reducing the inhibitory effect of lactic acid and thus increasing probiotic production.

Carbon dioxide capture using resin-wafer electrodeionization

DOEpatents

Lin, YuPo J.; Snyder, Seth W.; Trachtenberg, Michael S.; Cowan, Robert M.; Datta, Saurav

2015-09-08

The present invention provides a resin-wafer electrodeionization (RW-EDI) apparatus including cathode and anode electrodes separated by a plurality of porous solid ion exchange resin wafers, which when in use are filled with an aqueous fluid. The apparatus includes one or more wafers comprising a basic ion exchange medium, and preferably includes one or more wafers comprising an acidic ion exchange medium. The wafers are separated from one another by ion exchange membranes. The fluid within the acidic and/or basic ion exchange wafers preferably includes, or is in contact with, a carbonic anhydrase (CA) enzyme to facilitate conversion of bicarbonate ion to carbon dioxide within the acidic medium. A pH suitable for exchange of CO.sub.2 is electrochemically maintained within the basic and acidic ion exchange wafers by applying an electric potential across the cathode and anode.

Acrylic acid removal by acrylic acid utilizing bacteria from acrylonitrile-butadiene-styrene resin manufactured wastewater treatment system.

PubMed

Wang, C C; Lee, C M

2006-01-01

The aim of this study is to isolate the acrylic acid utilizing bacteria from the ABS resin manufactured wastewater treatment system. The bacteria should have the ability to remove acrylic acid and tolerate the acrylonitrile and acrylamide toxicity. The aim is also to understand the performance of isolated pure strain for treating different initial acrylic acid concentrations from synthetic wastewater. The results are: twenty strains were isolated from the ABS resin manufactured wastewater treatment system and twelve of them could utilize 600 mg/l acrylic acid for growth. Seven of twelve strains could tolerate the acrylonitrile and acrylamide toxicity, when the concentration was below 300 mg/l. Bacillus thuringiensis was one of the seven strains and the optimum growth temperature was 32 degrees C. Bacillus thuringiensis could utilize acrylic acid for growth, when the initial acrylic acid concentration was below 1,690.4 mg/l. Besides this, when the initial acrylic acid concentration was below 606.8 mg/l, the acrylic acid removal efficiency exceeded 96.3%. Bacillus thuringiensis could tolerate 295.7 mg/l acrylamide and 198.4 mg/l acrylonitrile toxicity but could not tolerate 297.3 mg/l epsilon-caprolactam.

Reaction pH of urea-formaldehyde resins as related to strength properties of southern pine particleboard

Treesearch

C. -Y. Hse

1974-01-01

Twelve urea-formaldehyde resins were prepared with factorial combinations of 4 alkaline and 3 acidic reaction phases; i. e., the reaction mixture was adjusted to pH 7, 8, 9, or 10 for the first hour and then made weakly acid to pH 5.8, 4.8, or 3.8.

ION EXCHANGE PROCESS FOR THE RECOVERY AND PURIFICATION OF MATERIALS

DOEpatents

Long, R.S.; Bailes, R.H.

1958-04-15

A process for the recovery of certain metallic ions from aqueous solutions by ion exchange techniques is described. It is applicable to elements such as vanadium, chromium, nnanganese, and the like, which are capable of forming lower valent cations soluble in aqueous solutions and which also form ldgher valent anions soluble in aqueous acidic solutions. For example, small amounts of vanadium occurring in phosphoric acid prepared from phosphate rock may be recovered by reducing the vanadium to a trivalent cation adsorbing; the vanadium in a cationic exchange resin, then treating the resin with a suitable oxidizing agent to convert the adsorbed vanadium to a higher valent state, and finally eluting; the vanadium as an anion from the resin by means of an aqueous acidic solution.

Resin catalysts and method of preparation

DOEpatents

Smith, Jr., Lawrence A.

1986-01-01

Heat stabilized catalyst compositions are prepared from nuclear sulfonic acid, for example, macroporous crosslinked polyvinyl aromatic compounds containing sulfonic acid groups are neutralized with a metal of Al, Fe, Zn, Cu, Ni, ions or mixtures and alkali, alkaline earth metals or ammonium ions by contacting the resin containing the sulfonic acid with aqueous solutions of the metals salts and alkali, alkaline earth metal or ammonium salts. The catalysts have at least 50% of the sulfonic acid groups neutralized with metal ions and the balance of the sulfonic acid groups neutralized with alkali, alkaline earth ions or ammonium ions.

Resin catalysts and method of preparation

DOEpatents

Smith, L.A. Jr.

1986-12-16

Heat stabilized catalyst compositions are prepared from nuclear sulfonic acid, for example, macroporous crosslinked polyvinyl aromatic compounds containing sulfonic acid groups are neutralized with a metal of Al, Fe, Zn, Cu, Ni, ions or mixtures and alkali, alkaline earth metals or ammonium ions by contacting the resin containing the sulfonic acid with aqueous solutions of the metals salts and alkali, alkaline earth metal or ammonium salts. The catalysts have at least 50% of the sulfonic acid groups neutralized with metal ions and the balance of the sulfonic acid groups neutralized with alkali, alkaline earth ions or ammonium ions.

Cytotoxic diterpenes from roots of Crossopetalum gaumeri, a Celastraceae species from Yucatan Peninsula.

PubMed

Miron-Lopez, Gumersindo; Bazzocchi, Isabel L; Jimenez-Diaz, Ignacio A; Moujir, Laila M; Quijano-Quiñones, Ramiro; Quijano, Leovigildo; Mena-Rejon, Gonzalo J

2014-05-01

Four new diterpenes, crossogumerins A-D (1-4) along with six known ones (5-10) were isolated from the root bark of Crossopetalum gaumeri, an endemic medicinal plant from the Yucatan Peninsula. Their structures were elucidated on the basis of 1D and 2D NMR techniques, including HMQC, HMBC, and ROESY experiments. Compounds 1-5, 8-10 were evaluated for cytotoxicity against HeLa (carcinoma of the cervix) and Hep-2 (lung carcinoma) human tumor cells lines and against normal Vero cells (African green monkey kidney) in lag and log phase of growth. Podocarpane diterpenes, crossogumerin B (2) and nimbiol (10), exhibited the highest activity against HeLa cells (IC50 values of 3.1 and 8.1 μM, respectively), but also selectivity on Vero cells (SI 22.6 and 7.5, respectively). The preliminary SAR studies suggest that an epoxy moiety in ring B and a hydrogen bond-donor group strategically positioned in the diterpene core are important requirements for cytotoxicity and selectivity. Copyright © 2014. Published by Elsevier Ltd.

Structure-based drug design studies of the interactions of ent-kaurane diterpenes derived from Wedelia paludosa with the Plasmodium falciparum sarco/endoplasmic reticulum Ca²⁺-ATPase PfATP6.

PubMed

Guimarães, Daniel Silqueira Martins; Fonseca, Amanda Luisa da; Batista, Ronan; Comar Junior, Moacyr; Oliveira, Alaíde Braga de; Taranto, Alex Gutterres; Varotti, Fernando de Pilla

2015-04-01

Malaria is responsible for more deaths around the world than any other parasitic disease. Due to the emergence of strains that are resistant to the current chemotherapeutic antimalarial arsenal, the search for new antimalarial drugs remains urgent though hampered by a lack of knowledge regarding the molecular mechanisms of artemisinin resistance. Semisynthetic compounds derived from diterpenes from the medicinal plant Wedelia paludosa were tested in silico against the Plasmodium falciparum Ca2+-ATPase, PfATP6. This protein was constructed by comparative modelling using the three-dimensional structure of a homologous protein, 1IWO, as a scaffold. Compound 21 showed the best docking scores, indicating a better interaction with PfATP6 than that of thapsigargin, the natural inhibitor. Inhibition of PfATP6 by diterpene compounds could promote a change in calcium homeostasis, leading to parasite death. These data suggest PfATP6 as a potential target for the antimalarial ent-kaurane diterpenes.

Bond strength of Bis-GMA and glass ionomer pit and fissure sealants using cyclic fatigue.

PubMed

Dewji, H R; Drummond, J L; Fadavi, S; Punwani, I

1998-02-01

The aim of the study was to determine the bond strength of glass ionomer and resin-modified glass ionomer sealants compared to Bis-GMA sealants using both static and cyclic fatigue shear testing. Four materials were evaluated: D, a Bis-GMA sealant with 10% phosphoric acid etchant; FC, a resin-modified glass ionomer sealant with 20% polyacrylic acid etchant; FD, a resin-modified glass ionomer sealant with 10% polyacrylic acid etchant; and FSC, a self-cured glass ionomer sealant with no etchant. Gelatin capsules filled with the sealant material were bonded to the enamel surfaces of bovine teeth after appropriate surface conditioning and then tested in shear static and cyclic fatigue. Static and cyclic shear bond strengths, respectively, for each group were (MPa): FC: 21.1+/-2.8 and 17.1+/-3.1; FD: 14.6+/-5.9 and 8.5+/-3.1; D: 10.8+/-4.9 and 4.7+/-2.6; FSC: 8.7 (1.0 and 2.9+/-0.6. The resin-modified glass ionomer sealants had better fatigue bond strength than both Bis-GMA and self-cured glass ionomer sealants with the surface conditioning affecting the bond strength of the resin-modified glass ionomer sealants.

[Bonding strength of resin and tooth enamel after teeth bleaching with cold plasma].

PubMed

Zhu, Meng-meng; Wang, Guo-min; Sun, Ke; Li, Ying-long; Pan, Jie

2016-02-18

To investigate the immediate bond strength and surface structure of resin and the tooth enamel which treated by cold plasma. In the study, 40 bovine incisors were divided into two equal parts. In this sense, all enamel adhesive samples were prepared and then randomly divided into 4 groups (n =20). group 1: acid + single bond 2+resin composite (control group); group 2:beyond bleaching+ acid+single bond 2+resin composite; group 3: treated by cold plasma for 5 minutes+ acid+single bond 2+resin composite; group 4: treated by cold plasma for 5 minutes+single bond 2+resin composite. Single bond 2 bonding system and Filtek Z250 resin were used in this experiment. The shear bond strength was tested by universal testing machine. The surface of the enamel in different processes was observed by scanning electron microscope (SEM). Statistical analyses by the single factor analysis of variance and multiple pairwise comparisons were performed with SPSS 17.0 . The shear bond strength of group 4 (8.60 MPa) was significantly lower than that of the other three groups (P<0.05). The shear bond strength of group 2 (17.89 MPa) was higher than that of group 4, but lower than group 1 and group 3 (P<0.05).There was no significant difference between group 1 (34.82 MPa) and group 3 (34.69 MPa). Scanning electron microscope indicated that the enamel treated by cold plasma had slight molten form, which was different from etched enamel surface.The fractured surface of group 3 was mix fracture, which was similar to the control group (group 1). Compared with the conventional clinic bleaching, immediate bond strength of resin-enamel that treated by cold plasma has not been affected.

Synthesis, characterization and applications of a new cation exchanger tamarind sulphonic acid (TSA) resin.

PubMed

Singh, A V; Sharma, Naresh Kumar; Rathore, Abhay S

2012-01-01

A new composite cation exchanger, tamarind sulphonic acid (TSA) resin has been synthesized. The chemically modified TSA ion exchange resin has been used for the removal and preconcentration of Zn2+, Cd2+, Fe2+, Co2+ and Cu2+ ions in aqueous solution and effluent from the Laxmi steel plant in Jodhpur, India. This type of composite represents a new class of hybrid ion exchangers with good ion exchange capacity, stability, reproducibility and selectivity for toxic metal ions found in effluent from the steel industry. The characterization of the resin was carried out by determining the ion-exchange capacity, elemental analysis, pH titration, Fourier transform infrared spectra and thermal analysis. The distribution coefficients (K(d)) of toxic metal ions were determined in a reference aqueous solution and the steel plant effluent at different pH values; the absorbency of different metal ions on the TSA resin was studied for up to 10 cycles. The adsorption of different metal ions on TSA resin follows the order: Co2+ > Cu2+ > Zn2+ > Fe2+ > Cd2+. The ion exchange capacity of TSA resin is 2.87%.

Bond strength of orthodontic light-cured resin-modified glass ionomer cement.

PubMed

Cheng, Hsiang Yu; Chen, Chien Hsiu; Li, Chuan Li; Tsai, Hung Huey; Chou, Ta Hsiung; Wang, Wei Nan

2011-04-01

The purpose of this study was to compare the bond strengths and debonded interfaces achieved with light-cured resin-modified glass ionomer cement (RMGIC) and conventional light-cured composite resin. In addition, the effects of acid etching and water contamination were examined. One hundred human premolars were randomly divided into five equal groups. The mini Dyna-lock upper premolar bracket was selected for testing. The first four groups were treated with light-cured RMGIC with or without 15 per cent phosphoric acid-etching treatment and with or without water contamination preceding bracket bonding. The control samples were treated with the conventional light-cured Transbond composite resin under acid etching and without water contamination. Subsequently, the brackets were debonded by tensile force using an Instron machine. The modified adhesive remnant index (ARI) scores were assigned to the bracket base of the debonded interfaces using a scanning electron microscope. The bond strength and modified ARI scores were determined and analysed statistically by one-way analysis of variance and chi-square test. Under all four conditions, the bond strength of the light-cure RMGIC was equal to or higher than that of the conventional composite resin. The highest bond strength was achieved when using RMGIC with acid etching but without water contamination. The modified ARI scores were 2 for Fuji Ortho LC and 3 for Transbond. No enamel detachment was found in any group. Fifteen per cent phosphoric acid etching without moistening the enamel of Fuji Ortho LC provided the more favourable bond strength. Enamel surfaces, with or without water contamination and with or without acid etching, had the same or a greater bond strength than Transbond.

Assessment of microleakage of class V restored by resin composite and resin-modified glass ionomer and pit and fissure resin-based sealants following Er:YAG laser conditioning and acid etching: in vitro study

PubMed Central

Luong, Emilie; Shayegan, Amir

2018-01-01

Aim The aim of this study was to make a comparison between microleakage of conventionally restored class V cavities using acid etchant and the ones conditioned by erbium-doped yttrium aluminum garnet (Er:YAG) laser, and also to assess and compare the effectiveness of enamel surface treatments of occlusal pits and fissures by acid etching and conditioned by Er:YAG laser-etch. Materials and methods Seventy-two extracted third molars were used in this study. The samples were divided into two major groups: class V cavities and pit and fissure sealants. Each subgroup was divided into conventional acid etching, Er:YAG laser conditioning and conventional acid etching, and combination with Er:YAG laser conditioning (n=12). The teeth were placed in 2% methylene blue dye solution, were sectioned, and were evaluated according to the dye penetration criteria. Two samples per subgroup were chosen for scanning electron microscopic (SEM) analysis. Results There was a significant difference between occlusal and cervical margin groups. Laser conventional composite cementum group showed more microleakage values compared to other groups. There was no significant difference between occlusal margin groups. However, there was a significant difference between cervical margin groups in terms of microleakage. In sealant groups, there was a significant difference between laser and conventional with/without laser treatment groups in terms of microleakage. Conclusion Based on the results reported in this study, it can be concluded that the application of the Er:YAG laser beneath the resin composite, the resin-modified glass ionomers (GIs), and the fissure sealant placement may be an alternative enamel and dentin etching method to acid etching. PMID:29881311

Experimental resin cements containing bioactive fillers reduce matrix metalloproteinase-mediated dentin collagen degradation.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Thimoty F; Toledano, Manuel

2012-09-01

Collagen dentin matrix may represent a suitable scaffold to be remineralized in the presence of bioactive materials. The purpose of this study was to determine if experimental resin cements containing bioactive fillers may modulate matrix metalloproteinase-mediated collagen degradation of etched dentin. Human dentin beams demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (Sylc; OSspray Ltd, London, UK), and (3) resin with β-tricalcium phosphate-modified calcium silicate cement (HCAT-β) particles. The filler/resin ratio was 40/60 wt%. The specimens were stored in artificial saliva, and the determination of C-terminal telopeptide (ICTP) was performed by radioimmunoassay after 24 hours, 1 week, and 4 weeks. Scanning electron microscopic analysis of dentin surfaces after 4 weeks of storage was also executed. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced the MMP activity in demineralized dentin. Resin-containing Bioglass 45S5 particles exerted higher and more stable protection of collagen at all tested dentin states and time points. HCAT-β induced collagen protection from MMPs only in EDTA-treated specimens. Dentin remineralization was achieved when dentin was infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced in resin-infiltrated dentin. The inclusion of Bioglass 45S5 particles exerted an additional protection of collagen during dentin remineralization. Copyright © 2012 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Evaluation of polymeric adsorbent resins for efficient detoxification of liquor generated during acid pretreatment of lignocellulosic biomass.

PubMed

Sandhya, Soolamkandath Variem; Kiran, Kumar; Kuttiraja, Mathiyazhakan; Preeti, Varghese Elizabeth; Sindhu, Raveendran; Vani, Sankar; Kumar, Sukumaran Rajeev; Pandey, Ashok; Binod, Parameswaran

2013-11-01

Production of fuel ethanol from lignocellulosic biomass conventionally includes biomass pretreatment, hydrolysis, and fermentation. The liquor generated during dilute acid pretreatment of biomass contains considerable quantities of pentose sugars as well as various degradation products of sugars and lignin, like furfural, hydroxymethyl furfural (HMF), organic acids, aldehydes and others, which are known to be inhibitory for microbial growth. This pentose rich liquor is a potent resource which can be used to produce alcohol or other value added metabolites by microbial fermentation. However, the presence of these inhibitory compounds is a major hindrance and their removal is essential for efficient utilization of this byproduct stream. In the present work, the polymeric adsorbent resins, XAD-4, XAD-7 and XAD-16 were evaluated for their ability to adsorb fermentation inhibitors like furfural and HMF from the acid pretreated liquor. These resins could remove 55-75% of furfural and 100% of HMF and more than 90% sugar remained un-adsorbed in the pretreated liquor. Desorption of furfural from stationary phase was evaluated by using ethanol and hot water. The results suggest that these polymeric resins may be used for detoxification of acid pretreatment liquor with selective removal of sugar degradation products without affecting the sugar content in the solution.

Methods development for separation of inorganic anions, organic acids and bases, and neutral organic compounds by ion chromatography and capillary electrophoresis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jie

1999-04-01

A novel anion-exchange resin containing three amine groups was prepared by reaction of a chloromethylated polystyrene-divinylbenzene (PS-DVB) resin with diethylenetriamine. After being protonated by contact with an aqueous acid, this resin can be used for ion chromatographic separation of anions. The charge on the resins can be varied from +1 to +3 by changing the mobile phase pH. The selectivity of the new ion exchangers for various inorganic anions was quite different from that of conventional anion exchangers. The performance of this new anion exchanger was studied by changing the pH and the concentration of the eluent, and several differentmore » eluents were used with some common anions as testing analytes. Conductivity detection and UV-visible detection were applied to detect the anions after separation. The new resin can also be used for HPLC separation of neutral organic compounds. Alkylphenols and alkylbenzenes were separated with this new polymeric resin, and excellent separations were obtained under simple conditions. This report contains Chapter 1: General introduction and Chapter 6: General conclusions.« less

Surface roughness of composite resins subjected to hydrochloric acid.

PubMed

Roque, Ana Carolina Cabral; Bohner, Lauren Oliveira Lima; de Godoi, Ana Paula Terossi; Colucci, Vivian; Corona, Silmara Aparecida Milori; Catirse, Alma Blásida Concepción Elizaur Benitez

2015-01-01

The purpose of this study was to determine the influence of hydrochloric acid on surface roughness of composite resins subjected to brushing. Sixty samples measuring 2 mm thick x 6 mm diameter were prepared and used as experimental units. The study presented a 3x2 factorial design, in which the factors were composite resin (n=20), at 3 levels: microhybrid composite (Z100), nanofilled composite (FiltekTM Supreme), nanohybrid composite (Ice), and acid challenge (n=10) at 2 levels: absence and presence. Acid challenge was performed by immersion of specimens in hydrochloric acid (pH 1.2) for 1 min, 4 times per day for 7 days. The specimens not subjected to acid challenge were stored in 15 mL of artificial saliva at 37 oC. Afterwards, all specimens were submitted to abrasive challenge by a brushing cycle performed with a 200 g weight at a speed of 356 rpm, totaling 17.8 cycles. Surface roughness measurements (Ra) were performed and analyzed by ANOVA and Tukey test (p≤0.05). Surface roughness values were higher in the presence (1.07±0.24) as compared with the absence of hydrochloric acid (0.72±0.04). Surface roughness values were higher for microhybrid (1.01±0.27) compared with nanofilled (0.68 ±0.09) and nanohybrid (0.48±0.15) composites when the specimens were not subjects to acid challenge. In the presence of hydrochloric acid, microhybrid (1.26±0.28) and nanofilled (1.18±0,30) composites presents higher surface roughness values compared with nanohybrid (0.77±0.15). The hydrochloric acid affected the surface roughness of composite resin subjected to brushing.

Brown Algae Padina sanctae-crucis Børgesen: A Potential Nutraceutical

PubMed Central

Nogueira, Raquel B. S. S.; Tomaz, Anna Cláudia A.; Pessoa, Déborah R.; Xavier, Aline L.; Pita, João Carlos L. R.; Sobral, Marianna V.; Pontes, Marcela L. C.; Pessôa, Hilzeth L. F.; Diniz, Margareth F. F. M.; Miranda, George Emmanuel C.; Vieira, Maria Aparecida R.; Marques, Marcia O. M.; Souza, Maria de Fátima V.; Cunha, Emídio V. L.

2017-01-01

Padina sanctae-crucis Børgesen is distributed worldwide in tropical and subtropical seas; belongs to the Dictyotaceae family, and has proven to be an exceptional source of biologically active compounds. Four compounds were isolated and identified, namely: dolastane diterpene new for the genus Padina; phaeophytin and hidroxy-phaeophytin new for the family Dictyotaceae, and; mannitol first described in this species. Saturated fatty acids as compared to the percentages of unsaturated fatty acids were shown to be present in greater abundance. Palmitic and linolenic acid were the main saturated and unsaturated acids, respectively. Cytotoxic and antioxidant activities were evaluated using human erythrocytes. In vivo evaluations of acute toxicity and genotoxicity were performed in mice. Methanolic extract of P. sanctae-crucis presented antioxidant activity and did not induce cytotoxicity, genotoxicity or acute toxicity. Since Padina sanctae-crucis is already used as food, has essential fatty acids for the nutrition of mammals, does not present toxicity and has antioxidant activity, it can be considered as a potential nutraceutical. PMID:28954390

Phytotoxic activity of Salvia x jamensis.

PubMed

Bisio, Angela; Fraternale, Daniele; Damonte, Gianluca; Millo, Enrico; Lanteri, Anna Paola; Russo, Eleonora; Romussi, Giovanni; Parodi, Brunella; Ricci, Donata; De Tommasi, Nunziatina

2009-12-01

A study has been carried out on the surface exudate of Salvia x jamensis, which showed a significant phytotoxic activity against Papaver rhoeas L. and Avena sativa L.. Bioguided separation of the exudate yielded active fractions from which 3 beta-hydroxy-isopimaric acid (1), hautriwaic acid (2), betulinic acid (3), 7,8 beta-dihydrosalviacoccin (4), isopimaric acid (5), 14 alpha-hydroxy-isopimaric acid (7), 15,16-epoxy-7 alpha, 10 beta-dihydroxy-clerod-3,13(16),14-trien-17,12;18,19-diolide (8), cirsiliol (5,3',4'-trihydroxy-6,7-dimethoxyflavone, 9) and two new neoclerodane diterpenes (6 and 10) were isolated. The structures of 6 and 10 were identified as 15,16-epoxy-10 beta-hydroxy-clerod-3,13(16),14-trien-17,12;18,19-diolide and 15,16-epoxy-7 alpha,10-dihydroxy-clerod-2,13(16),14-trien-17,12;18,19-diolide respectively on the basis of spectroscopic data analysis. All compounds, but 7, 8 and 10, were active in inhibiting the germination of the tested species.

Determining resin/fiber content of laminates

NASA Technical Reports Server (NTRS)

Garrard, G. G.; Houston, D. W.

1979-01-01

Article discusses procedure where hydrazine is used to extract graphite fibers from cured polyimide resin. Method does not attack graphite fibers and is faster than hot-concentrated-acid digestion process.

A new configuration of membrane stack for retrieval of nickel absorbed in resins*

PubMed Central

Chen, Xue-fen; Wu, Zu-cheng

2005-01-01

A new configuration integrated ion exchange effect with both electro-migration and electrochemical reaction in a single cell was developed to effectively retrieve metal ions from simulated wastewater using ion exchange resins without additive chemicals. By simply assembling cation exchange resins and anion exchange resins separated by homogeneous membranes, we found that the system will always be acidic in the concentrate compartment so that ion exchange resins could be in-situ regenerated without hydroxide precipitation. Such a realizable design will be really suitable for wastewater purification. PMID:15909341

Resin-Bound Crypto-Thioester for Native Chemical Ligation.

PubMed

Naruse, Naoto; Ohkawachi, Kento; Inokuma, Tsubasa; Shigenaga, Akira; Otaka, Akira

2018-04-20

The resin-bound N-sulfanylethylanilide (SEAlide) peptide was found to function as a crypto-thioester peptide. Exposure of the peptide resin to an aqueous solution under neutral conditions in the presence of thiols affords thioesters without accompanying racemization of C-terminal amino acids. Furthermore, the resin-bound SEAlide peptides react with N-terminal cysteinyl peptides in the absence of phosphate salts to afford ligated products, whereas soluble SEAlide peptides do not. This unexpected difference in reactivity of the SEAlide peptides allows for a one-pot/three-fragment ligation using resin-bound and unbound peptides.

Effect of surface treatment methods on the shear bond strength of auto-polymerized resin to thermoplastic denture base polymer.

PubMed

Koodaryan, Roodabeh; Hafezeqoran, Ali

2016-12-01

Polyamide polymers do not provide sufficient bond strength to auto-polymerized resins for repairing fractured denture or replacing dislodged denture teeth. Limited treatment methods have been developed to improve the bond strength between auto-polymerized reline resins and polyamide denture base materials. The objective of the present study was to evaluate the effect of surface modification by acetic acid on surface characteristics and bond strength of reline resin to polyamide denture base. 84 polyamide specimens were divided into three surface treatment groups (n=28): control (N), silica-coated (S), and acid-treated (A). Two different auto-polymerized reline resins GC and Triplex resins were bonded to the samples (subgroups T and G, respectively, n=14). The specimens were subjected to shear bond strength test after they were stored in distilled water for 1 week and thermo-cycled for 5000 cycles. Data were analyzed with independent t-test, two-way analysis of variance (ANOVA), and Tukey's post hoc multiple comparison test (α=.05). The bond strength values of A and S were significantly higher than those of N ( P <.001 for both). However, statistically significant difference was not observed between group A and group S. According to the independent Student's t-test, the shear bond strength values of AT were significantly higher than those of AG ( P <.001). The surface treatment of polyamide denture base materials with acetic acid may be an efficient and cost-effective method for increasing the shear bond strength to auto-polymerized reline resin.

Control of resin production in Araucaria angustifolia, an ancient South American conifer.

PubMed

Perotti, J C; da Silva Rodrigues-Corrêa, K C; Fett-Neto, A G

2015-07-01

Araucaria angustifolia is an ancient slow-growing conifer that characterises parts of the Southern Atlantic Forest biome, currently listed as a critically endangered species. The species also produces bark resin, although the factors controlling its resinosis are largely unknown. To better understand this defence-related process, we examined the resin exudation response of A. angustifolia upon treatment with well-known chemical stimulators used in fast-growing conifers producing both bark and wood resin, such as Pinus elliottii. The initial hypothesis was that A. angustifolia would display significant differences in the regulation of resinosis. The effect of Ethrel(®) (ET - ethylene precursor), salicylic acid (SA), jasmonic acid (JA), sulphuric acid (SuA) and sodium nitroprusside (SNP - nitric oxide donor) on resin yield and composition in young plants of A. angustifolia was examined. In at least one of the concentrations tested, and frequently in more than one, an aqueous glycerol solution applied on fresh wound sites of the stem with one or more of the adjuvants examined promoted an increase in resin yield, as well as monoterpene concentration (α-pinene, β-pinene, camphene and limonene). Higher yields and longer exudation periods were observed with JA and ET, another feature shared with Pinus resinosis. The results suggest that resinosis control is similar in Araucaria and Pinus. In addition, A. angustifolia resin may be a relevant source of valuable terpene chemicals, whose production may be increased by using stimulating pastes containing the identified adjuvants. © 2014 German Botanical Society and The Royal Botanical Society of the Netherlands.

Effect of surface treatments on the bond strength of soft denture lining materials to an acrylic resin denture base.

PubMed

Gundogdu, Mustafa; Yesil Duymus, Zeynep; Alkurt, Murat

2014-10-01

Adhesive failure between acrylic resin and resilient liner material is commonly encountered in clinical practice. The purpose of this study was to evaluate the effect of different surface treatments on the bond strength of 2 different resilient lining materials to an acrylic resin denture base. Ninety-six dumbbell-shaped specimens were fabricated from heat-polymerized acrylic resin, and 3 mm of the material was cut from the thin midsection. The specimens were divided into 6 groups according to their surface treatments: no surface treatment (control group), 36% phosphoric acid etching (acid group), erbium:yttrium-aluminum-garnet (Er:YAG) laser (laser group), airborne-particle abrasion with 50-μm Al2O3 particles (abrasion group), an acid+laser group, and an abrasion+laser group. The specimens in each group were divided into 2 subgroups according to the resilient lining material used: heat-polymerized silicone based resilient liner (Molloplast B) and autopolymerized silicone-based resilient liner (Ufi Gel P). After all of the specimens had been polymerized, they were stored in distilled water at 37°C for 1 week. A tensile bond strength test was then performed. Data were analyzed with a 2-way ANOVA, and the Sidak multiple comparison test was used to identify significant differences (α=.05). The effects of the surface treatments and resilient lining materials on the surface of the denture base resin were examined with scanning electron microscopy. The tensile bond strength was significantly different between Molloplast B and Ufi Gel P (P<.001). The specimens of the acid group had the highest tensile bond strength, whereas those of the abrasion group had the lowest tensile bond strength. The scanning electron microscopy observations showed that the application of surface treatments modified the surface of the denture base resin. Molloplast B exhibited significantly higher bond strength than Ufi Gel P. Altering the surface of the acrylic resin denture base with 36% phosphoric acid etching increased bond strength. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Gersemiols A-C and Eunicellol A, Diterpenoids from the Arctic Soft Coral Gersemia fruticosa.

PubMed

Angulo-Preckler, Carlos; Genta-Jouve, Grégory; Mahajan, Nipun; de la Cruz, Mercedes; de Pedro, Nuria; Reyes, Fernando; Iken, Katrin; Avila, Conxita; Thomas, Olivier P

2016-04-22

Three new diterpenes named gersemiols A-C (1-3) and a new eunicellane diterpene, eunicellol A (4), have been isolated together with the known sesquiterpene (+)-α-muurolene (5) from the Arctic soft coral Gersemia fruticosa. The name gersemiane was assigned to the rare and unnamed diterpene skeleton of compounds 1-3 corresponding to 4-isopropyl-1,5,8a-trimethyltetradecahydrophenanthrene. The chemical structures were elucidated on the basis of extensive spectroscopic analysis (HR-ESIMS, 1D and 2D NMR) as well as coupling constant calculations for the determination of the relative configurations. All compounds were tested for their antimicrobial activity against several bacteria and fungi and eunicellol A was found to exhibit moderate and selective antibacterial activity.

Bacterial Diterpene Synthases: New Opportunities for Mechanistic Enzymology and Engineered Biosynthesis

PubMed Central

Smanski, Michael J.; Peterson, Ryan M.; Huang, Sheng-Xiong; Shen, Ben

2012-01-01

Diterpenoid biosynthesis has been extensively studied in plants and fungi, yet cloning and engineering diterpenoid pathways in these organisms remain challenging. Bacteria are emerging as prolific producers of diterpenoid natural products, and bacterial diterpene synthases are poised to make significant contributions to our understanding of terpenoid biosynthesis. Here we will first survey diterpenoid natural products of bacterial origin and briefly review their biosynthesis with emphasis on diterpene synthases (DTSs) that channel geranylgeranyl diphosphate to various diterpenoid scaffolds. We will then highlight differences of DTSs of bacterial and higher organism origins and discuss the challenges in discovering novel bacterial DTSs. We will conclude by discussing new opportunities for DTS mechanistic enzymology and applications of bacterial DTS in biocatalysis and metabolic pathway engineering. PMID:22445175

A novel conversion of C(19)-diterpenoid alkaloids into aconane-type diterpenes with eight-membered ring system via skeletal rearrangement of corresponding diazonium derivatives.

PubMed

Ji, Hong; Chen, Qiao-Hong; Wang, Feng-Peng

2009-03-01

A new and efficient approach toward the conversion of C(19)-diterpenoid alkaloids into diterpenes with [6+8+5+6] ring system is reported. Treatment of imines 5, 14, and 24 derived from the C(19)-diterpenoid alkaloids with NaNO(2)-NaOAc-HOAc afforded a series of novel rearrangement diterpenes 6-8, 15-19, and 25-27, respectively. The lactone 11 was obtained in 41% yield by treating 5 with NaNO(2)-HBr-Br(2). The formation of diazonium intermediate is postulated, which was subsequently subjected to skeletal rearrangement, leading to the enlargement of B ring. All the new compounds were isolated and fully characterized.

Technology development for phosphoric acid fuel cell powerplant, phase 2

NASA Technical Reports Server (NTRS)

Christner, L.

1979-01-01

A technique for producing an acid inventory control member by spraying FEP onto a partially screened carbon paper backing is discussed. Theoretical analysis of the acid management indicates that the vapor composition of 103% H3PO4 is approximately 1.0 ppm P4O10. An SEM evaluation of corrosion resistance of phenolic resins and graphite/phenolic resin composites in H3PO4 at 185 C shows specific surface etching. Carbonization of graphite/phenolic bipolar plates is achieved without blistering.

The effect of diamic acid additives on the dielectric constant of polyimides

NASA Technical Reports Server (NTRS)

Stoakley, Diane M.; St. Clair, Anne K.

1988-01-01

The effect of six selected diamic acids additives (including 2,2-prime bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride-aniline (An); 4,4-prime-oxydiphthalic anhydride-An, 3,3-prime diaminodiphenyl sulfone-phthalic anhydride (PA); 4,4-prime-oxydianiline-PA; 2,2-bis 4(4-aminophenoxy)phenyl hexafluoropropane-PA; and 2,2-bis 4(3-aminophenoxy)phenyl hexafluoropropane-PA) on the dielectric constants of low-dielectric-constant polyimide resins was evaluated. It was found that the effect of the incorporation of the diamic acids on reducing the dielectric constant of polyimides may be limited as the dielectric constant of the base resin itself becomes very low. The additives were found to lower the resin's values of glass transition temperature, with no effect on thermooxidative stability.

Commercial Ion Exchange Resin Vitrification in Borosilicate Glass

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cicero-Herman, C.A.; Workman, P.; Poole, K.

1998-05-01

Bench-scale studies were performed to determine the feasibility of vitrification treatment of six resins representative of those used in the commercial nuclear industry. Each resin was successfully immobilized using the same proprietary borosilicate glass formulation. Waste loadings varied from 38 to 70 g of resin/100 g of glass produced depending on the particular resin, with volume reductions of 28 percent to 68 percent. The bench-scale results were used to perform a melter demonstration with one of the resins at the Clemson Environmental Technologies Laboratory (CETL). The resin used was a weakly acidic meth acrylic cation exchange resin. The vitrification processmore » utilized represented a approximately 64 percent volume reduction. Glass characterization, radionuclide retention, offgas analyses, and system compatibility results will be discussed in this paper.« less

Comparing the variation of needle and wood terpenoids in Scots pine provenances.

PubMed

Manninen, A M; Tarhanen, S; Vuorinen, M; Kainulaine, P

2002-01-01

We determined variation in both the concentration and composition of terpenoids in needles and wood within nine Scots pine (Pinus sylvestris) provenances. Seedlings of different provenances representing a 1200-km N-S transect from Estonia to northern Finland were cultivated in Suonenjoki nursery field, central Finland, for seven years. Growth of seedlings and the number of vertical resin ducts in wood were also determined. alpha-Pinene and 3-carene were the major monoterpenes both in the needles and wood. The total monoterpene concentration was about five times higher in the needles than in the wood. A strong positive correlation was found between proportional quantities of several terpenes of the needles and wood, particularly for 3-carene, sabinene, and terpinolene. The needles contained both labdane-type and tricyclic resin acids, whereas the wood contained only tricyclic ones. The wood had a four times higher tricyclic resin acid concentration than the needles. The highest total monoterpene concentration in the needles and in the wood occurred in the most northern Muonio provenance and in the most southern Saaremaa provenance plants, respectively. The amount of high 3-carene genotype trees decreased among the northern provenances. The wood of the most northern Muonio provenance showed the lowest total resin acid concentration, but provenance did not affect total tricyclic resin acids in the needles. Korpilahti provenance trees from central Finland had the best growth in height. In addition, Korpilahti and Ruokolahti provenance trees showed largest radial growth of stem and smallest number of vertical resin ducts. The results suggest that especially the proportional quantity of 3-carene in the needles could be used in estimating the amount of this compound in the wood and vice versa.

Characterization of an anti-tuberculosis resin glycoside from the prairie medicinal plant Ipomoea leptophylla.

PubMed

Barnes, Curtis C; Smalley, Mary K; Manfredi, Kirk P; Kindscher, Kelly; Loring, Hillary; Sheeley, Douglas M

2003-11-01

The organic soluble extract from the leaves of the native North American prairie plant Ipomoea leptophylla (big root morning glory) showed in vitro activity against M. tuberculosis. Bioassay-guided fractionation of this extract resulted in the identification of two new resin glycosides (6, 7). Base-catalyzed hydrolysis of these glycosides gave operculinic acid (1) as the glycosidic acid component as well as trans-cinnamic acid, propanoic acid, and lauric acid. The complete structure elucidation was accomplished through derivatization, 1D and 2D NMR spectroscopy (TOCSY, ROESY, HSQC, HMBC), and MS/MS experiments on 6 and 7 as well as the permethylated derivative 8.

[Study of purity tests for silicone resins].

PubMed

Sato, Kyoko; Otsuki, Noriko; Ohori, Akio; Chinda, Mitsuru; Furusho, Noriko; Osako, Tsutomu; Akiyama, Hiroshi; Kawamura, Yoko

2012-01-01

In the 8th edition of Japan's Specifications and Standards for Food Additives, the purity test for silicone resins requires the determination of the refractive index and kinetic viscosity of the extracted silicone oil, and allows for only a limited amount of silicon dioxide. In the purity test, carbon tetrachloride is used to separate the silicone oil and silicon dioxide. To exclude carbon tetrachloride, methods were developed for separating the silicone oil and silicon dioxide from silicone resin, which use hexane and 10% n-dodecylbenzenesulfonic acid in hexane. For silicone oil, the measured refractive index and kinetic viscosity of the silicone oil obtained from the hexane extract were shown to be equivalent to those of the intact silicone oil. In regard to silicon dioxide, it was confirmed that, following the separation with 10% n-dodecylbenzenesulfonic acid in hexane, the level of silicon dioxide in silicone resin can be accurately determined. Therefore, in this study, we developed a method for testing the purity of silicone resins without the use of carbon tetrachloride, which is a harmful reagent.

The management of defective resin composite restorations: current trends in dental school teaching in Japan.

PubMed

Lynch, C D; Hayashi, M; Seow, L L; Blum, I R; Wilson, N H F

2013-01-01

The aim of this article is to investigate the contemporary teaching of the management of defective direct resin composite restorations in dental schools in Japan. A questionnaire relating to the teaching of the management of defective resin composite restorations was developed and e-mailed to 29 dental schools in Japan in 2010. Completed responses were received from 19 of the 29 invited schools (response rate = 66%). Eighteen schools (95%) report that they included the teaching of repair of direct defective resin composite restorations in their dental school programs. Thirteen schools reported that they included both clinical and didactic instruction on the repair of direct resin composite restorations. Fourteen schools did not teach any mechanical roughening of the exposed resin composite restoration surface before undertaking a repair. The most commonly reported treatment was acid etching with phosphoric acid (12 schools). The most commonly taught material for completing repairs was a flowable resin composite (16 schools). The teaching of repair of defective resin composite restorations is well established within many Japanese dental schools, to a greater extent than in some other regions of the world. The impact of this teaching on subsequent clinical practices in Japan should be investigated. Furthermore, it is concluded that there is a need for much stronger leadership in operative and conservative dentistry, ideally at the global level, to resolve differences in key aspects of operative procedures such as repairs.

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

21 CFR 177.1655 - Polysulfone resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

...)(2) of this section. (c) Polysulfone resins, when extracted at reflux temperatures for 6 hours with... acetic acid in distilled water, and n-heptane, yield total extractives in each extracting solvent not to...

ADSORPTION METHOD FOR SEPARATING THORIUM VALUES FROM URANIUM VALUES

DOEpatents

Boyd, G.E.; Russell, E.R.; Schubert, J.

1959-08-01

An improved ion exchange method is described for recovery of uranium and thorium values as separate functions from an aqueous acidic solution containing less than 10/sup -3/ M thorium ions and between 0.1 and 1 M uranyl ions. The solution is passed through a bed of cation exchange resin in the acid form to adsorb all the thorium ions and a portion of the uranyl ions. The uranium is eluted by means of aqueous 0.1 to 0.4 M sulfuric acid. The thorium may then be stripped from the resin by elution with aqueous 0.5 M oxalic acid.

ADSORPTION METHOD FOR SEPARATING THORIUM VALUES FROM URANIUM VALUES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boyd, G.E.; Russell, E.R.; Schubert, J.

An improved ion exchange method is described for recovery of uranium and thorium values as separate functions from an aqueous acidic solution containing less than 10/sup -3/ M thorium ions and between 0.1 and 1 M uranyl ions. The solution is passed through a bed of cation exchange resin in the acid form to adsorb all the thorium ions and a portion of the uranyl ions. The uranium is eluted by means of aqueous 0.1 to 0.4 M sulfuric acid. The thorium may then be stripped from the resin by elution with aqueous 0.5 M oxalic acid.

Self-etching adhesive on intact enamel, with and without pre-etching.

PubMed

Devarasa, G M; Subba Reddy, V V; Chaitra, N L; Swarna, Y M

2012-05-01

Bond strengths of composite resin to enamel using self-etch adhesive (SEA) Clearfil SE bond system on intact enamel and enamel pre-etched with phosphoric acid were compared. The objective was to determine if the pre-etching would increase the bond strengths of the SEA systems to intact enamel and to evaluate the effect of pre-etching on bond formation of self-etch adhesives on intact enamel. Labial surfaces of 40 caries free permanent upper central and lateral incisors were cleaned, sectioned of their roots. All specimens were mounted on acrylic block and divided randomly into four groups. In two groups the application of self-etch adhesive, Clearfil SE bond was carried as per manufacturer's instructions, composite cylinders were built, whereas in the other two groups, 37% phosphoric acid etching was done before the application of self-etching adhesives. Then the resin tags were analyzed using scanning electron microscope and shear bond strength was measured using Instron universal testing machine. When phosphoric acid was used, there was significant increase in the depth of penetration of resin tags and in the Shear Bond Strength of composite to enamel. The results indicate that out of both treatment groups, pre-etching the intact enamel with 37% phosphoric acid resulted in formation of longer resin tags and higher depth of penetration of resin tags of the Clearfil SE bond, and attaining higher bond strength of the Clearfil SE bond to intact enamel. Copyright © 2011 Wiley Periodicals, Inc.

Preparation of an amphiphilic resin-supported BINAP ligand and its use for rhodium-catalyzed asymmetric 1,4-addition of phenylboronic acid in water.

PubMed

Otomaru, Yusuke; Senda, Taichi; Hayashi, Tamio

2004-09-16

[reaction: see text] The axially chiral bisphosphine ligand, 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (binap), was supported on a polystyrene-poly(ethylene glycol) copolymer (PS-PEG) resin and was used successfully for the rhodium-catalyzed asymmetric 1,4-addition of phenylboronic acid to alpha,beta-unsaturated ketones in water.

Analysis of Commercial Unsaturated Polyester Repair Resins

DTIC Science & Technology

2009-07-01

resins utilizing renewable fatty acid -based monomers. 15. SUBJECT TERMS vinyl ester, styrene, fatty acid monomers, HAP, triglycerides 16. SECURITY...criteria for selecting the appropriate repair include whether the component can be removed and whether the back side is accessible. For a typical moderate...field repair, any remaining coating in the repair area is removed by hand sanding or portable tools. Damage is cut out in an appropriate

SPPS of protected peptidyl aminoalkyl amides.

PubMed

Karavoltsos, Manolis; Mourtas, Spyros; Gatos, Dimitrios; Barlos, Kleomenis

2002-11-01

Monophthaloyl diamines derived from naturally occurring amino acids were attached through their free amino functions to resins of the trityl type. The phthaloyl groups were removed by hydrazinolysis, and peptide chains were assembled using Fmoc/tBu-amino acids on the liberated amino functions. The peptidyl aminoalkyl amides obtained were cleaved from the resins by mild acidolysis, with the tBu-side chain protection remaining intact.

Improved bonding of adhesive resin to sintered porcelain with the combination of acid etching and a two-liquid silane conditioner.

PubMed

Kato, H; Matsumura, H; Ide, T; Atsuta, M

2001-01-01

This study determined the bond strengths of adhesive resins joined to a feldspathic porcelain (VMK 68) for the purpose of developing the most durable surface preparation for the porcelain. Three porcelain surfaces-ground, air-abraded with alumina, and etched with hydrofluoric acid-were prepared. A two-liquid porcelain conditioner that contained both 4-methacryloyloxyethyl trimellitate anhydride (4-META) and a silane coupler (Porcelain Liner M) was used as the priming agent. Each of the two liquid components of the conditioner was also used individually in order to examine the effects of the respective chemical ingredients on adhesive bonding. Two methyl methacrylate (MMA)-based resins initiated with tri-n-butylborane (TBB) either with or without 4-META (MMA-TBB and 4-META/MMA-TBB resins) were used as the luting agents. Shear bond strengths were determined both before and after thermocycling. Shear testing results indicated that thermocycling was effective for disclosing poor bonding systems, and that both mechanical and chemical retention were indispensable for bonding the porcelain. Of the combinations assessed, etching with hydrofluoric acid followed by two-liquid priming with the Porcelain Liner M material generated the most durable bond strength (33.3 MPa) for the porcelain bonded with the 4-META/MMA-TBB resin (Super-Bond C&B).

The nature and fate of natural resins in the geosphere. XII. Investigation of C-ring aromatic diterpenoids in Raritan amber by pyrolysis-GC-matrix isolation FTIR-MS

PubMed Central

Anderson, Ken B

2006-01-01

Upper Cretaceous amber from the Raritan Formation (Sayerville, New Jersey) has been investigated by Pyrolysis-GC-MS and Pyrolysis-GC-matrix isolation FTIR-MS. Results establish the existence of two distinct forms of amber in this deposit. Both forms are Class Ib ambers, but they are unambiguously differentiated on the basis of their (intact) diterpenoid composition. The presence of callitrisate in both forms, and cupraene in samples designated form 1, strongly suggest that both derive from related-but-distinct species within the Cupressaceae. In addition to callitrisate, dehydroabietate and analogous 17-nor-, 16,17-dinor- and 15,16,17-trinor- analogues of these compounds are also observed. The distributions of these products in multiple samples suggest that they are the result of biological emplacement, rather than diagenetic modification of the parent compounds. This indicates that the distributions of diterpenes observed in these samples are representative of the original bioterpenoids and, hence, are useful for chemotaxonomic analyses. PMID:16759406

Tetracyclic diterpenoid hydrocarbons in some Australian coals, sediments and crude oils

NASA Astrophysics Data System (ADS)

Noble, Rohinton A.; Alexander, Robert; Kagi, Robert Ian; Knox, John

1985-10-01

Tetracyclic diterpenoid hydrocarbons (diterpanes) based on the ent-beyerane, phyllocladane and ent-kaurane skeletons have been identified in the hydrocarbon extracts of some Australian coals, sediments and crude oils. Structures were assigned to the geological diterpanes by comparison with synthetically prepared reference compounds. Studies of a sample suite consisting of low-rank coals and sediments indicate that the ratios of C-16 epimers of phyllocladane and ent-kaurane are maturity dependent, and that the relative proportion of the thermodynamically preferred 16β (H)-compounds increases with increasing thermal maturity. Thermodynamic equilibrium for the interconversion reactions is attained in sediments before the onset of crude oil generation. The most likely natural product precursors for the tetracyclic diterpanes are considered to be the tetracyclic diterpene hydrocarbons which occur widely in the leaf resins of conifers. Tetracyclic diterpanes have been identified in sediments and coals of Permian age or younger, suggesting that these compounds are markers for both modern and extinct families of conifers. In particular, phyllocladane is proposed as a marker for the Podocarpaceae family of conifers.

Analgesic activity of diterpene alkaloids from Aconitum baikalensis.

PubMed

Nesterova, Yu V; Povet'yeva, T N; Suslov, N I; Zyuz'kov, G N; Pushkarskii, S V; Aksinenko, S G; Schultz, E E; Kravtsova, S S; Krapivin, A V

2014-08-01

We compared analgesic activities of individual alkaloids extracted from Baikal aconite (Aconitum baikalensis): napelline, hypaconitine, songorine, mesaconitine, 12-epinapelline N-oxide. The detected analgesic activity was comparable to that of sodium metamizole. The mechanisms of analgesia were different in diterpene alkaloids of different structure. The antinociceptive effect of atisine alkaloids (12-epinapelline N-oxide, songorine) was naloxonedependent and realized via opioid receptor modulation.

Lolitrem B and Indole Diterpene Alkaloids Produced by Endophytic Fungi of the Genus Epichloë and Their Toxic Effects in Livestock.

PubMed

Philippe, Guerre

2016-02-15

Different group of alkaloids are produced during the symbiotic development of fungal endophytes of the genus Epichloë in grass. The structure and toxicity of the compounds vary considerably in mammalian herbivores and in crop pests. Alkaloids of the indole-diterpene group, of which lolitrem B is the most toxic, were first characterized in endophyte-infected perennial ryegrass, and are responsible for "ryegrass staggers." Ergot alkaloids, of which ergovaline is the most abundant ergopeptide alkaloid produced, are also found in ryegrass, but generally at a lower rate than lolitrem B. Other alkaloids such as lolines and peramine are toxic for crop pests but have weak toxicological properties in mammals. The purpose of this review is to present indole-diterpene alkaloids produced in endophyte infected ryegrass from the first characterization of ryegrass staggers to the determination of the toxicokinetics of lolitrem B and of their mechanism of action in mammals, focusing on the different factors that could explain the worldwide distribution of the disease. Other indole diterpene alkaloids than lolitrem B that can be found in Epichloë infected ryegrass, and their tremorgenic properties, are presented in the last section of this review.

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... consist of basic resin produced by reacting polyphenylene sulfide with peracetic acid such that the... sanction or approval. (c) Specifications. The glass transition temperature of the polymer is 360±5 °C as...

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... consist of basic resin produced by reacting polyphenylene sulfide with peracetic acid such that the... sanction or approval. (c) Specifications. The glass transition temperature of the polymer is 360±5 °C as...

Rechargeable infection-responsive antifungal denture materials.

PubMed

Cao, Z; Sun, X; Yeh, C-K; Sun, Y

2010-12-01

Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be "washed out" by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions.

Low-Melt Polyamic Acid Based Powder Coatings

NASA Technical Reports Server (NTRS)

Jolley, Scott T. (Inventor)

2017-01-01

The present invention is directed to a method for powder coating a metal substrate using a low-melt polyamic acid (PAA) polymer that readily imidizes to polyimides. These low-melt PAAs have been shown to be useful in resins applied as powder coatings to metal surfaces. The resin includes an end-capping material capable of providing crosslinking functionality to at least one end of the low-melt PAA polymer. The end-capping material functions dually as a polymerization chain terminator and crosslinking agent, thus producing resins that have molecular weights low enough to flow well and form good cured films applicable for use in powder coating.

ION EXCHANGE ADSORPTION PROCESS FOR PLUTONIUM SEPARATION

DOEpatents

Boyd, G.E.; Russell, E.R.; Taylor, M.D.

1961-07-11

Ion exchange processes for the separation of plutonium from fission products are described. In accordance with these processes an aqueous solution containing plutonium and fission products is contacted with a cation exchange resin under conditions favoring adsorption of plutonium and fission products on the resin. A portion of the fission product is then eluted with a solution containing 0.05 to 1% by weight of a carboxylic acid. Plutonium is next eluted with a solution containing 2 to 8 per cent by weight of the same carboxylic acid, and the remaining fission products on the resin are eluted with an aqueous solution containing over 10 per cent by weight of sodium bisulfate.

Purification of organic acids by chromatography with strong anionic resins: Investigation of uptake mechanisms.

PubMed

Lemaire, Julien; Blanc, Claire-Line; Lutin, Florence; Théoleyre, Marc-André; Stambouli, Moncef; Pareau, Dominique

2016-08-05

Bio-based organic acids are promising renewable carbon sources for the chemical industry. However energy-consuming purification processes are used, like distillation or crystallization, to reach high purities required in some applications. That is why preparative chromatography was studied as an alternative separation technique. In a previous work dealing with the purification of lactic, succinic and citric acids, the Langmuir model was insufficient to explain the elution profiles obtained with a strong anionic resin. Consequently the Langmuir model was coupled with a usual ion-exchange model to take into account the retention of their conjugate bases (<2%), which are commonly neglected at low pH (<1.5). Elution simulations with both uptake mechanisms fitted very well with experimental pulse tests. Only two parameters were optimized (equilibrium constant of acid uptake and ion-exchange selectivity coefficient of conjugate base) and their value were coherent with experimental and resin suppliers' data. These results confirmed that the singular tailing and apparent delay observed with succinic and citric acids can be explained by the high affinity of succinate and citrate for resin cationic sites. The model was implemented in a preparative chromatography simulation program in order to optimize operating parameters of our pilot-scale ISMB unit (Improved Simulated Moving Bed). The comparison with experimental ISMB profiles was conclusive. Copyright © 2016 Elsevier B.V. All rights reserved.

Secondary metabolite concentrations and terpene emissions of Scots pine xylem after long-term forest fertilization.

PubMed

Turtola, S; Manninen, A M; Holopainen, J K; Levula, T; Raitio, H; Kainulainen, P

2002-01-01

Secondary compounds are known to be associated with the resistance of conifer xylem against insects and fungi. The effects of long-term forest fertilization with nitrogen (N) or with N, calcium (Ca), and phosphorus (P) on secondary compounds in the xylem of 50-yr-old Scots pine (Pinus sylvestris L.) trees were examined. Xylem samples were collected from trees growing in three locations in southern Finland: Vilppula, Padasjoki, and Punkaharju. Forests were fertilized every fifth (Vilppula and Padasjoki) or tenth (Punkaharju) year since the 1950s. We compared concentrations of individual and total monoterpenes and resin acids in the heartwood and sapwood of Scots pine. Terpene emissions were analyzed from the sapwood and total phenolics from the heartwood. Fertilization did not have any significant effect on the concentrations and emissions of xylem monoterpenes. Concentrations of several individual terpenes in sapwood were positively correlated with the corresponding terpene emission. The concentrations of individual resin acids (i.e., abietic and dehydroabietic) decreased significantly in Punkaharju, but increased in the sapwood of N-fertilized trees compared with control ones at Padasjoki and Vilppula. The concentrations of resin acids in the heartwood were not significantly affected by fertilization. Both fertilization treatments decreased the total phenolic concentrations in the heartwood of trees growing in Padasjoki. There was a significant positive correlation between the total phenolics and total resin acid concentration. Overall, resin acids and phenolics seemed be more responsive than monoterpenes to N treatment. These results suggest that forest fertilization might cause slight changes in secondary compound concentrations of xylem, and thus might have significance in the decay resistance of wood.

Determining efficacy of monitoring devices on ceramic bond to resin composite

PubMed Central

Osorio, Estrella; Aguilera, Fátima S.; Osorio, Raquel; García-Godoy, Franklin; Cabrerizo-Vilchez, Miguel A.; Toledano, Manuel

2012-01-01

Objectives: This paper aims to assess the effectiveness of 3D nanoroughness and 2D microroughness evaluations, by their correlation with contact angle measurements and shear bond strength test, in order to evaluate the effect of two different acids conditioning on the bonding efficacy of a leucite-based glass-ceramic to a composite resin. Study Design: Ceramic (IPS Empress) blocks were treated as follows: 1) no treatment, 2) 37% phosphoric acid (H3PO4), 15 s, 3) 9% hydrofluoric acid (HF), 5 min. Micro- and nano-roughness were assessed with a profilometer and by means of an atomic force microscopy (AFM). Water contact angle (CA) measurements were determined to assess wettability of the ceramic surfaces with the asixymetric drop shape analysis contact diameter technique. Shear bond strength (SBS) was tested to a resin composite (Z100) with three different adhesive systems (Scotchbond Multipurpose Plus, Clearfil New Bond, ProBOND). Scanning electron microscopy (SEM) images were performed. Results: Nanoroughness values assessed in 50x50 μm areas were higher for the HF group, these differences were not detected by profilometric analysis. HF treatment created the nano- roughest surfaces and the smallest CA (p<0.05), producing the highest SBS to the composite resin with all tested adhesive systems (p<0.05). No differences existed between the SBS produced by the adhesive systems evaluated with any of the surface treatments tested. Conclusions: Nano-roughness obtained in a 50x50 µm scan size areas was the most reliable data to evaluate the topographical changes produced by the different acid treatments on ceramic surfaces. Key words:Dental ceramic, acid etching, bonding efficacy, resin composite, adhesive systems, contact angle, roughness. PMID:22549693

Cardiovascular Activity of Labdane Diterpenes from Andrographis paniculata in Isolated Rat Hearts

PubMed Central

Awang, Khalijah; Abdullah, Nor Hayati; Hadi, A. Hamid A.; Su Fong, Yew

2012-01-01

The dichloromethane (DCM) extract of Andrographis paniculata Nees was tested for cardiovascular activity. The extract significantly reduced coronary perfusion pressure by up to 24.5 ± 3.0 mm Hg at a 3 mg dose and also reduced heart rate by up to 49.5 ± 11.4 beats/minute at this dose. Five labdane diterpenes, 14-deoxy-12-hydroxyandrographolide (1), 14-deoxy-11,12-didehydroandrographolide (2), 14-deoxyandrographolide (3), andrographolide (4), and neoandrographolide (5), were isolated from the aerial parts of this medicinal plant. Bioassay-guided studies using animal model showed that compounds, (2) and (3) were responsible for the coronary vasodilatation. This study also showed that andrographolide (4), the major labdane diterpene in this plant, has minimal effects on the heart. PMID:22536026

Integrated Extraction Chromatographic Separation of the Lithophile Elements Involved in Long-Lived Radiogenic Isotope Systems (Rb-Sr, U-Th-Pb, Sm-Nd, La-Ce, and Lu-Hf) Useful in Geochemical and Environmental Sciences.

PubMed

Pin, Christian; Gannoun, Abdelmouhcine

2017-02-21

A fast and efficient sample preparation method in view of isotope ratio measurements is described, allowing the separation of 11 elements involved, either as "parent" or as "daughter" isotopes, in six radiogenic isotope systems used as chronometers and tracers in earth, planetary, and environmental sciences. The protocol is based on small extraction chromatographic columns, used either alone or in tandem, through which a single nitric acid solution is passed, without any intervening evaporation step. The columns use commercially available extraction resins (Sr resin, TRU resin, Ln resin, RE resin, and again Ln resin for isolating Sr and Pb, LREE then La-Ce-Nd-Sm, Lu(Yb), and Hf, Th, and U, respectively) along with an additional, in-house prepared resin for separating Rb. A simplified scheme is proposed for samples requiring the separation of Sr, Pb, Nd, and Hf only. Adverse effects of troublesome major elements (Fe 3+ , Ti) are circumvented by masking with ascorbic acid and hydrofluoric acid, respectively. Typical recoveries in the 85-95% range are achieved, with procedural blanks of 10-100 pg, negligible with regard to the amounts of analytes processed. The fractions separated are suitable for high precision isotope ratio measurements by TIMS or MC-ICP-MS, as demonstrated by the repeat analyses of several international reference materials of basaltic composition for 87 Sr/ 86 Sr, 208,207,206 Pb/ 204 Pb, 143 Nd/ 144 Nd, 176 Hf/ 177 Hf, and 230 Th/ 232 Th. Concentration data could be obtained by spiking and equilibrating the sample with appropriate isotopic tracers before the onset of the separation process and, finally, measuring the isotope ratios modified by the isotope dilution process.

Purification of bioactive phenolics from Phanerochaete chysosporium biomass extract on selected macroporous resins

NASA Astrophysics Data System (ADS)

Idris, Z. M.; Dzahir, M. I. H. M.; Jamal, P.; Barkat, A. A.; Xian, R. L. W.

2017-06-01

In this study, two different types of macroporous resins known as XAD-7HP and HP-20 were evaluated for the adsorption and desorption properties against bioactive phenolics extracted from Phanerochaete chrysosporium. From the previous static sorption studies, it was found that the adsorption capacity for both resins had has no significant difference. Then, the kinetic adsorption data were analyzed with both pseudo-first-order and pseudo-second-order equations and the later performed better. The adsorption isotherm data were fitted well by both Langmuir and Freundlich models. Meanwhile in desorption study, HP-20 and XAD-7HP gave 90.52% and 88.28% recoveries, respectively. Considering the desorption results of the macroporous resins, HP-20 and XAD-7HP were packed in chromatography column to further purify the phenolics. For dynamic adsorption, breakthrough capacity of HP-20 (0.522) was found to be higher than XAD-7HP (0.131). Different ethanol concentrations (30% to 50% (v/v)) were investigated at fixed flowrate (1 ml/min) on phenolics recovery from both types of resins. The highest recovery of bioactive phenolics was 94.3% using XAD-7HP resins at 50% (v/v) of ethanol. Only 77.1% of bioactive phenolics were recovered using HP-20 resin at the same experimental conditions. The purified extract subsequently was analyzed using HPLC. The results showed that three phenolics (gallic acid 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid) were identified with higher concentrations as compared to non-purified extract. Finally, the purified extract was tested for scavenging activity against DPPH, and it showed that the activity increased significantly to 90.80% from 59.94% in non-purified extract.

Study on dehydrochlorination of waste poly (vinyl chloride) resins by microwave irradiation

NASA Astrophysics Data System (ADS)

Moriwaki, Saburo; Qian, Qingrong; Sunohara, Satoshi; Machida, Motoi; Tatsumoto, Hideki

Waste poly (vinyl chloride: PVC) resins are experimentally dehydrochlorinated by microwave irradiation. The following unique results are obtained: (1) plasticizer in PVC resin absorbs microwave power more effectively than PVC polymer. The higher the plasticizer content in PVC resin, the higher is the dehydrochlorination reaction (2) low PVC polymer content materials such as cushion floor require high microwave irradiation power to secure a high dehydrochlorination yield, (3) calcium carbonate in PVC resin reacts with released hydrochloric acid gas and results calcium chloride during microwave irradiation, (4) additives in PVC resin strongly influence dehydrochlorination yield, (5) it is evidenced that the PVC copolymer is also dehydrochlorinated by microwave irradiation.

The effects of dentin and intaglio indirect ceramic optimized polymer restoration surface treatment on the shear bond strength of resin cement

NASA Astrophysics Data System (ADS)

Puspitarini, A.; Suprastiwi, E.; Usman, M.

2017-08-01

Ceramic optimized polymer (ceromer) bonds to the tooth substrate through resin cements. The bond strength between dentin, resin cement, and ceromer depends on the applied surface treatment. To analyze the effects of dentin and intaglio ceromer surface treatment on the shear bond strength self-adhesive resin cement. Forty-five dentin premolar and ceromer specimens were bonded with resin cement and divided into three groups as follows: in group 1, no treatment was applied; in group 2, dentin surface treatment was carried out with acid etching and a bonding agent; and in group 3, dentin surface treatment was carried out with acid etching, a bonding agent, and intaglio ceromer surface treatment with etching and silane. All specimens were incubated at 37 °C for 24 hours, and the shear bond strength was measured using a universal testing machine. Group 3 showed the highest shear bond strength, followed by group 2. The surface treatment of dentin and intaglio ceromer showed significantly improved shear bond strength in the group comparison. Dentin and intaglio ceromer surface treatment can improved the shear bond strength self-adhesive resin cement.

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2014 CFR

2014-04-01

... following prescribed conditions: (a) The cross-linked polyester resins are produced by the condensation of... fiber Polyester fiber produced by the condensation of one or more of the acids listed in paragraph (a)(1...

21 CFR 177.2500 - Polyphenylene sulfone resins.

Code of Federal Regulations, 2014 CFR

2014-04-01

... polyphenylene sulfide with peracetic acid such that the finished resins meet the specifications set forth in... glass transition temperature of the polymer is 360±5 °C as determined by the use of differential...

Separation of thorium and uranium in nitric acid solution using silica based anion exchange resin.

PubMed

Chen, Yanliang; Wei, Yuezhou; He, Linfeng; Tang, Fangdong

2016-09-30

To separate thorium and uranium in nitric acid solution using anion exchange process, a strong base silica-based anion exchange resin (SiPyR-N4) was synthesized. Batch experiments were conducted and the separation factor of thorium and uranium in 9M nitric acid was about 10. Ion exchange chromatography was applied to separate thorium and uranium in different ratios. Uranium could be eluted by 9M nitric acid and thorium was eluted by 0.1M nitric acid. It was proved that thorium and uranium can be separated and recovered successfully by this method. Copyright © 2016 Elsevier B.V. All rights reserved.

Advanced thermoplastic resins, phase 1

NASA Technical Reports Server (NTRS)

Hendricks, C. L.; Hill, S. G.; Falcone, A.; Gerken, N. T.

1991-01-01

Eight thermoplastic polyimide resin systems were evaluated as composite matrix materials. Two resins were selected for more extensive mechanical testing and both were versions of LaRC-TPI (Langley Research Center - Thermoplastic Polyimide). One resin was made with LaRC-TPI and contained 2 weight percent of a di(amic acid) dopant as a melt flow aid. The second system was a 1:1 slurry of semicrystalline LaRC-TPI powder in a polyimidesulfone resin diglyme solution. The LaRC-TPI powder melts during processing and increases the melt flow of the resin. Testing included dynamic mechanical analysis, tension and compression testing, and compression-after-impact testing. The test results demonstrated that the LaRC-TPI resins have very good properties compared to other thermoplastics, and that they are promising matrix materials for advanced composite structures.

Engineering and Design: Composite Materials for Civil Engineering Structures

DTIC Science & Technology

1997-03-31

the effects of acidic, salt, and fresh waters . Acidic, salt, and fresh waters are corrosive to ferrous metals. In Corps of Engineers structures, high...what is commonly called a toughened epoxy. (5) Polymeric resins will absorb moisture. Since many applications are in contact with water (at least...ultraviolet radiation. Some coatings can reduce the amount of moisture absorption by the structure. All polymeric resins will absorb water to some

The shear bond strength of self-adhesive resin cements to dentin and enamel: an in vitro study.

PubMed

Rodrigues, Raphaela F; Ramos, Carla M; Francisconi, Paulo A S; Borges, Ana Flávia S

2015-03-01

Clinicians continue to search for ways to simplify bonding procedures without compromising clinical efficacy. The purpose of this study was to evaluate the shear strength of self-adhesive cements RelyX U100 and RelyX U200, and conventional resin cement RelyX ARC to enamel and dentin after different surface treatments. The crowns of 120 bovine incisor teeth were separated from the roots and embedded in epoxy resin in polyvinyl chloride tubes. In each tooth, the area to be cemented was delimited with central holed adhesive tape. The teeth were distributed into 12 groups (n=10) according to the substrate; etched or not with 37% phosphoric acid; and cement type of enamel-U100, enamel-phosphoric acid-U100, enamel-U200, enamel-phosphoric acid-U200, enamel-ARC, enamel-phosphoric acid-ARC, dentin-U100, dentin-phosphoric acid-U100, dentin-U200, dentin-phosphoric acid-U200, dentin-ARC, and dentin-phosphoric acid-ARC. After 7 days of storage in artificial saliva, shear strength tests were performed by using a universal testing machine (0.5 mm/min). The data were analyzed with 3-way ANOVA and the Tukey test (α=.05). Fracture analysis was performed with a light microscope. Two specimens from each group were analyzed with a scanning electron microscope. In enamel, ARC (9.96 MPa) had higher shear strength (P=.038) than U100 (5.14 MPa); however, after surface etching, U100 (17.81 MPa) and U200 (17.52 MPa) had higher shear strength (P<.001). With dentin, no significant differences were observed (P=.999), except for dentin-ARC (0.34 MPa) (P=.001). Most fractures were of the adhesive type. U200 self-adhesive cement had similar bond strength to the ARC in enamel, but the combination with phosphoric acid had the best bond strength. For dentin, self-adhesive resin cements are equally effective alternatives to conventional resin cement. Copyright © 2015 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Enrichment and low-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water after cleanup by cation exchange resin.

PubMed

Küsters, Markus; Gerhartz, Michael

2010-04-01

For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission.

A complete 1H and 13C NMR data assignment for the diterpene methyl (-)-zanzibarate by 2D spectroscopy and NOE experiments.

PubMed

Imamura, P M; Miranda, P C M L; Giacomini, R A

2004-06-01

The 1H and 13C NMR spectra of methyl (-)-zanzibarate (1), an ent-labdanic diterpene isolated from the epicarp of Hymenaea courbaril var. altissima (Leguminosaea, Cesalpinoideae, Detariae), was fully assigned by COSY experiments, 13C/1H shift correlation diagrams and NOE experiments. Copyright 2004 John Wiley & Sons, Ltd.

Abietic acid isolated from pine resin (Resina Pini) enhances angiogenesis in HUVECs and accelerates cutaneous wound healing in mice.

PubMed

Park, Jun Yeon; Lee, Yun Kyung; Lee, Dong-Soo; Yoo, Jeong-Eun; Shin, Myoung-Sook; Yamabe, Noriko; Kim, Su-Nam; Lee, Seulah; Kim, Ki Hyun; Lee, Hae-Jeung; Roh, Seok Sun; Kang, Ki Sung

2017-05-05

Resin known as Resina Pini is listed in the Korean and Japanese pharmacopoeias and has been used for treating skin wounds and inflammation. Resin is composed of more than 50% abietic acid and 10% neutral substances. In the present study, the wound-healing effects of abietic acid and the possible underlying mechanism of action were investigated in various in vitro and in vivo models. The effects of abietic acid on tube formation and migration were measured in human umbilical vein vascular endothelial cells (HUVECs). Protein expression of mitogen-activated protein kinase (MAPK) activation was evaluated via Western blotting analysis. The wound-healing effects of abietic acid were assessed using a mouse model of cutaneous wounds. The results showed that abietic acid enhanced cell migration and tube formation in HUVECs. Abietic acid induced significant angiogenic potential, which is associated with upregulation of extracellular signal-regulated kinase (ERK) and p38 expression. Additionally, 0.8μM abietic acid-treated groups showed accelerated wound closure compared to the controls in a mouse model of cutaneous wounds. The current data indicate that abietic acid treatment elevated cell migration and tube formation in HUVECs by the activation of ERK and p38 MAPKs. We suggest that abietic acid can be developed as a wound-healing agent. Copyright © 2017 Elsevier Ltd. All rights reserved.

Plant terpenes: defense responses, phylogenetic analysis, regulation and clinical applications.

PubMed

Singh, Bharat; Sharma, Ram A

2015-04-01

The terpenoids constitute the largest class of natural products and many interesting products are extensively applied in the industrial sector as flavors, fragrances, spices and are also used in perfumery and cosmetics. Many terpenoids have biological activities and also used for medical purposes. In higher plants, the conventional acetate-mevalonic acid pathway operates mainly in the cytosol and mitochondria and synthesizes sterols, sesquiterpenes and ubiquinones mainly. In the plastid, the non-mevalonic acid pathway takes place and synthesizes hemi-, mono-, sesqui-, and diterpenes along with carotenoids and phytol tail of chlorophyll. In this review paper, recent developments in the biosynthesis of terpenoids, indepth description of terpene synthases and their phylogenetic analysis, regulation of terpene biosynthesis as well as updates of terpenes which have entered in the clinical studies are reviewed thoroughly.

Adsorption of saponin compound in Carica papaya leaves extract using weakly basic ion exchanger resin

NASA Astrophysics Data System (ADS)

Abidin, Noraziani Zainal; Janam, Anathasia; Zubairi, Saiful Irwan

2016-11-01

Adsorption of saponin compound in papaya leaves juice extract using Amberlite® IRA-67 resin was not reported in previous studies. In this research, Amberlite® IRA-67 was used to determine the amount of saponin that can be adsorbed using different weights of dry resin (0.1 g and 0.5 g). Peleg model was used to determine the maximum yield of saponin (43.67 mg) and the exhaustive time (5.7 days) prior to a preliminary resin-saponin adsorption study. After adsorption process, there was no significant difference (p>0.05) in total saponin content (mg) for sample treated with 0.1 g (3.79 ± 0.55 mg) and sample treated with 0.5 g (3.43 ± 0.51 mg) dry weight resin. Long-term kinetic adsorption of resin-saponin method (>24 hours) should be conducted to obtain optimum freed saponin extract. Besides that, sample treated with 0.1 g dry weight resin had high free radical scavenging value of 50.33 ± 2.74% compared to sample treated with 0.5 g dry weight resin that had low free radical scavenging value of 24.54 ± 1.66% dry weights. Total saponin content (mg), total phenolic content (mg GAE) and free radical scavenging activity (%) was investigated to determine the interaction of those compounds with Amberlite® IRA-67. The RP-HPLC analysis using ursolic acid as standard at 203 nm showed no peak even though ursolic acid was one of the saponin components that was ubiquitous in plant kingdom. The absence of peak was due to weak solubility of ursolic acid in water and since it was only soluble in solvent with moderate polarity. The Pearson's correlation coefficient for total saponin content (mg) versus total phenolic content (mg GAE) and radical scavenging activity (%) were +0.959 and +0.807. Positive values showed that whenever there was an increase in saponin content (mg), the phenolic content (mg GAE) and radical scavenging activity (%) would also increase. However, as the resin-saponin adsorption was carried out, there was a significant decrease of radical scavenging activity (%) as the amount of the resin increased. Moreover, the saponin amount did not show any reduction as the amount of resin resin increased. Therefore, there was other active ingredient which has the antioxidant properties were affected by the adsoprtion process. For that reason, the kinetic equilibrium of resin-saponin adsorption studies against the ratio of resin-to-extract has to be carried out to determine the efficacy of the extract therapeutic properties prior to the cell culture studies.

VALIDATION FOR THE PERMANGANATE DIGESTION OF REILLEX HPQ ANION RESIN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kyser, E.

2009-09-23

The flowsheet for the digestion of Reillex{trademark} HPQ was validated both under the traditional alkaline conditions and under strongly acidic conditions. Due to difficulty in performing a pH adjustment in the large tank where this flowsheet must be performed, the recommended digestion conditions were changed from pH 8-10 to 8 M HNO{sub 3}. Thus, no pH adjustment of the solution is required prior to performing the permanganate addition and digestion and the need to sample the digestion tank to confirm appropriate pH range for digestion may be avoided. Neutralization of the acidic digestion solution will be performed after completion ofmore » the resin digestion cycle. The amount of permanganate required for this type of resin (Reillex{trademark} HPQ) was increased from 1 kg/L resin to 4 kg/L resin to reduce the amount of residual resin solids to a minimal amount (<5%). The length of digestion time at 70 C remains unchanged at 15 hours. These parameters are not optimized but are expected to be adequate for the conditions. The flowsheet generates a significant amount of fine manganese dioxide (MnO{sub 2}) solids (1.71 kg/L resin) and involves the generation of a significant liquid volume due to the low solubility of permanganate. However, since only two batches of resin (40 L each) are expected to be digested, the total waste generated is limited.« less

Extractive scintillating polymer sensors for trace-level detection of uranium in contaminated ground water.

PubMed

Duval, Christine E; DeVol, Timothy A; Husson, Scott M

2016-12-01

This contribution describes the synthesis of robust extractive scintillating resin and its use in a flow-cell detector for the direct detection of uranium in environmental waters. The base poly[(4-methyl styrene)-co-(4-vinylbenzyl chloride)-co-(divinylbenzene)-co-(2-(1-napthyl)-4-vinyl-5-phenyloxazole)] resin contains covalently bound fluorophores. Uranium-binding functionality was added to the resin by an Arbuzov reaction followed by hydrolysis via strong acid or trimethylsilyl bromide (TMSBr)-mediated methanolysis. The resin was characterized by Fourier-transform infrared spectroscopy and spectrofluorometry. Fluorophore degradation was observed in the resin hydrolyzed by strong acid, while the resin hydrolyzed by TMSBr-mediated methanolysis maintained luminosity and showed hydrogen bonding-induced Stokes' shift of ∼100 nm. The flow cell detection efficiency for uranium of the TMSBr-mediated methanolysis resin was evaluated at pH 4, 5 and 6 in DI water containing 500 Bq L -1 uranium-233 and demonstrated flow cell detection efficiencies of 23%, 16% and 7%. Experiments with pH 4, synthetic groundwater with 50 Bq L -1 uranium-233 exhibited a flow cell detection efficiency of 17%. The groundwater measurements show that the resins can concentrate the uranyl cation from waters with high concentrations of competitor ions at near-neutral pH. Findings from this research will lay the groundwork for development of materials for real-time environmental sensing of alpha- and beta-emitting radionuclides. Copyright © 2016 Elsevier B.V. All rights reserved.

Acidic resin-catalysed conversion of fructose into furan derivatives in low boiling point solvents.

PubMed

Zhu, Hong; Cao, Quan; Li, Chunhu; Mu, Xindong

2011-09-27

Conversion of fructose into furan derivatives 5-hydroxymethylfurfural (HMF) and 5-methoxymethylfurfural (MMF) is performed in tetrahydrofuran (THF) and methanol-organic solvent systems, catalysed by an acidic resin Amberlyst-15. The melted fructose can be converted into HMF on the surface of the solid resin catalyst in the presence of THF as an extracting phase, which is a good solvent for HMF and other by-products. The solid resin catalyst can be reused eleven times without losing its catalytic ability, with an average HMF yield of approximately 50%. Upon the addition of methanol, the generated HMF can further react with methanol to form MMF, and the total yield of HMF and MMF could be promoted to 65%. GC-MS analysis confirms the formation of a small amount of methyl levulinate in methanolorganic solvent system. Copyright © 2011 Elsevier Ltd. All rights reserved.

Attempt to induce lightwood in eastern hemlock by treating with paraquat

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kiatgrajai, P.; Rowe, J.W.; Conner, A.H.

1976-01-01

Treatment of eastern hemlock (Tsuga canadensis (L.) Carr.) with the herbicide paraquat did not induce formation of lightwood. However, a dead zone of phloem extended above the paraquat-treatment site. Traumatic resin ducts were observed in the wood immediately adjacent to this dead zone. Although some of these ducts were filled with resin, most were empty. A very small amount of resin soaking was observed at the edges of the dead phloem. Although there was an increase in the extractives content of the wood behind the dead phloem, this did not reach levels with commercial potential. The increase in turpentine levelmore » was mostly due to slightly volatile waxes. The nonvolatile ether extractives were predominately acids other than the fatty and resin acids typical of pines. Electron microscopy revealed fungal hyphae in the wood behind the dead phloem, and several species of fungi were cultured from the wood.« less

Rechargeable Infection-responsive Antifungal Denture Materials

PubMed Central

Cao, Z.; Sun, X.; Yeh, C.-K.; Sun, Y.

2010-01-01

Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be “washed out” by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions. PMID:20940361

[Monitoring method for macroporous resin column chromatography process of salvianolic acids based on near infrared spectroscopy].

PubMed

Hou, Xiang-Mei; Zhang, Lei; Yue, Hong-Shui; Ju, Ai-Chun; Ye, Zheng-Liang

2016-07-01

To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing. Copyright© by the Chinese Pharmaceutical Association.

Impact of pH and application time of meta-phosphoric acid on resin-enamel and resin-dentin bonding.

PubMed

Cardenas, A F M; Siqueira, F S F; Bandeca, M C; Costa, S O; Lemos, M V S; Feitora, V P; Reis, A; Loguercio, A D; Gomes, J C

2018-02-01

To evaluate the immediate microshear resin-enamel bond strength (μSBS) and the immediate and 6-month microtensile bond strength (μTBS) and nanoleakage (NL) of the adhesive interface performed by different pHs of 40% meta-phosphoric acid (MPA) were compared with conventional 37% ortho-phosphoric acid (OPA) under different application times. Additionally, the enamel etching patterns were evaluated and the chemical/morphological changes induced by these differents groups were evaluated. One hundred and ninety-eight extracted human molars were randomly assigned into experimental groups according to the combination of independent variables: Acid [37% ortho-phosphoric acid (OPA), 40% meta-phosphoric acid (MPA) at pHs of: 0.5, 1 and 2] and Application Time [7, 15 and 30s]. Enamel-bond specimens were prepared and tested under μSBS. Resin-dentin beams were tested under μTBS tested immediately or after 6-months of water storage. Nanoleakage was evaluated using bonded-beams of each tooth/time-period. Enamel etching pattern and chemical and ultra-morphology analyses were also performed. The μSBS (MPa) data were subjected to a two-way repeated measures ANOVA (Acid vs. Application time). For μTBS, Acid vs application time vs storage time data were subjected to three-way ANOVA and Tukey's test (α = 0.05). MPA pH 0.5 showed μTBS similar to OPA, independently of the application time on enamel (p>0.05) or dentin (p>0.05). OPA provided higher nanoleakage values than MPA (p = 0.003). Significant decreases in TBS and increases in NL were only observed for OPA after 6 months (p = 0.001). An increase in the application time resulted in a more pronounced etching pattern for MPA. Chemical analysis showed that dentin demineralized by MPA depicted peaks of brushite and octacalcium phosphate. MPA exposed less collagen than OPA. However, optimal results for MPA were dependent on pH/application time. The use of 40% meta-phosphoric acid with a pH of 0.5 is an alternative acid-etching agent for dentin and enamel bonding. Furthermore, the use of MPA preserves the resin-dentin interface over a 6-months period, due to presence of brushite and octacalcium phosphate and a reduced demineralization pattern. Copyright © 2017 Elsevier Ltd. All rights reserved.

Manoyl oxide (13R), the biosynthetic precursor of forskolin, is synthesized in specialized root cork cells in Coleus forskohlii.

PubMed

Pateraki, Irini; Andersen-Ranberg, Johan; Hamberger, Britta; Heskes, Allison Maree; Martens, Helle Juel; Zerbe, Philipp; Bach, Søren Spanner; Møller, Birger Lindberg; Bohlmann, Jörg; Hamberger, Björn

2014-03-01

Forskolin, a complex labdane diterpenoid found in the root of Coleus forskohlii (Lamiaceae), has received attention for its broad range of pharmacological activities, yet the biosynthesis has not been elucidated. We detected forskolin in the root cork of C. forskohlii in a specialized cell type containing characteristic structures with histochemical properties consistent with oil bodies. Organelle purification and chemical analysis confirmed the localization of forskolin and of its simplest diterpene precursor backbone, (13R) manoyl oxide, to the oil bodies. The labdane diterpene backbone is typically synthesized by two successive reactions catalyzed by two distinct classes of diterpene synthases. We have recently described the identification of a small gene family of diterpene synthase candidates (CfTPSs) in C. forskohlii. Here, we report the functional characterization of four CfTPSs using in vitro and in planta assays. CfTPS2, which synthesizes the intermediate copal-8-ol diphosphate, in combination with CfTPS3 resulted in the stereospecific formation of (13R) manoyl oxide, while the combination of CfTPS1 and CfTPS3 or CfTPS4 led to formation of miltiradiene, precursor of abietane diterpenoids in C. forskohlii. Expression profiling and phylogenetic analysis of the CfTPS family further support the functional diversification and distinct roles of the individual diterpene synthases and the involvement of CfTPS1 to CfTPS4 in specialized metabolism and of CfTPS14 and CfTPS15 in general metabolism. Our findings pave the way toward the discovery of the remaining components of the pathway to forskolin, likely localized in this specialized cell type, and support a role of oil bodies as storage organelles for lipophilic bioactive metabolites.

Manoyl Oxide (13R), the Biosynthetic Precursor of Forskolin, Is Synthesized in Specialized Root Cork Cells in Coleus forskohlii1[W][OPEN

PubMed Central

Pateraki, Irini; Andersen-Ranberg, Johan; Hamberger, Britta; Heskes, Allison Maree; Martens, Helle Juel; Zerbe, Philipp; Bach, Søren Spanner; Møller, Birger Lindberg; Bohlmann, Jörg; Hamberger, Björn

2014-01-01

Forskolin, a complex labdane diterpenoid found in the root of Coleus forskohlii (Lamiaceae), has received attention for its broad range of pharmacological activities, yet the biosynthesis has not been elucidated. We detected forskolin in the root cork of C. forskohlii in a specialized cell type containing characteristic structures with histochemical properties consistent with oil bodies. Organelle purification and chemical analysis confirmed the localization of forskolin and of its simplest diterpene precursor backbone, (13R) manoyl oxide, to the oil bodies. The labdane diterpene backbone is typically synthesized by two successive reactions catalyzed by two distinct classes of diterpene synthases. We have recently described the identification of a small gene family of diterpene synthase candidates (CfTPSs) in C. forskohlii. Here, we report the functional characterization of four CfTPSs using in vitro and in planta assays. CfTPS2, which synthesizes the intermediate copal-8-ol diphosphate, in combination with CfTPS3 resulted in the stereospecific formation of (13R) manoyl oxide, while the combination of CfTPS1 and CfTPS3 or CfTPS4 led to formation of miltiradiene, precursor of abietane diterpenoids in C. forskohlii. Expression profiling and phylogenetic analysis of the CfTPS family further support the functional diversification and distinct roles of the individual diterpene synthases and the involvement of CfTPS1 to CfTPS4 in specialized metabolism and of CfTPS14 and CfTPS15 in general metabolism. Our findings pave the way toward the discovery of the remaining components of the pathway to forskolin, likely localized in this specialized cell type, and support a role of oil bodies as storage organelles for lipophilic bioactive metabolites. PMID:24481136

Feasibility study on the utilization of rubber latex effluent for producing bacterial biopolymers.

PubMed

Tang, S N; Fakhru'l-Razi, A; Hassan, M A; Karim, M I

1999-01-01

Rubber latex effluent is a polluting source that has a high biochemical oxygen demand (BOD). It is estimated that about 100 million liters of effluent are discharged daily from rubber processing factories. Utilization of this effluent such as the use of a coupled system not only can reduce the cost of treatment but also yield a fermentation feedstock for the production of bioplastic. This study initially was carried out to increase the production of organic acids by anaerobic treatment of rubber latex effluent. It was found that through anaerobic treatment the concentration of organic acids did not increase. Consequently, separation of organic acids from rubber latex effluent by anion exchange resin was examined as a preliminary study of recovering acetic and propionic acids. However, the suspended solids (SS) content in the raw effluent was rather high which partially blocked the ion-exchange columns. Lime was used to remove the SS in the rubber latex effluent. After the lime precipitation process, organic acids were found to adsorb strongly onto the anion exchange resin. Less adsorption of organic acids onto the resin was observed before the lime precipitation. This was probably due to more sites being occupied by colloidal particles on the resin thus inhibiting the adsorption of organic acids. The initial concentration of organic acids in the raw effluent was 3.9 g/L. After ion exchange, the concentration of the organic acids increased to 27 g/L, which could be utilized for production of polyhydroxyalkanoates (PHA). For PHA accumulation stage, concentrated rubber latex effluent obtained from ion exchange resins and synthetic acetic acid were used as the carbon source. Quantitative analyses from fed batch culture via HPLC showed that the accumulation of PHA in Alcaligenes eutrophus was maximum with a concentration of 1.182 g/L when cultivated on synthetic acetic acid, corresponding to a yield of 87% based on its cell dry weight. The dry cell weight increased from 0.71 to 1.67 g/L. On the other hand, using concentrated rubber latex effluent containing acetic and propionic acids resulted in reduced PHA content by dry weight (14%) but the dry cell weight increased from 0.49 to 1.30 g/L. The results clearly indicated that the cells grow well in rubber latex effluent but no PHA was accumulated. This could be due to the high concentration of propionic acid in culture broth or other factors such as heavy metals. Thus further work is required before rubber latex effluent can be utilized as a substrate for PHA production industrially.

Diclofenac removal in urine using strong-base anion exchange polymer resins.

PubMed

Landry, Kelly A; Boyer, Treavor H

2013-11-01

One of the major sources of pharmaceuticals in the environment is wastewater effluent of which human urine contributes the majority of pharmaceuticals. Urine source separation has the potential to isolate pharmaceuticals at a higher concentration for efficient removal as well as produce a nutrient byproduct. This research investigated the efficacy of using strong-base anion exchange polymer resins to remove the widely detected and abundant pharmaceutical, diclofenac, from synthetic human urine under fresh and ureolyzed conditions. The majority of experiments were conducted using a strong-base, macroporous, polystyrene resin (Purolite A520E). Ion-exchange followed a two-step removal rate with rapid removal in 1 h and equilibrium removal in 24 h. Diclofenac removal was >90% at a resin dose of 8 mL/L in both fresh and ureolyzed urine. Sorption of diclofenac onto A520E resin was concurrent with desorption of an equivalent amount of chloride, which indicates the ion-exchange mechanism is occurring. The presence of competing ions such as phosphate and citrate did not significantly impact diclofenac removal. Comparisons of three polystyrene resins (A520E, Dowex 22, Dowex Marathon 11) as well as one polyacrylic resin (IRA958) were conducted to determine the major interactions between anion exchange resin and diclofenac. The results showed that polystyrene resins provide the highest level of diclofenac removal due to electrostatic interactions between quaternary ammonium functional groups of resin and carboxylic acid of diclofenac and non-electrostatic interactions between resin matrix and benzene rings of diclofenac. Diclofenac was effectively desorbed from A520E resin using a regeneration solution that contained 4.5% (m/m) NaCl in an equal-volume mixture of methanol and water. The greater regeneration efficiency of the NaCl/methanol-water mixture over the aqueous NaCl solution supports the importance of non-electrostatic interactions between resin matrix and benzene rings of diclofenac. Experiments with ketoprofen, in addition to diclofenac, suggest that polystyrene anion exchange resins can be used to selectively remove other acidic pharmaceuticals from urine. Copyright © 2013 Elsevier Ltd. All rights reserved.

Identification of resinous materials on 16th and 17th century reverse-glass objects by gas chromatography/mass spectrometry

NASA Astrophysics Data System (ADS)

Baumer, Ursula; Dietemann, Patrick; Koller, Johann

2009-07-01

Objects of hinterglasmalerei, reverse-glass paintings, are painted on the back side of glass panels. Obviously, the paint layers are applied in reverse order, starting with the uppermost layer. The finished hinterglas painting is viewed through the glass, thus revealing an impressive gloss and depth of colour. The binding media of two precious objects of hinterglasmalerei from the 16th and 17th century have been identified as almost exclusively resinous. Identification was performed by a special optimised analysis procedure, which is discussed in this paper: solvent extracts are analysed by gas chromatography/mass spectrometry, both with and without derivatisation or hydrolysis. In an additional step, oxalic acid is added to the methanol extracts prior to injection. This attenuates the peaks of the non-acidic compounds, whereas the acids elute with good resolution. The non-acidic compounds are emphasised after injection of the underivatised extracts. This approach minimises compositional changes caused by the sample preparation and derivatisation steps. Chromatograms of aged samples with a very complex composition are simplified, which allows a more reliable and straightforward identification of significant markers for various materials. The binding media of the hinterglas objects were thus shown to consist of mixtures of different natural resins, larch turpentine, heat-treated Pinaceae resin or mastic. Typical compounds of dragon's blood, a natural red resin, were also detectable in red glazes by the applied analysis routine. Identification of the binding media provides valuable information that can be used in the development of an adequate conservation treatment.

Influence of surface conditions and silane agent on the bond of resin to IPS Empress 2 ceramic.

PubMed

Spohr, Ana Maria; Sobrinho, Lourenço Correr; Consani, Simonides; Sinhoreti, Mario Alexandre Coelho; Knowles, Jonathan C

2003-01-01

The aim of this study was to evaluate the effect of different ceramic surface treatments on the tensile bond strength between IPS Empress 2 ceramic framework and Rely X adhesive resin cement, with or without the application of a silane coupling agent. One hundred twenty disks were made, embedded in resin, and randomly divided into six groups: group 1 = sandblasting (100 microm), no silanation; group 2 = sandblasting (100 microm), silane treatment; group 3 = sandblasting (50 microm), no silanation; group 4 = sandblasting (50 microm), silane treatment; group 5 = hydrofluoric acid etching, no silanation; and group 6 = hydrofluoric acid etching, silane treatment. The disks were bonded into pairs with adhesive resin cement. All samples were stored in distilled water at 37 degrees C for 24 hours and then thermocycled. The samples were submitted to tensile testing. The use of silane improved the bond strength in relation to the groups in which silane was not applied (P < .05). The most effective surface treatment was etching with 10% hydrofluoric acid, both with (25.6 MPa) and without silane application (16.4 MPa); these values showed a statistically significant difference compared to sandblasting with 50- and 100-microm Al2O3. Sandblasting with 50-microm Al2O3, with (11.8 MPa) and without silane (5.4 MPa), demonstrated significantly higher tensile bond strength than sandblasting with 100-microm Al2O3, with (8.3 MPa) and without silane (3.8 MPa). Combined application of 10% hydrofluoric acid and silane enhanced the bond strength between the IPS Empress 2 ceramic framework and resin agent.

Characterization of the homologs of flerovium with crown ether based extraction chromatography resins: studies in nitric acid

DOE PAGES

Despotopulos, John D.; Kmak, Kelly N.; Gharibyan, Narek; ...

2016-09-17

Eichrom’s Pb resin, a crown-ether-based extraction chromatography resin, was characterized for separation of the flerovium (Fl) homologs, Pb and Sn. Batch uptake of Pb(II) and Sn(IV) radionuclides was determined from an HNO 3 matrix. Pb(II) was strongly retained on the resin at all HNO 3 concentrations, while Sn(IV) showed no uptake. Extraction kinetics for Pb(II) were examined and show suitable uptake on the second time scale. Here, separation methods for the isolation of individual homologs, Pb(II) and Sn(IV), have been established using 2 mL pre-packed vacuum flow Pb resin columns.

The biocompatability of mesoporous inorganic-organic hybrid resin films with ionic and hydrophilic characteristics.

PubMed

Kim, Gahee; Hong, Lan Young; Jung, Jungwoon; Kim, Dong-Pyo; Kim, Heesoo; Kim, Ik Jung; Kim, Jung Ran; Ree, Moonhor

2010-03-01

New mesoporous silicate-titania resin systems hybridized with 4,5-dihydroxy-m-benzenedisulfonic acid and poly(ethylene glycol)-dimethacrylate component were developed. These inorganic-organic hybrid resins were found to reveal highly controlled ionic and hydrophilic surface with excellent durability and adhesion onto various substrates. The resin films revealed high resistance to nonspecific adsorption of fibrinogen and to adherence by several bacterial pathogens such as Escherichia coli, Staphylococcus aureus, Staphylococcus epidermidis and Enterococcus faecalis. Furthermore, excellent biocompatibility of the developed resins was proved by both HEp-2 cell adhesion in vitro and subcutaneous implantation in mice. The inorganic-organic hybrid resins are strongly promising for biomedical applications including biomedical devices and biosensors. Copyright 2009 Elsevier Ltd. All rights reserved.

Bio-phenolic resin from oil palm empty fruit bunches

NASA Astrophysics Data System (ADS)

Zakaria, Zuhaili; Zakaria, Sarani; Roslan, Rasidi; Chia, Chin Hua; Jaafar, Sharifah Nabihah Syed; Amran, Umar Adli

2018-04-01

Utilization of oil palm empty fruit bunches (EFB) in the production of bio-phenolic resin is an alternative way to reduce the dependency of petroleum-based phenol. In this study, resol type bio-phenolic resin (BPR) was synthesized from EFB fibers using sulfuric acid as the catalyst to produce liquefied empty fruit bunches (LEFB) followed by resinification reaction with formaldehyde in alkaline condition. The SEM image of LEFB residue showed separation of fiber bundles into individual fibers. This indicate that lignin was destroyed during the liquefaction process. The increased of formaldehyde/LEFB molar ratio has resulted an increase of viscosity, solid content and pH of the resin. The obtained FTIR spectra confirmed that functional groups of BPR resins was almost similar with commercial resin.

Phenolic cation exchange resin material for recovery of cesium and strontium

DOEpatents

Ebra, Martha A.; Wallace, Richard M.

1983-01-01

A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear waste solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs.sup.+ and Sr.sup.2+ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

Phenolic cation-exchange resin material for recovery of cesium and strontium. [Patent application

DOEpatents

Ebra, M.A.; Wallace, R.M.

1982-05-05

A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear wate solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs/sup +/ and Sr/sup 2 +/ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

In vivo effects of two acidic soft drinks on shear bond strength of metal orthodontic brackets with and without resin infiltration treatment.

PubMed

Hammad, Shaza M; Enan, Enas T

2013-07-01

To evaluate the in vivo effects of two acidic soft drinks (Coca-Cola and Sprite) on the shear bond strength of metal orthodontic brackets with and without resin infiltration treatment. In addition, the enamel surface was evaluated, after debonding, using a scanning electron microscope. Sixty noncarious maxillary premolars, scheduled for extraction in 30 orthodontic patients, were used. Patients were randomly divided into two groups according to the soft drink tested (Coca-Cola or Sprite). In each group, application of resin infiltration (Icon. DMG, Hamburg, Germany) was done on one side only before bonding of brackets. Patients were told to rinse their mouth with their respective soft drink at room temperature for 5 minutes, three times a day for 3 months. Shear bond strength was tested with a universal testing machine. After shearing test, a scanning electron microscope was used to evaluate enamel erosion. Statistical analysis was performed by twoway analysis of variance followed by the least significant difference test. The Coca-Cola group without resin infiltration showed the lowest resistance to shearing forces. Scanning electron micrographs of both groups after resin application showed a significant improvement compared with results without resin use, as the enamel appeared smoother and less erosive. Pretreatment with the infiltrating resin has proved to result in a significant improvement in shear bond strength, regardless of the type of soft drink consumed.

Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

1997-01-01

Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC Multipurpose Tape Machine. Process parameters were determined and composite panels fabricated. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

Antiinflammatory and antioxidant activities of gum mastic.

PubMed

Mahmoudi, M; Ebrahimzadeh, M A; Nabavi, S F; Hafezi, S; Nabavi, S M; Eslami, Sh

2010-09-01

Pistacia lentiscus has traditionally been used in the treatment of many diseases. Its resin was investigated for its mineral contents, anti-inflammatory and antioxidant activities in rats. Inhibition of carrageenan induced edema was used to evaluate anti-inflammatory activity. Fe2+ chelating ability, 1,1-diphenyl-2-picryl hydrazyl radical (DPPH) and nitric oxide scavenging activities were used to evaluate antioxidant activities and mineral contents were determined by atomic absorption spectroscopy. Gallic acid content was determined by HPLC. Resin produced statistically significant inhibition of edema at all doses when compared to the control groups. A 100% inhibition of inflammation was observed at 800 mg/kg i.p. Resin exhibit no toxicity up to 3 g/kg body weights i.p. in mice. Weak DPPH and nitric oxide scavenging activities were observed but showed good Fe2+ chelating ability (IC50 = 162 microg ml(-1)). The amount of elements was decreased in the order: Cu > Fe, Zn > Mn > Ni, Cd. Gallic acid content was 0.1 mg/g resin. These experimental data support the use of Pistacia lentiscus resin as an antiinflammatory and antioxidant agent.

Selective adsorption and recovery of Au(III) from three kinds of acidic systems by persimmon residual based bio-sorbent: a method for gold recycling from e-wastes.

PubMed

Fan, Ruiyi; Xie, Feng; Guan, Xueliang; Zhang, Qinglin; Luo, Zhengrong

2014-07-01

A low cost bio-sorbent, named "PPF resin", was prepared by crosslinking the persimmon residual with formaldehyde. The adsorption behavior of PPF resin towards Au(III) from varied HCl and HNO3 concentration solutions was studied. PPF resin could adsorb almost complete Au(III) from high acidic systems. The influence of dilution ratio, solid-liquid ratio and time towards Au(III) from aqua regia leached PCBs liquor was censored in detail by batch and continuous adsorption methods. The PPF resin before and after adsorption was characterized by FT-IR, XRD and XPS spectra which provided evidences for the reduction of Au(III) to Au(0) with a proposed mechanism of Au(III) adsorption-reduction process. After saturated column adsorption of 0.1g PPF resin, 0.0506 g gold (purity: 99.9%) was obtained by the method of incineration. The present results provide a new approach for gold recovery from the secondary resources. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of EDTA and phosphoric Acid pretreatment on the bonding effectiveness of self-etch adhesives to ground enamel.

PubMed

Ibrahim, Ihab M; Elkassas, Dina W; Yousry, Mai M

2010-10-01

This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9-1.0), intermediary strong AdheSE (pH=1.6-1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel.

Effect of EDTA and Phosphoric Acid Pretreatment on the Bonding Effectiveness of Self-Etch Adhesives to Ground Enamel

PubMed Central

Ibrahim, Ihab M.; Elkassas, Dina W.; Yousry, Mai M.

2010-01-01

Objectives: This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Methods: Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9–1.0), intermediary strong AdheSE (pH=1.6–1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Results: Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Conclusions: Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel. PMID:20922162

Poly(ethylene imine)-based granular sorbents by a new process of templated gel-filling. High capacity and selectivity of copper sorption in acidic and alkaline media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chanda, M.; Rempel, G.L.

A new process has been developed for making granular gel-type sorbents from chelating resins using metal ion as template. Named as templated gel-filling, the process uses the chosen metal as templating host ion on high-surface-area silica to build a templated gel layer from a solution of the chelating resin in a suitable solvent in which the resin is soluble but its metal complex is insoluble. After cross-linking the templated gel layer, the silica support is removed by alkali to produce a hollow shell of the templated gel. The shells are then soaked in a concentrated aqueous solution of the samemore » metal ion and suspended in the same resin solution to afford gel-filling. The shells thus filled with metal-templated gel are treated with cross-linking agent, followed by acid to remove the template ion and activate the resin for metal sorption. Poly(ethyleneimine) and its partially ethylated derivative have been used to produce granular gel-type sorbents by this process, with Cu(II) as the template ion. These sorbents are found to offer high capacity and selectivity for copper over nickel, cobalt, and zinc in both acidic and alkaline media. Containing a relatively high fraction of imbibed water, the sorbents exhibit markedly enhanced rate behavior, in both sorption and stripping.« less

Polyvinyl alcohol cross-linked with two aldehydes

NASA Technical Reports Server (NTRS)

Sheibley, D. W.; Rieker, L. L.; Hsu, L. C.; Manzo, M. A. (Inventor)

1982-01-01

A film forming polyvinyl alcohol resin is admixed, in aqueous solution, with a dialdehyde crosslinking agent which is capable of crosslinking the polyvinyl alcohol resin and a water soluble acid aldehyde containing a reactive aldehyde group capable of reacting with hydroxyl groups in the polyvinyl alcohol resin and an ionizable acid hydrogen atom. The dialdehyde is present in an amount sufficient to react with from 1 to 20% by weight of the theoretical amount required to react with all of the hydroxyl groups of the polyvinyl alcohol. The amount of acid aldehyde is from 1 to 50% by weight, same basis, and is sufficient to reduce the pH of the aqueous admixture to 5 or less. The admixture is then formed into a desired physical shape, such as by casting a sheet or film, and the shaped material is then heated to simultaneously dry and crosslink the article.

Energy efficient room temperature synthesis of cardanol-based novolac resin using acoustic cavitation.

PubMed

Jadhav, Nilesh L; Sastry, Sai Krishna C; Pinjari, Dipak V

2018-04-01

The present study deals with synthesis of cardanol-cased novolac (CBN) resin by the condensation reaction between cardanol and formaldehyde using acoustic cavitation. It is a step-growth polymerization which occurs in the presence of an acid catalyst such as adipic acid, citric acid, oxalic acid, sulphuric acid and hydrochloric acid. CBN was also synthesised by a conventional method for the sake of comparison of techniques. The effect of molar ratio, effect of catalyst, effect of different catalyst and effect of power on the conversion to CBN has been studied. The synthesised CBN was characterized using the Fourier Transform Infra Red Spectroscopy (FTIR), Gel Permeation Chromatography (GPC), Nuclear Magnetic Resonance (NMR) Spectroscopy and Thermogravimetric Analysis (TGA). The reaction was monitored by the Acid value, free formaldehyde content and viscosity of the synthesised product. The reaction time required for the conventionally synthesised CBN was 5 h (300 min) with 120 °C as an operating temperature while sonochemically the time reduced to 30 min at room temperature. The amount of time and energy saved can be quantified. Ultrasound facilitated synthesis was found to be an energy efficient and time-saving method for the synthesis of novolac resin. Copyright © 2017 Elsevier B.V. All rights reserved.

Transient and residual stresses in a pressable glass-ceramic before and after resin-cement coating determined using profilometry.

PubMed

Isgró, G; Addison, O; Fleming, G J P

2011-05-01

The effect of heat-pressing and subsequent pre-cementation (acid-etching) and resin-cementation operative techniques on the development of transient and residual stresses in different thicknesses of a lithium disilicate glass-ceramic were characterised using profilometry prior to biaxial flexure strength (BFS) determination. 60 IPS e.max Press discs were pressed and divested under controlled conditions. The discs were polished on one surface to thicknesses of 0.61±0.05, 0.84±0.08, and 1.06±0.07 mm (Groups A-C, respectively). The mean of the maximum deflection (acid-etching and resin-coating was determined using high resolution profilometery prior to BFS testing. Paired sample t-tests were performed (p<0.05) on the 20 individual samples in each group (Groups A-C) for each comparison. Differences between the baseline quantification and resin-cement coating deflection values and BFS values for Groups A-C were determined using a one-way ANOVA with post hoc Tukey tests (p<0.05). Baseline quantification for Groups A-C identified no significant differences between the group means of the maximum deflection values (p=0.341). Following HF acid-etching, a significant increase in deflection for all groups (p<0.001) was identified compared with the baseline quantification. Additionally, resin-cement coating significantly increased deflection for Group A (p<0.001), Group B (p<0.001) and Group C (p=0.001) specimens for the individual groups. The increased deflection from baseline quantification to resin-cement coating was significantly different (p<0.001) for the three specimen thicknesses, although the BFS values were not. The lower reported baseline quantification range of the mean of the maximum deflection for the IPS e.max(®) Press specimens was predominantly the result of specimen polishing regime inducing a tensile stress state across the surface defect integral which accounted for the observed surface convexity. Acid-etching and resin-cementation had a significant impact on the development and magnitude of the transient and residual stresses in the lithium disilicate glass-ceramic investigated. Copyright © 2011 Elsevier Ltd. All rights reserved.

Studies on the application of temperature-responsive ion exchange polymers with whey proteins.

PubMed

Maharjan, Pankaj; Campi, Eva M; De Silva, Kirthi; Woonton, Brad W; Jackson, W Roy; Hearn, Milton T W

2016-03-18

Several new types of temperature-responsive ion exchange resins of different polymer composition have been prepared by grafting the products from the co-polymerisation of N-phenylacrylamide, N-iso-propylacrylamide and acrylic acid derivatives onto cross-linked agarose. Analysis of the binding isotherms for these different resins obtained under batch adsorption conditions indicated that the resin based on N-iso-propylacrylamide containing 5% (w/w) N-phenylacrylamide and 5% (w/w) acrylic acid resulted in the highest adsorption capacity, Bmax, for the whey protein, bovine lactoferrin, e.g. 14 mg bovine lactoferrin/mL resin at 4 °C and 62 mg bovine lactoferrin/mL resin at 40 °C, respectively. Under dynamic loading conditions at 40 °C, 94% of the loaded bovine lactoferrin on a normalised mg protein per mL resin basis was adsorbed by this new temperature-responsive ion-exchanger, and 76% was eluted by a single cycle temperature shift to 4 °C without varying the composition of the 10mM sodium dihydrogen phosphate buffer, pH 6.5, or the flow rate. The binding characteristics of these different ion exchange resins with bovine lactoferrin were also compared to results obtained using other resins based on N-isopropylacrylamide but contained N-tert-butylacrylamide rather than N-phenylacrylamide, where the corresponding dynamic capture and release properties for bovine lactoferrin required different temperature conditions of 20 °C and 50 °C, respectively for optimal desorption/adsorption. The cationic protein, bovine lactoperoxidase, was also adsorbed and desorbed with these temperature-responsive resins under similar conditions of changing temperature, whereas the anionic protein, bovine β-lactoglobulin, was not adsorbed under this regime of temperature conditions but instead eluted in the flow-through. Copyright © 2016 Elsevier B.V. All rights reserved.

Compounds from the Fruits of the Popular European Medicinal Plant Vitex agnus-castus in Chemoprevention via NADP(H):Quinone Oxidoreductase Type 1 Induction.

PubMed

Li, Shenghong; Qiu, Shengxiang; Yao, Ping; Sun, Handong; Fong, Harry H S; Zhang, Hongjie

2013-01-01

As part of our continuing efforts in the search for potential biologically active compounds from medicinal plants, we have isolated 18 compounds including two novel nitrogen containing diterpenes from extracts of the fruits of Vitex agnus-castus. These isolates, along with our previously obtained novel compound vitexlactam A (1), were evaluated for potential biological effects, including cancer chemoprevention. Chemically, the nitrogenous isolates were found to be two labdane diterpene alkaloids, each containing an α , β -unsaturated γ -lactam moiety. Structurally, they were elucidated to be 9 α -hydroxy-13(14)-labden-16,15-amide (2) and 6 β -acetoxy-9 α -hydroxy-13(14)-labden-15,16-amide (3), which were named vitexlactams B and C, respectively. The 15 known isolates were identified as vitexilactone (4), rotundifuran (5), 8-epi-manoyl oxide (6), vitetrifolin D (7), spathulenol (8), cis-dihydro-dehydro-diconiferylalcohol-9-O- β -D-glucoside (9), luteolin-7-O-glucoside (10), 5-hydroxy-3,6,7,4'-tetramethoxyflavone (11), casticin (12), artemetin (13), aucubin (14), agnuside (15), β -sitosterol (16), p-hydroxybenzoic acid (17), and p-hydroxybenzoic acid glucose ester (18). All compound structures were determined/identified on the basis of 1D and/or 2D NMR and mass spectrometry techniques. Compounds 6, 8, 9, and 18 were reported from a Vitex spieces for the first time. The cancer chemopreventive potentials of these isolates were evaluated for NADP(H):quinone oxidoreductase type 1 (QR1) induction activity. Compound 7 demonstrated promising QR1 induction effect, while the new compound vitexlactam (3) was only slightly active.

Compounds from the Fruits of the Popular European Medicinal Plant Vitex agnus-castus in Chemoprevention via NADP(H):Quinone Oxidoreductase Type 1 Induction

PubMed Central

Li, Shenghong; Qiu, Shengxiang; Yao, Ping; Sun, Handong; Fong, Harry H. S.; Zhang, Hongjie

2013-01-01

As part of our continuing efforts in the search for potential biologically active compounds from medicinal plants, we have isolated 18 compounds including two novel nitrogen containing diterpenes from extracts of the fruits of Vitex agnus-castus. These isolates, along with our previously obtained novel compound vitexlactam A (1), were evaluated for potential biological effects, including cancer chemoprevention. Chemically, the nitrogenous isolates were found to be two labdane diterpene alkaloids, each containing an α, β-unsaturated γ-lactam moiety. Structurally, they were elucidated to be 9α-hydroxy-13(14)-labden-16,15-amide (2) and 6β-acetoxy-9α-hydroxy-13(14)-labden-15,16-amide (3), which were named vitexlactams B and C, respectively. The 15 known isolates were identified as vitexilactone (4), rotundifuran (5), 8-epi-manoyl oxide (6), vitetrifolin D (7), spathulenol (8), cis-dihydro-dehydro-diconiferylalcohol-9-O-β-D-glucoside (9), luteolin-7-O-glucoside (10), 5-hydroxy-3,6,7,4′-tetramethoxyflavone (11), casticin (12), artemetin (13), aucubin (14), agnuside (15), β-sitosterol (16), p-hydroxybenzoic acid (17), and p-hydroxybenzoic acid glucose ester (18). All compound structures were determined/identified on the basis of 1D and/or 2D NMR and mass spectrometry techniques. Compounds 6, 8, 9, and 18 were reported from a Vitex spieces for the first time. The cancer chemopreventive potentials of these isolates were evaluated for NADP(H):quinone oxidoreductase type 1 (QR1) induction activity. Compound 7 demonstrated promising QR1 induction effect, while the new compound vitexlactam (3) was only slightly active. PMID:23662135

Development and validation of an RP-HPLC method for quantification of cinnamic acid derivatives and kaurane-type diterpenes in Mikania laevigata and Mikania glomerata.

PubMed

Bertolucci, Suzan Kelly; Pereira, Ana Bárbara; Pinto, José Eduardo; de Aquino Ribeiro, José Antônio; de Oliveira, Alaíde Braga; Braga, Fernão Castro

2009-02-01

MIKANIA GLOMERATA and MIKANIA LAEVIGATA (Asteraceae) are medicinal plants popularly named 'guaco' in Brazil. The leaves of both species are used to treat respiratory diseases, with coumarin (CO) and kaurane-type diterpenes being regarded as the bioactive constituents. A new and simple RP-HPLC method was developed and validated for the simultaneous quantification of CO, O-coumaric (OC), benzoylgrandifloric (BA), cinnamoylgrandifloric (CA) and kaurenoic (KA) acids in the species. Optimal separation was achieved with an alternating gradient elution of methanol and acetonitrile and detection was carried out by DAD at three different wavelengths: 210 nm for CO, OC, KA; 230 nm for BA; and 270 nm for CA. The extracts showed good stability during 42 hours under normal laboratory conditions (temperature of 23 +/- 2 degrees C). The standard curves were linear over the range 0.5 - 5.0 microg (CO), 0.25 - 4.0 microg (OC), 1.0 - 8.0 microg (BA), 0.5 - 3.0 microg (CA) and 0.8 - 12.0 microg (KA), with R(2) > 0.999 for all compounds. The method showed good precision for intra-day (RSD < 4.6 %) and inter-day assays (RSD < 4.4 %). The recovery was between 99.9 and 105.3 %, except for CO and OC in M. glomerata (73.2 - 91.6 % and 86.3 - 117.4 %, respectively). The limits of quantification and detection were in the range of 0.025 - 0.800 microg and 0.007 - 0.240 microg. The method was tested for new and old columns, temperature variation (26 and 28 degrees C) and by different operators in the same laboratory. The method was successfully applied to samples of both species.

Gastroprotective activity of ferruginol in mice and rats: effects on gastric secretion, endogenous prostaglandins and non-protein sulfhydryls.

PubMed

Areche, Carlos; Theoduloz, Cristina; Yáñez, Tania; Souza-Brito, Alba R M; Barbastefano, Víctor; de Paula, Débora; Ferreira, Anderson L; Schmeda-Hirschmann, Guillermo; Rodríguez, Jaime A

2008-02-01

The gastroprotective mechanism of the natural diterpene ferruginol was assessed in mice and rats. The involvement of gastric prostaglandins (PGE(2)), reduced glutathione, nitric oxide or capsaicin receptors was evaluated in mice either treated or untreated with indometacin, N-ethylmaleimide (NEM), N-nitro-L-arginine methyl ester (L-NAME) or ruthenium red, respectively, and then orally treated with ferruginol or vehicle. Gastric lesions were induced by oral administration of ethanol. The effects of ferruginol on the parameters of gastric secretion were assessed in pylorus-ligated rats. Gastric PGE(2) content was determined in rats treated with ferruginol and/or indometacin. The reduction of gastric glutathione (GSH) content was determined in rats treated with ethanol after oral administration of ferruginol, lansoprazole or vehicle. Finally, the acute oral toxicity was assessed in mice. Indometacin reversed the gastroprotective effect of ferruginol (25 mg kg(-1)) but not NEM, ruthenium red or L-NAME. The diterpene (25 mg kg(-1)) increased the gastric juice volume and its pH value, and reduced the titrable acidity but was devoid of effect on the gastric mucus content. Ferruginol (25, 50 mg kg(-1)) increased gastric PGE(2) content in a dose-dependent manner and prevented the reduction in GSH observed due to ethanol-induced gastric lesions in rats. Single oral doses up to 3 g kg(-1) ferruginol did not elicit mortality or acute toxic effects in mice. Our results showed that ferruginol acted as a gastroprotective agent stimulating the gastric PGE(2) synthesis, reducing the gastric acid output and improving the antioxidant capacity of the gastric mucosa by maintaining the GSH levels.

Biologically Active Polymeric Coating Materials

DTIC Science & Technology

1975-04-01

unsaturated alkyds , or through a condensation reaction of an organometallic oxide and a resin containing carboxylic acid groups as side chains. The...extend the service life of antifouling coatings by means of polymerization of toxicant into paint resins . The coating binder is so constructed that the...from styrene (s6) and polyester (P54, figure 5) organometallic resins . To date, the antifouling performance of epoxy (WS 52B, figure 6) and

Detoxification of Organosolv-Pretreated Pine Prehydrolysates with Anion Resin and Cysteine for Butanol Fermentation.

PubMed

Li, Jing; Shi, Suan; Tu, Maobing; Via, Brain; Sun, Fubao Fuelbio; Adhikari, Sushil

2018-05-02

Bioconversion of lignocellulose to biofuels suffers from the degradation compounds formed during pretreatment and acid hydrolysis. In order to achieve an efficient biomass to biofuel conversion, detoxification is often required before enzymatic hydrolysis and microbial fermentation. Prehydrolysates from ethanol organosolv-pretreated pine wood were used as substrates in butanol fermentation in this study. Six detoxification approaches were studied and compared, including overliming, anion exchange resin, nonionic resin, laccase, activated carbon, and cysteine. It was observed that detoxification by anion exchange resin was the most effective method. The final butanol yield after anion exchange resin treatment was comparable to the control group, but the fermentation was delayed for 72 h. The addition of Ca(OH) 2 was found to alleviate this delay and improve the fermentation efficiency. The combination of Ca(OH) 2 and anion exchange resin resulted in completion of fermentation within 72 h and acetone-butanol-ethanol (ABE) production of 11.11 g/L, corresponding to a yield of 0.21 g/g sugar. The cysteine detoxification also resulted in good detoxification performance, but promoted fermentation towards acid production (8.90 g/L). The effect of salt on ABE fermentation was assessed and the possible role of Ca(OH) 2 was to remove the salts in the prehydrolysates by precipitation.

Generator for gallium-68 and compositions obtained therefrom

DOEpatents

Neirinckx, Rudi D.; Davis, Michael A.

1981-01-01

A generator for obtaining radioactive gallium-68 from germanium-68 bound in a resin containing unsubstituted phenolic hydroxyl groups. The germanium-68 is loaded into the resin from an aqueous solution of the germanium-68. A physiologically acceptable solution of gallium-68 having an activity of 0.1 to 50 millicuries per milliliter of gallium-68 solution is obtained. The solution is obtained from the bound germanium-68 which forms gallium-68 in situ by eluting the column with a hydrochloric acid solution to form an acidic solution of gallium-68. The acidic solution of gallium-68 can be neutralized.

Heliotropium huascoense resin exudate: chemical constituents and defensive properties.

PubMed

Villarroel, L; Torres, R; Urzúa, A; Reina, M; Cabrera, R; González-Coloma, A

2001-09-01

From the resinous exudate of Heliotropium huascoense a new compound, rel-(8R,9R)-carrizaloic acid, (1) (3-[rel-(8R,9R-9-hydroxy-9,13,13-trimethyl-12-oxo-10-cyclohexenyl)methyl]-4-methoxybenzoic acid), and three known flavonoids, [3-methylgalangin, 3,7-dimethylgalangin, and (-)-alpinone] have been isolated. The structure of 1 was determined by spectral and chemical methods. Several plant defensive properties of 1 (insecticidal and antifungal) have been evaluated.

Biologically active secondary metabolites from fungi. 12.(1) oidiolactones A-F, labdane diterpene derivatives isolated from oidiodendron truncata

PubMed

John; Krohn; Florke; Aust; Draeger; Schulz

1999-09-01

Two known (1 and 2) and four new (3-6) diterpenes named oidiolactones A-F, respectively, and the antibiotic cladosporin were isolated from the fungus Oidiodendron truncata. The structure determination was mainly based on 1D and 2D NMR spectroscopy. The structures of compound 4, displaying an equilibrium between open-chain and cyclized form, and of cladosporin were confirmed by X-ray analysis.

Spectroscopic and microbiological characterization of labdane diterpene 15,16-epoxy-4-hydroxy-labda-13(16),14-dien-3,12-dione isolated from the stems of Croton jacobinensis

NASA Astrophysics Data System (ADS)

Bernardino, A. C. S. S.; Teixeira, A. M. R.; de Menezes, J. E. S. A.; Pinto, C. C. C.; Santos, H. S.; Freire, P. T. C.; Coutinho, H. D. M.; Sena Junior, D. M.; Bandeira, P. N.; Braz-Filho, R.

2017-11-01

In the present study, the natural product named 15,16-epoxy-4-hydroxy-labda-13(16),14-dien-3,12-dione (C20H28O4), a labdane-type diterpene was isolated from the stems of Croton jacobinensis for the first time. This new compound was characterized by infrared and Raman spectroscopy combined with Density Functional Theory calculation. Additionally, the antimicrobial and modulatory antibiotic activities of the compound towards Escherichia coli and Pseudomonas aeruginosa strains were assessed. The labdane diterpene demonstrated a modulatory effect when combined with the antibiotics assayed against both bacteria. A synergistic effect against Escherichia coli can be observed when the compound is associated with gentamicin, reducing the concentration of this antibiotic that is required to inhibit bacterial growth. Other synergistic effects can be observed with gentamicin and cephalothin antibiotics against P. aeruginosa.

Clerodane diterpenes: sources, structures, and biological activities†

PubMed Central

Li, Rongtao; Morris-Natschke, Susan L.; Lee, Kuo-Hsiung

2016-01-01

The clerodane diterpenoids are a widespread class of secondary metabolites and have been found in several hundreds of plant species from various families and in organisms from other taxonomic groups. These substances have attracted interest in recent years due to their notable biological activities, particularly insect antifeedant properties. In addition, the major active clerodanes of Salvia divinorum can be used as novel opioid receptor probes, allowing greater insight into opioid receptor-mediated phenomena, as well as opening additional areas for chemical investigation. This article provides extensive coverage of naturally occurring clerodane diterpenes discovered from 1990 until 2015, and follows up on the 1992 review by Merritt and Ley in this same journal. The distribution, chemotaxonomic significance, chemical structures, and biological activities of clerodane diterpenes are summarized. In the cases where sufficient information is available, structure activity relationship (SAR) correlations and mode of action of active clerodanes have been presented. PMID:27433555

Microwave-assisted extraction of green coffee oil and quantification of diterpenes by HPLC.

PubMed

Tsukui, A; Santos Júnior, H M; Oigman, S S; de Souza, R O M A; Bizzo, H R; Rezende, C M

2014-12-01

The microwave-assisted extraction (MAE) of 13 different green coffee beans (Coffea arabica L.) was compared to Soxhlet extraction for oil obtention. The full factorial design applied to the microwave-assisted extraction (MAE), related to time and temperature parameters, allowed to develop a powerful fast and smooth methodology (10 min at 45°C) compared to a 4h Soxhlet extraction. The quantification of cafestol and kahweol diterpenes present in the coffee oil was monitored by HPLC/UV and showed satisfactory linearity (R(2)=0.9979), precision (CV 3.7%), recovery (<93%), limit of detection (0.0130 mg/mL), and limit of quantification (0.0406 mg/mL). The space-time yield calculated on the diterpenes content for sample AT1 (Arabica green coffee) showed a six times higher value compared to the traditional Soxhlet method. Copyright © 2014 Elsevier Ltd. All rights reserved.

Use of (S)-trans-gamma-monocyclofarnesol as a useful chiral building block for the stereoselective synthesis of diterpenic natural products.

PubMed

Serra, Stefano; Cominetti, Alessandra A; Lissoni, Veronica

2014-03-01

A comprehensive study of the exploitation of (S)-trans-gamma-monocyclofarnesol as a useful chiral building block for the stereoselective synthesis of natural diterpene derivatives is here described. The farnesol derivative (+)-1 was used as starting material in the preparation of the diterpenes (S)-dehydroambliol-A and (S)-trixagol, as well as for the syntheses of the dinorditerpene (S)-dinortrixagone and of the guanidine-interrupted terpenoid (S)-dotofide. Key steps of the presented syntheses were the cross-coupling between an allyl acetate and a Grignard reagent, the Wittig reaction, the selective preparation ofa diacylguanidine derivative and the alkylation of a sulfone derivative, followed by the reductive removal of the same functional group. It is worth noting that the natural products (+)-8, (+)-12 and (+)-15 were prepared stereoselectively for the first time, thus allowing the unambiguous assignment of their absolute configuration.

Total etch technique and cavity isolation.

PubMed

Fusayama, T

1992-01-01

In the total etch technique for chemically adhesive composite restorations, the phosphoric acid penetrates only 10 microns or less into the vital dentin with the dentinal tubules being filled with the odontoblast processes. The acid is completely removed by subsequent air-water jet spray washing. The tubule apertures are perfectly sealed by the protective bonding agent layer with the resin tags adhering to the tubule walls and the resin-impregnated dentin surface. Isolation of the cavity from moisture contamination is required for only less than a few seconds after drying the etched cavity until the bonding agent coating and after this coating until the composite resin placement. Such a short time for isolation is quite easy even without a rubber dam when a trained assistant is cooperating.

Method for the chemical separation of GE-68 from its daughter Ga-68

DOEpatents

Fitzsimmons, Jonathan M.; Atcher, Robert W.

2010-06-01

The present invention is directed to a generator apparatus for separating a daughter gallium-68 radioisotope substantially free of impurities from a parent gernanium-68 radioisotope, including a first resin-containing column containing parent gernanium-68 radioisotope and daughter gallium-68 radioisotope, a source of first eluent connected to said first resin-containing column for separating daughter gallium-68 radioisotope from the first resin-containing column, said first eluent including citrate whereby the separated gallium is in the form of gallium citrate, a mixing space connected to said first resin-containing column for admixing a source of hydrochloric acid with said separated gallium citrate whereby gallium citrate is converted to gallium tetrachloride, a second resin-containing column for retention of gallium-68 tetrachloride, and, a source of second eluent connected to said second resin-containing column for eluting the daughter gallium-68 radioisotope from said second resin-containing column.

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

21 CFR 177.1556 - Polyaryletherketone resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... molecular weight of 20,000 grams per mole, as determined by light scattering measurements in sulfuric acid at room temperature. (b) Optional adjuvant substances. The basic polyaryletherketone resins... centimeter) of food-contact surface, when extracted at reflux temperature for 2 hours with the following...

Reduction of non-enzymatic browning of orange juice and semi-concentrates by removal of reaction substrate.

PubMed

Sharma, Satish K; Juyal, Shashibala; Rao, V K; Yadav, V K; Dixit, A K

2014-07-01

A study was conducted to standardize the technology for the removal of amino acids (one of the browning reaction substrates) from sweet orange cv. Malta Common juice to reduce colour and quality deterioration in single strength juice and during subsequent concentration. Juice of sweet orange (Citrus sinensis) cv. Malta Common fruits was extracted by screw type juice extractor, preserved in 500 ppm SO2 and clarified by using "Pectinase CCM" enzyme (0.2% for 2 h at 50 ± 2 °C). For removal of amino acids juice was passed under gravity through a glass column packed with an acidic cation exchange resin (CER), Dowex-50 W and quantity to be treated in one lot was standardized. The CER treated and untreated juices were concentrated to 15 and 30°Brix in a rotary vacuum evaporator. Results indicate that 121 ml of orange juice when passed through a glass column (5 cm internal diameter) packed with cation exchange resin (Dowex-50 W) upto a height of 8 cm, could remove about 98.4% of the amino acids with minimum losses in other juice constituents. With cation exchange resin treatment, the non-enzymatic browning and colour deterioration of orange juice semi-concentrates was reduced to about 3 folds in comparison to untreated counterparts. The retention of vitamin C and sugars was also better in semi-concentrates prepared from cation exchange resin treated juice. Thus, cation exchange resin treatment of orange juice prior to concentration and storage is highly beneficial in reduction of non-enzymatic browning, colour deterioration and retention of nutritional, sensory quality of product during preparation and storage.

Soil and sediment sample analysis for the sequential determination of natural and anthropogenic radionuclides.

PubMed

Michel, H; Levent, D; Barci, V; Barci-Funel, G; Hurel, C

2008-02-15

A new sequential method for the determination of both natural (U, Th) and anthropogenic (Sr, Cs, Pu, Am) radionuclides has been developed for application to soil and sediment samples. The procedure was optimised using a reference sediment (IAEA-368) and reference soils (IAEA-375 and IAEA-326). Reference materials were first digested using acids (leaching), 'total' acids on hot plate, and acids in microwave in order to compare the different digestion technique. Then, the separation and purification were made by anion exchange resin and selective extraction chromatography: transuranic (TRU) and strontium (SR) resins. Natural and anthropogenic alpha radionuclides were separated by uranium and tetravalent actinide (UTEVA) resin, considering different acid elution medium. Finally, alpha and gamma semiconductor spectrometer and liquid scintillation spectrometer were used to measure radionuclide activities. The results obtained for strontium-90, cesium-137, thorium-232, uranium-238, plutonium-239+240 and americium-241 isotopes by the proposed method for the reference materials provided excellent agreement with the recommended values and good chemical recoveries. Plutonium isotopes in alpha spectrometry planchet deposits could be also analysed by ICPMS.

Bilirubin and bile acids removal by haemoperfusion through synthetic resin "Persorb".

PubMed

Filip, K; Malý, J; Horký, J; Tlustáková, M; Kálal, J; Vrána, M

1990-01-01

A new type of styrene-divinylbenzene copolymer coated with polyhema was tested for biocompatibility and ability to remove bile acid, bilirubin, phenols and cholesterol in dogs with surgically induced biliary obstruction. After 4-hr hemoperfusion through a polypropylene column containing 325 g of resin, performed 7-10 days after the ligature of the cystic and common bile duct, the serum levels of bile acids, bilirubin, phenols and cholesterol decreased by 60.9 +/- 30.3% (p less than 0.001), 34.8 +/- 12.2% (p less than 0.001), 19.4 +/- 15.6% (p less than 0.001) and 15.3 +/- 4.2% (p less than 0.05), respectively. The procedure was well tolerated, no bleeding or other adverse reactions occurred. The average platelet count decreased by 19.4 +/- 15.6% (p less than 0.05). Hemoperfusion through the Czechoslovak resin coated with polyhema is safe and efficient for removal of bile acids and other protein-bound and lipid-soluble substances which accumulate in cholestatic syndromes and hepatic failure. Thus, it may play an important role in the treatment of such events as a method of artificial liver support.

Effect of different surface treatments on the shear bond strength of nanofilled composite repairs

PubMed Central

Ahmadizenouz, Ghazaleh; Esmaeili, Behnaz; Taghvaei, Arnica; Jamali, Zahra; Jafari, Toloo; Amiri Daneshvar, Farshid; Khafri, Soraya

2016-01-01

Background. Repairing aged composite resin is a challenging process. Many surface treatment options have been proposed to this end. This study evaluated the effect of different surface treatments on the shear bond strength (SBS) of nano-filled composite resin repairs. Methods. Seventy-five cylindrical specimens of a Filtek Z350XT composite resin were fabricated and stored in 37°C distilled water for 24 hours. After thermocycling, the specimens were divided into 5 groups according to the following surface treatments: no treatment (group 1); air abrasion with 50-μm aluminum oxide particles (group 2); irradiation with Er:YAG laser beams (group 3); roughening with coarse-grit diamond bur + 35% phosphoric acid (group 4); and etching with 9% hydrofluoric acid for 120 s (group 5). Another group of Filtek Z350XT composite resin samples (4×6 mm) was fabricated for the measurement of cohesive strength (group 6). A silane coupling agent and an adhesive system were applied after each surface treatment. The specimens were restored with the same composite resin and thermocycled again. A shearing force was applied to the interface in a universal testing machine. Data were analyzed using one-way ANOVA and post hoc Tukey tests (P < 0.05). Results. One-way ANOVA indicated significant differences between the groups (P < 0.05). SBS of controls was significantly lower than the other groups; differences between groups 2, 3, 4, 5 and 6 were not significant. Surface treatment with diamond bur + 35% phosphoric acid resulted in the highest bond strength. Conclusion. All the surface treatments used in this study improved the shear bond strength of nanofilled composite resin used. PMID:27092209

Green Thermosetting Factory: Novel Star-Shaped Biobased Systems and Their Thermosetting Resins; Synthesis and Characterization

NASA Astrophysics Data System (ADS)

Jahandideh, Arash

Increasing attentions toward sustainable development, economic and environmental issues have led to many attempts at replacing the petroleum-based materials with renewables. Substitution of petroleum-based platforms with green alternative technologies is beneficiary in different ways. Using bio-renewables reduces the dependency of the national plastic industry to the petroleum resources and substantially promotes the environmental profile and sustainability of the product. It is expected that the emergence of the corn-based thermosetting industry generates substantial profits for the corn production sector. Developments in the emerging biobased thermosets are spectacular from a technological point of view. However, there are still several disadvantages associated with the current biobased thermosetting resins, e.g. low processability, environmental issues, expensive sources and poor thermomechanical properties. Use of natural fibers not only contributes to the production of a more environmentally friendly product, but also has advantages such as low-weight product and low manufacturing costs. The results of this study show a possibility of production of biocomposites made from natural fibers and star-shaped resin, synthesized from corn-based materials (lactic acid and itaconic acid) and different multihydroxyl core molecules. These resins were synthesized via two-steps strategy: polycondensation of the monomers with the core molecules followed by end-functionalization of the branches by methacrylic anhydride or itaconic acid. The results have shown that these resin are capable of competing with or even surpassing fossil fuel based resins in terms of cost and eco-friendliness aspect. Inexpensive biobased raw material, better environmental profile, low viscosity, and better processability of the matrix along with better thermomechanical properties of the produced biocomposites are of advantages expected for these systems.

Arnica montana L. - a plant of healing: review.

PubMed

Kriplani, Priyanka; Guarve, Kumar; Baghael, Uttam S

2017-08-01

Arnica montana is a widely used therapeutic plant used traditionally to treat various ailments. The objective of this study was to evaluate the botany, phytochemistry and ethnopharmacology along with special emphasis given on pharmacological activity of plant A. montana. The plant extracts have been reported to possess antibacterial, antitumor, antioxidant, anti-inflammatory, antifungal and immunomodulatory activity. A wide range of chemical compounds including sesquiterpene lactones and their short-chain carbonic acid esters, flavonoids, carotenoids, essential oils, diterpenes, arnidiol, pyrrolizidine alkaloids, coumarins, phenolic acids, lignans and oligosaccharides, etc., are found in different parts of the plant. It has been scrutinized that extensive research has been carried out to explore the therapeutic potential of flowers of the plant. Therefore, investigations should be carried out to explore the therapeutic potential of other parts of the plant for better therapeutic utilization. © 2017 Royal Pharmaceutical Society.

Effects of reaction pH on properties and performance of urea-formaldehyde resins

Treesearch

Chung-Yun Hse; Zhi-Yuan Xia; Bunchiro Tomita

1994-01-01

Urea formaldehyde resins were formulated with combination variables of three reaction pH (1.0, 4.8, and 8.0) and four molar ratios of formaldehyde to urea (2.5, 3.0, 3.5, and 4.0). The resins were prepared by placing all formaldehyde and water in reaction kettle and pH was adjusted with sulfuric acid and sodium hydroxide, respectively. Urea was added in 15 equal parts...

Insect-Induced Conifer Defense. White Pine Weevil and Methyl Jasmonate Induce Traumatic Resinosis, de Novo Formed Volatile Emissions, and Accumulation of Terpenoid Synthase and Putative Octadecanoid Pathway Transcripts in Sitka Spruce1[w

PubMed Central

Miller, Barbara; Madilao, Lufiani L.; Ralph, Steven; Bohlmann, Jörg

2005-01-01

Stem-boring insects and methyl jasmonate (MeJA) are thought to induce similar complex chemical and anatomical defenses in conifers. To compare insect- and MeJA-induced terpenoid responses, we analyzed traumatic oleoresin mixtures, emissions of terpenoid volatiles, and expression of terpenoid synthase (TPS) genes in Sitka spruce (Picea sitchensis) following attack by white pine weevils (Pissodes strobi) or application of MeJA. Both insects and MeJA caused traumatic resin accumulation in stems, with more accumulation induced by the weevils. Weevil-induced terpenoid emission profiles were also more complex than emissions induced by MeJA. Weevil feeding caused a rapid release of a blend of monoterpene olefins, presumably by passive evaporation of resin compounds from stem feeding sites. These compounds were not found in MeJA-induced emissions. Both weevils and MeJA caused delayed, diurnal emissions of (−)-linalool, indicating induced de novo biosynthesis of this compound. TPS transcripts strongly increased in stems upon insect attack or MeJA treatment. Time courses and intensity of induced TPS transcripts were different for monoterpene synthases, sesquiterpene synthases, and diterpene synthases. Increased levels of weevil- and MeJA-induced TPS transcripts accompanied major changes in terpenoid accumulation in stems. Induced TPS expression profiles in needles were less complex than those in stems and matched induced de novo emissions of (−)-linalool. Overall, weevils and MeJA induced similar, but not identical, terpenoid defense responses in Sitka spruce. Findings of insect- and MeJA-induced accumulation of allene oxide synthase-like and allene oxide cyclase-like transcripts are discussed in the context of traumatic resinosis and induced volatile emissions in this gymnosperm system. PMID:15618433

Sensomics analysis of key bitter compounds in the hard resin of hops (Humulus lupulus L.) and their contribution to the bitter profile of Pilsner-type beer.

PubMed

Dresel, Michael; Dunkel, Andreas; Hofmann, Thomas

2015-04-08

Recent brewing trials indicated the occurrence of valuable bitter compounds in the hard resin fraction of hop. Aiming at the discovery of these compounds, hop's ε-resin was separated by means of a sensory guided fractionation approach and the key taste molecules were identified by means of UV/vis, LC-TOF-MS, and 1D/2D-NMR studies as well as synthetic experiments. Besides a series of literature known xanthohumol derivatives, multifidol glucosides, flavon-3-on glycosides, and p-coumaric acid esters, a total of 11 bitter tastants are reported for the first time, namely, 1",2"-dihydroxanthohumol F, 4'-hydroxytunicatachalcone, isoxantholupon, 1-methoxy-4-prenylphloroglucinol, dihydrocyclohumulohydrochinone, xanthohumols M, N, and P, and isoxanthohumols M, N, and P, respectively. Human sensory analysis revealed low bitter recognition threshold concentrations ranging from 5 (co-multifidol glucopyranoside) to 198 μmol/L (trans-p-coumaric acid ethyl ester) depending on their chemical structure. For the first time, LC-MS/MS quantitation of these taste compounds in Pilsner-type beer, followed by taste re-engineering experiments, revealed the additive contribution of iso-α-acids and the identified hard resin components to be truly necessary and sufficient for constructing the authentic bitter percept of beer. Finally, brewing trails using the ε-resin as the only hop source impressively demonstrated the possibility to produce beverages strongly enriched with prenylated hop flavonoids.

Drought stress alters the concentration of wood terpenoids in Scots pine and Norway spruce seedlings.

PubMed

Turtola, Satu; Manninen, Anne-Marja; Rikala, Risto; Kainulainen, Pirjo

2003-09-01

Drought is known to have an impact on the resistance of conifers to various pests, for example, by affecting resin flow in trees. Little is known, however, about the quantitative and qualitative changes in resin when trees are growing in low moisture conditions. We exposed Scots pine (Pinus sylvestris L.) and Norway spruce (Picea abies (L.) Karst.) seedlings to medium and severe drought stress for two growing seasons and analyzed the monoterpenes and resin acids in the main stem wood after two years of treatment. In addition to secondary chemistry, we measured the level of nutrients in the needles and the growth response of seedlings. After the first year of treatment, drought stress did not affect the growth of seedlings, but in the second year, shoot growth was retarded, especially in Scots pine. In both conifer species, severe drought increased the concentrations of several individual monoterpenes and resin acids. Total monoterpenes and resin acids were 39 and 32% higher in severe drought-treated Scots pine seedlings than in the controls, and 35 and 45% higher in Norway spruce seedlings. In Scots pine needles, the concentrations of nitrogen and phosphorus increased, while magnesium and calcium decreased compared to controls. In Norway spruce needles, nutrient concentrations were not affected. The results suggest that drought stress substantially affects both the growth of conifers and the chemical quality of the wood. We discuss the potential trade-off in growth and defense of small conifer seedlings.

Parallel solid-phase synthesis and high-throughput 1H NMR evaluation of a 96-member 1,2,4-trisubstituted-pyrimidin-6-one-5-carboxylic acid library.

PubMed

Hamper, Bruce C; Kesselring, Allen S; Chott, Robert C; Yang, Shengtian

2009-01-01

A solid-phase organic synthesis method has been developed for the preparation of trisubstituted pyrimidin-6-one carboxylic acids 12, which allows elaboration to a 3-dimensional combinatorial library. Three substituents are introduced by initial Knoevenagel condensation of an aldehyde and malonate ester resin 7 to give resin bound 1. Cyclization of 1 with an N-substituted amidine 10, oxidation, and cleavage afforded pyrimidinone 12. The initial solid-phase reaction sequence was followed by gel-phase (19)FNMR and direct-cleavage (1)H NMR of intermediate resins to determine the optimal conditions. The scope of the method for library production was determined by investigation of a 3 x 4 pilot library of twelve compounds. Cyclocondensation of N-methylamidines and 7 followed by CAN oxidation gave mixtures of the resin bound pyrimidin-6-one 11 and the regioisomeric pyrimidin-4-one 15, which after cleavage from the resin afforded a nearly 1:1 mixture of pyrimidin-6-one and pyrimidin-4-one carboxylic acids 12 and 16, respectively. The regiochemical assignment was confirmed by ROESY1D and gHMBC NMR experiments. A library was prepared using 8 aldehydes, 3 nitriles, and 4 amines to give a full combinatorial set of 96 pyrimidinones 12. Confirmation of structural identity and purity was carried out by LCMS using coupled ELS detection and by high-throughput flow (1)H NMR.

Metal binding characterization and conformational studies using Raman microscopy of resin-bound poly(aspartic acid).

PubMed

Stair, Jacqueline L; Holcombe, James A

2007-03-01

The metal binding capacities, conditional stability constants, and secondary structure of immobilized polyaspartic acid (PLAsp) (n = 6, 20, and 30) on TentaGel resin were determined when binding Mg2+, Co2+, Cd2+, and Ni2+. Metal binding to the synthesized peptides was evaluated using breakthrough curves from a packed microcolumn and flame atomic absorption spectrophotometry (FAAS) detection. The metal capacities reached values of 590, 2160, and 3710 mumol of metal/g of resin for the 6-mer, 20-mer, and 30-mer, respectively, and this resulted in 2-3 residues per metal for all peptides and metals tested. Surprisingly, the concentrated environment of the resin along with the spatial distribution of attachment groups allowed for most residues to participate in metal binding regardless of the peptide length. Conditional stability constants calculated using single metal binding isotherms indicated that binding strength decreased as the chain length increased on the resin. Raman microscopy on single beads was used to determine PLAsp secondary structure, and all peptides were of a mixed conformation (i.e., beta-sheets, alpha-helices, random chain, etc.) during neutral conditioning and metal binding. Uniquely, the longer 20-mer and 30-mer peptides showed a distinct change from a mixed conformation to beta-sheets and alpha-helices during metal release with acid. This study confirms that metal release by longer immobilized peptides is often assisted by a conformational change, which easily spoils the binding cavity, while shorter peptides may release metal primarily by H+ displacement.

Marginal integrity of low-shrinkage and methacrylate-based composite resins: Effect of three different hemostatic agents

PubMed Central

Khoroushi, Maryam; Sahraneshin-Samani, Mahsa

2016-01-01

Background Moisture control is very important in restorative procedures in dentistry. Use of hemostatic agents helps control moisture; however, they might result in changes on enamel and dentin surfaces, affecting composite resin bond quality. The aim of this in vitro study was to evaluate the marginal microleakage of two different composite resins with the use of three different hemostatic agents. Material and Methods Standardized Class V cavities were prepared on the buccal and lingual surfaces of 48 premolars with cervical margins 1 mm apical to the cementoenamel junction (CEJ). The samples were randomly divided into 8 groups. In groups 1 to 4, an etch-and-rinse adhesive (Adper Single Bond) was applied as the bonding system, followed by exposure to different hemostatic agent: group 1: no hemostatic agent (control); group 2: ViscoStat; group 3: ViscoStat Clear; and group 4: trichloracetic acid, as hemostatic agents. The cavities were restored with Z-250 composite resin. In group 5 to 8 Silorane System Adhesive (Filtek P90 Adhesive) was applied as a bonding agent, followed by exposure to different hemostatic agents in a manner similar to that in groups 1to 4. The cavities were restored with Filtek P90, a low-shrinkage composite resin. The samples in each group were evaluated for dye penetration under a stereomicroscope at ×36 after 24 hours and a 500-round thermocycling procedure at enamel and dentin margins. Statistical analysis was carried out using Kruskal-Wallis and Mann-Whitney tests (α=0.05). Results Z-250 composite resin exhibited significantly higher dentin microleakage scores compared to Filtek P90 (P = 0.004). Trichloracetic acid increased dentin microleakage with Filtek P90 (P=0.033). Conclusions Under the limitations of this in vitro study, application of hemostatic agents did not affect microleakage of the two tested composite resins except for trichloracetic acid that increased marginal microleakage when used with Filtek P90. Key words:Composite resin, dental leakage, hemostatics, silorane system adhesive. PMID:27034759

Influence of laser structuring of PEEK, PEEK-GF30 and PEEK-CF30 surfaces on the shear bond strength to a resin cement.

PubMed

Henriques, Bruno; Fabris, Douglas; Mesquita-Guimarães, Joana; Sousa, Anne C; Hammes, Nathalia; Souza, Júlio C M; Silva, Filipe S; Fredel, Márcio C

2018-08-01

The aim of this study was to evaluate the influence of a surface conditioning technique using laser ablation and acid etching on PEEK substrate on its bonding strength to a resin cement. Cylindrical specimens of unfilled PEEK, 30% glass fiber reinforced PEEK and 30% carbon fiber reinforced PEEK were separated in four groups according to the following surface treatments: acid etching with H 2 SO 4 , laser ablation with 200 µm holes spaced 400 µm apart (D2E4), laser ablation with 200 µm holes spaced 600 µm apart (D2E6), and laser ablation (D2E4) followed by acid etching. A dual-curing resin cement (Allcem CORE) was then applied to the PEEK surface. Specimens were aged in distilled water at 37 °C for 24 h. Shear bond strength tests were performed to the fracture of the samples. Two-way ANOVA statistical analysis was performed with a significance level of 0.05. Scanning electron microscopy analysis was performed to analyse the conditioned and fracture surfaces. SEM images of the test interfaces showed that the resin cement could not flow in the holes designed by the laser ablation on the PEEK surface. The shear bond strength of PEEK to resin cement was not improved by the surface modification of the PEEK. Also, there was a statistically significant decrease in shear bond strength for unfilled PEEK specimens. On carbon or glass reinforced PEEK, the change was not significant. SEM images of the fracture surfaces revealed that the failure mode was mainly adhesive. Although laser ablation promoted the PEEK surface modification by the formation of retentive holes, the test resin cement could not thoroughly flow on the rough modified surfaces to establish an effective mechanical interlocking. That negatively affected the shear bonding strength of PEEK to the resin cement. Further studies should be carried out to increase the bonding between PEEK and resin cements. Copyright © 2018 Elsevier Ltd. All rights reserved.

Selective concentration of aromatic bases from water with a resin adsorbent

USGS Publications Warehouse

Stuber, H.A.; Leenheer, J.A.

1983-01-01

Aromatic bases are concentrated from water on columns of a resin adsorbent and recovered by aqueous-acid elution. The degree of concentration attainable depends on the ratio of the capacity factor (k) of the neutral form of the amine to that of the ionized form. Capacity factors of ionic forms of amines on XAD-8 resin (a methylacrylic ester polymer) are greater than zero, ranging from 20 to 250 times lower than those of their neutral forms; they increase with increasing hydrophobicity of the amine. Thus, desorption by acid is an edition (k during desorption >0) rather than a displacement (k during desorption = 0) process. The degree of concentration attainable on XAD-8 resin varies with the hydrophobicity of the amine, being limited for hydrophilic solutes (for example, pyridine) by small neutral-form k's, reaching a maximum for amines of intermediate hydrophobicity (for example, quinoline), and decreasing for more hydrophobc solutes (for example, acridine) because of their large ionic-form k's.

Biocatalytic Synthesis of Epoxy Resins from Fatty Acids as a Versatile Route for the Formation of Polymer Thermosets with Tunable Properties.

PubMed

Torron, Susana; Semlitsch, Stefan; Martinelle, Mats; Johansson, Mats

2016-12-12

The work herein presented describes the synthesis and polymerization of series of bio-based epoxy resins prepared through lipase catalyzed transesterification. The epoxy-functional polyester resins with various architectures (linear, tri-branched, and tetra-branched) were synthesized through condensation of fatty acids derived from epoxidized soybean oil and linseed oil with three different hydroxyl cores under bulk conditions. The selectivity of the lipases toward esterification/transesterification reactions allowed the formation of macromers with up to 12 epoxides in the backbone. The high degree of functionality of the resins resulted in polymer thermosets with T g values ranging from -25 to over 100 °C prepared through cationic polymerization. The determining parameters of the synthesis and the mechanism for the formation of the species were determined through kinetic studies by 1 H NMR, SEC, and molecular modeling studies. The correlation between macromer structure and thermoset properties was studied through real-time FTIR measurements, DSC, and DMA.

Preparative separation and purification of rosmarinic acid from perilla seed meal via combined column chromatography.

PubMed

Tang, Weizhuo; Sun, Baoshan; Zhao, Yuqing

2014-02-01

In this study, the preparative separation and purification of rosmarinic acid (RA) from perilla seed meal (PSM), which is a by-product of edible oil production, was achieved using combined column chromatography over macroporous and polyamide resins. To optimize the RA enrichment process, the performance and separation characteristics of nine selected macroporous resins with different chemical and physical properties were investigated. SP825 resin was the most effective: the content of RA increased from 0.27% in the original extract to 16.58% in the 50% ethanol fraction (a 61.4-fold increase). During further purification treatment on polyamide resin, 90.23% pure RA could be obtained in the 70% ethanol fraction. RA with a higher purity (>95%) could also be easily obtained using one crystallization operation. The proposed method is simple, easily operated, cost-effective, and environmentally friendly and is suitable for both large-scale RA production and waste management. Copyright © 2013 Elsevier B.V. All rights reserved.

Maintenance and Preservation of Concrete Structures. Report 3. Abrasion-Erosion Resistance of Concrete.

DTIC Science & Technology

1980-07-01

ORG. REPORT NUMBER 7. AUTH R(s) 11. CONTRACT OR GRANT NUMBER(&) Tony C Liu C I PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT. PROJECT... organic acids, alkalis, solvents, etc. Polyurethane 25. Two types of elastomeric polyurethane systems were investi- gated: T19 and T21. a. The T19 specimens...polymer with a viscosity of about 450 cps at 250 C. The catalyst used to polymerize the resin is an organic acid. The mixing ratio of the resin to

Influence of caries infiltrant contamination on shear bond strength of different adhesives to dentin.

PubMed

Jia, Liuhe; Stawarczyk, Bogna; Schmidlin, Patrick R; Attin, Thomas; Wiegand, Annette

2013-03-01

To analyze whether the contamination with a caries infiltrant system impairs the adhesive performance of etch-and-rinse and self-etching adhesives on dentin. Dentin contamination with the caries infiltrant system (Icon, DMG) was simulated by applying either hydrochloric acid (15 % HCl, Icon Etch, 15 s), the resin infiltrant (Icon infiltrant, 4 min), or both prior to the application of the respective adhesives (each group n = 10). In the control groups, the etch-and-rinse adhesive (Optibond FL, Kerr) and the self-etching adhesive (iBOND Self Etch, Hereaus) were applied without former contamination with the infiltrant system. Additionally, the adhesive performance of the resin infiltrant alone was tested. Shear bond strength of a nano-hybrid composite was analyzed after thermocycling (5,000×, 5-55°C) of the specimens and analyzed by ANOVA/Scheffé post hoc tests (p < 0.05) and Weibull statistics. Failure mode was inspected under a stereomicroscope at × 25 magnification. Contamination with the resin infiltrant alone did not impair shear bond strength, while contamination with hydrochloric acid or with hydrochloric acid and the resin infiltrant reduced shear bond strength (MPa) of the adhesives (Optibond FL: 20.5 ± 3.6, iBOND Self Etch: 17.9 ± 2.6) significantly. Hydrochloric acid contamination increased the number of adhesive failures. The adhesive performance of the caries infiltrant system alone was insufficient. The contamination with the caries infiltrant system impaired the shear bond strength of conventional dental adhesives. Contamination of the caries infiltrant system on dentin should be avoided due to the detrimental effect of hydrochloric acid etching.

Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

PubMed

Kara, Derya; Fisher, Andrew; Hill, Steve J

2009-06-15

A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

Immunomodulatory Effects of Diterpene Quinone Derivatives from the Roots of Horminum pyrenaicum in Human PBMC

PubMed Central

Becker, K.; Schwaiger, S.; Waltenberger, B.; Pezzei, C. K.; Schennach, H.

2018-01-01

Several phytochemicals were shown to interfere with redox biology in the human system. Moreover, redox biochemistry is crucially involved in the orchestration of immunological cascades. When screening for immunomodulatory compounds, the two interferon gamma- (IFN-γ-) dependent immunometabolic pathways of tryptophan breakdown via indoleamine 2,3-dioxygenase-1 (IDO-1) and neopterin formation by GTP-cyclohydrolase 1 (GTP-CH-I) represent prominent targets, as IFN-γ-related signaling is strongly sensitive to oxidative triggers. Herein, the analysis of these pathway activities in human peripheral mononuclear cells was successfully applied in a bioactivity-guided fractionation strategy to screen for anti-inflammatory substances contained in the root of Horminum (H.) pyrenaicum L. (syn. Dragon's mouth), the only representative of the monophyletic genus Horminum. Four abietane diterpene quinone derivatives (horminone, 7-O-acetylhorminone, inuroyleanol and its 15,16-dehydro-derivative, a novel natural product), two nor-abietane diterpene quinones (agastaquinone and 3-deoxyagastaquinone) and two abeo 18 (4 → 3) abietane diterpene quinones (agastol and its 15,16-dehydro-derivative) could be identified. These compounds were able to dose-dependently suppress the above mentioned pathways with different potency. Beside the description of new active compounds, this study demonstrates the feasibility of integrating IDO-1 and GTP-CH-I activity in the search for novel anti-inflammatory compounds, which can then be directed towards a more detailed mode of action analysis. PMID:29576845

Fatigue of the Resin-Enamel Bonded Interface and the Mechanisms of Failure

PubMed Central

Yahyazadehfar, Mobin; Mutluay, Mustafa Murat; Majd, Hessam; Ryou, Heonjune; Arola, Dwayne

2013-01-01

The durability of adhesive bonds to enamel and dentin and the mechanisms of degradation caused by cyclic loading are important to the survival of composite restorations. In this study a novel method of evaluation was used to determine the strength of resin-enamel bonded interfaces under both static and cyclic loading, and to identify the mechanisms of failure. Specimens with twin interfaces of enamel bonded to commercial resin composite were loaded in monotonic and cyclic 4-point flexure to failure within a hydrated environment. Results for the resin-enamel interface were compared with those for the resin composite (control) and values reported for resin-dentin adhesive bonds. Under both modes of loading the strength of the resin-enamel interface was significantly (p≤0.0001) lower than that of the resin composite and the resin-dentin bonded interface. Fatigue failure of the interface occurred predominately by fracture of enamel, adjacent to the interface, and not due to adhesive failures. In the absence of water aging or acid production of biofilms, the durability of adhesive bonds to enamel is lower than that achieved in dentin bonding. PMID:23571321

Method to upgrade bio-oils to fuel and bio-crude

DOEpatents

Steele, Philip H; Pittman, Jr., Charles U; Ingram, Jr., Leonard L; Gajjela, Sanjeev; Zhang, Zhijun; Bhattacharya, Priyanka

2013-12-10

This invention relates to a method and device to produce esterified, olefinated/esterified, or thermochemolytic reacted bio-oils as fuels. The olefinated/esterified product may be utilized as a biocrude for input to a refinery, either alone or in combination with petroleum crude oils. The bio-oil esterification reaction is catalyzed by addition of alcohol and acid catalyst. The olefination/esterification reaction is catalyzed by addition of resin acid or other heterogeneous catalyst to catalyze olefins added to previously etherified bio-oil; the olefins and alcohol may also be simultaneously combined and catalyzed by addition of resin acid or other heterogeneous catalyst to produce the olefinated/esterified product.

21 CFR 173.5 - Acrylate-acrylamide resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... and acrylic acid, with the greater part of the polymer being composed of acrylamide units. (2) Sodium polyacrylate-acrylamide resin is produced by the polymerization and subsequent hydrolysis of acrylonitrile in a sodium silicate-sodium hydroxide aqueous solution, with the greater part of the polymer being composed of...

21 CFR 173.5 - Acrylate-acrylamide resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... and acrylic acid, with the greater part of the polymer being composed of acrylamide units. (2) Sodium polyacrylate-acrylamide resin is produced by the polymerization and subsequent hydrolysis of acrylonitrile in a sodium silicate-sodium hydroxide aqueous solution, with the greater part of the polymer being composed of...

ADSORPTION OF CERIUM VALUES FROM AQUEOUS SOLUTIONS

DOEpatents

Roberts, F.P.

1963-08-13

Cerium can be removed from aqueous nitric acid (2 to 13 M) solutions by passing the latter over a PbO/sub 2/-containing anion exchange resin. The cerium is taken up by the resin, while any lanthanides, yttrium, and strontium present remain in the solution. (AEC)

EVALUATION OF METHODS FOR THE ISOLATION OR CONCENTRATION OF ORGANIC SUBSTANCES FROM WATER USING XAD-4 QUATERNARY RESIN

EPA Science Inventory

A synthetic resin (Amberlite XAD-4 Quaternary in the OH- form) was evaluated as an adsorption medium for the concentration/isolation of acids, amines, aldehydes, carbohydrates, chlorobiphenyls, esters, hydrocarbons, ketones, phenols, polynuclear aromatic hydrocarbons, and trihalo...

Synthesis of cross-linked chitosan modified with the glycine moiety for the collection/concentration of bismuth in aquatic samples for ICP-MS determination.

PubMed

Oshita, Koji; Noguchi, Osamu; Oshima, Mitsuko; Motomizu, Shoji

2007-10-01

A chelating resin, cross-linked chitosan modified with the glycine moiety (glycine-type chitosan resin), was developed for the collection and concentration of bismuth in aquatic samples for ICP-MS measurements. The adsorption behavior of bismuth and 55 elements on glycine-type chitosan resin was systematically examined by passing a sample solution containing 56 elements through a mini-column packed with the resin (wet volume; 1 ml). After eluting the elements adsorbed on the resin with nitric acid, the eluates were measured by ICP-MS. The glycine-type chitosan resin could adsorb several cations by a chelating mechanism and several oxoanions by an anion-exchange mechanism. Especially, the resin could adsorb almost 100% Bi(III) over a wide pH region from pH 2 to 6. Bismuth could be strongly adsorbed at pH 3, and eluted quantitatively with 10 ml of 3 M nitric acid. A column pretreatment method with the glycine-type chitosan resin was used prior to removal of high concentrations of matrices in a seawater sample and the preconcentration of trace bismuth in river water samples for ICP-MS measurements. The column pretreatment method was also applied to the determination of bismuth in real samples by ICP-MS. The LOD of bismuth was 0.1 pg ml(-1) by 10-fold column preconcentration for ICP-MS measurements. The analytical results for bismuth in sea and river water samples by ICP-MS were 22.9 +/- 0.5 pg ml(-1) (RSD, 2.2%) and 2.08 +/- 0.05 pg ml(-1) (RSD, 2.4%), respectively.

Synthesis, characterization and application of ion exchange resin as a slow-release fertilizer for wheat cultivation in space

NASA Astrophysics Data System (ADS)

Li, Bowei; Dong, Chen; Chu, Zhengpei; Zhang, Weizhe; Wang, Minjuan; Liu, Hong; Xie, Beizhen

2016-10-01

In addition to the bio-regenerative air revitalization, water recycling and waste management systems and their associated challenges, enhancing the crop yield with less fertilizer input for sustainable food production in space is also a challenge that needs to be overcome. The purpose of this study is to investigate the feasibility of applying ion exchange resin as a slow-release fertilizer for wheat cultivation in space. Strong-acid cationic exchange resins and weak-base anion exchange resins soaked in 1X, 5X, 10X and 15X Hoagland nutrient solutions, respectively, were used as fertilizers in clinoptilolite to cultivate wheat plants, and the morphological and physiological characteristics of the wheat plants were studied and compared with that of the wheat planted in vermiculite and nutrient solutions. The results showed that more ions were attached on the surface of the ion exchange resins as the solution concentration increased. After 14 days, the fresh weight of wheat planted in the ion exchange resin-clinoptilolite (IER-clinoptilolite) treated with 10X and 15X solutions were 190% and 192% higher than that of wheat planted in nutrient solution with the same concentration. Chlorophyll content of wheat plants cultivated in the two kinds of solid medium is significantly higher than that of liquid cultivation. The lowest peroxidase (POD) activity and malondialdehyde (MDA) contents of wheat plants cultivated in the IER-clinoptilolite appeared on the 14th day. According to all the experimental data, it's promising to produce slow-release nutrient fertilizer by using strong-acid cationic exchange resins and weak-base anion exchange resins for wheat cultivation in space.

Simultaneous separation and detection of actinides in acidic solutions using an extractive scintillating resin.

PubMed

Roane, J E; DeVol, T A

2002-11-01

An extractive scintillating resin was evaluated for the simultaneous separation and detection of actinides in acidic solutions. The transuranic extractive scintillating (TRU-ES) resin is composed of an inert macroporous polystyrene core impregnated with organic fluors (diphenyloxazole and 1,4-bis-(4-methyl-5-phenyl-2-oxazolyl)benzene) and an extractant (octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide in tributyl phosphate). The TRU-ES resin was packed into FEP Teflon tubing to produce a flow cell (0.2-mL free column volume), which is placed into a scintillation detection system to obtain pulse height spectra and time series data during loading and elution of actinides onto/from the resin. The alpha-particle absolute detection efficiencies ranged from 77% to 96.5%, depending on the alpha energy and quench. In addition to the on-line analyses, off-line analyses of the effluent can be conducted using conventional detection methods. The TRU-ES resin was applied to the quantification of a mixed radionuclide solution and two actual waste samples. The on-line characterization of the mixed radionuclide solution was within 10% of the reported activities whereas the agreement with the waste samples was not as good due to sorption onto the sample container walls and the oxidation state of plutonium. Agreement between the on-line and off-line analyses was within 35% of one another for both waste samples.

Separation of arsenic(III) and arsenic(V) in ground waters by ion-exchange

USGS Publications Warehouse

Ficklin, W.H.

1983-01-01

The predominant species of arsenic in ground water are probably arsenite and arsenate. These can be separated with a strong anion-exchange resin (Dowex 1 ?? 8; 100-200 mesh, acetate form) in a 10 cm ?? 7 mm column. Samples are filtered and acidified with concentrated hydrochloric acid (1 ml per 100 ml of sample) at the sample site. Five ml of the acidified sample are used for the separation. At this acidity, As(III) passes through the acetate-form resin, and As(V) is retained. As(V) is eluted by passage of 0.12M hydrochloric acid through the column (resulting in conversion of the resin back into the chloride form). Samples are collected in 5-ml portions up to a total of 20 ml. The arsenic concentration in each portion is determined by graphite-furnace atomic-absorption spectrophotometry. The first two fractions give the As(III) concentration and the last two the As(V) concentration. The detection limit for the concentration of each species is 1 ??g l. ?? 1983.

Physical characteristics of the paper filter and low cafestol content filter coffee brews.

PubMed

Rendón, Mery Yovana; Dos Santos Scholz, Maria Brígida; Bragagnolo, Neura

2018-06-01

The results found in the literature concerning the effect of consuming filter coffee brews on increasing the blood cholesterol levels due to the presence of diterpenes, are divergent. Thus the present research evaluated the diterpene (cafestol and kahweol) concentrations in filter coffee brews prepared with paper filters of different sizes, colors and origins (Brazil, Japan, The United States of America, Germany, France and the Netherlands), with and without micro perforations. This is the first study that reports the physical characteristics of paper filter and its importance to obtain filter coffee brew with low cafestol content. Thus, a sample of Catuai cultivar coffee with high cafestol content was roasted to a medium-light degree and used to prepare the brews in a 1:10 ratio (coffee powder to water). The diterpenes were extracted by direct saponification and quantified and identified by HPLC-DAD-MS/MS. The paper filters were physically characterized by measuring their grammage, and the fat permeation rate calculated in order to better understand the differences between the filters which allow one to obtain higher or lower diterpene contents. The cafestol and kahweol concentrations in the brews varied from 1.62 to 2.98 mg/L and from 0.73 to 1.96 mg/L, respectively. The highest cafestol and kahweol concentrations were obtained using paper filters with micro perforations, considering similar sized paper filters. The paper filters showed high fat permeability and grammages between 50.46 and 67.48 g/m 2 . The diterpene retention capacities of the filters produced in the different countries were similar. The results showed that the porosity of the paper filter and the particle size of the ground roasted coffee were determinant factors in obtaining filter coffee brews with lower cafestol contents. Copyright © 2018 Elsevier Ltd. All rights reserved.

Phenylethynyl Containing Reactive Additives

NASA Technical Reports Server (NTRS)

Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

2002-01-01

Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidi none to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

URANIUM RECOVERY AND PURIFICATION PROCESS AND PRODUCTION OF HIGH PURITY URANIUM TETRAFLUORIDE

DOEpatents

Bailes, R.H.; Long, R.S.; Grinstead, R.R.

1957-09-17

A process is described wherein an anionic exchange technique is employed to separate uramium from a large variety of impurities. Very efficient and economical purification of contamimated uranium can be achieved by treatment of the contaminated uranium to produce a solution containing a high concentration of chloride. Under these conditions the uranium exists as an aniomic chloride complex. Then the uranium chloride complex is adsorbed from the solution on an aniomic exchange resin, whereby a portion of the impurities remain in the solution and others are retained with the uramium by the resin. The adsorbed impurities are then removed by washing the resin with pure concentrated hydrochloric acid, after which operation the uranium is eluted with pure water yielding an acidic uranyl chloride solution of high purity.

Investigation of bracket bonding for orthodontic treatments using en-face optical coherence tomography

NASA Astrophysics Data System (ADS)

Sinescu, Cosmin; Negrutiu, Meda L.; Hughes, Michael; Bradu, Adrian; Todea, Carmen; Rominu, Roxana; Dodenciu, Dorin; Laissue, Philippe L.; Podoleanu, Adrian G.

2008-04-01

Despite good diagnosis and treatment planning, orthodontic treatment can fail if bonding fails. It is now common practice to address the aesthetic appearance of patients using aesthetic brackets instead of metal ones. Therefore, bonding aesthetic brackets has become an issue for orthodontists today. Orthodontic bonding is mainly achieved using composite resin but can also be performed with glass ionomer or resin cements. For improving the quality of bonding, the enamel is acid etched for 30 seconds with 38% phosphoric acid and then a bonding agent is applied. In our study we investigated and compared the quality of bonding between ceramic brackets, polymeric brackets and enamel, respectively using a new investigation method-OCT. The aim of our study was to evaluate the resin layer at the bracket base-tooth interface.

Phenylethynyl Containing Reactive Additives

NASA Technical Reports Server (NTRS)

Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

2002-01-01

Phenylethynyl containing reactive additives were prepared from aromatic diamine, containing phenylethvnvl groups and various ratios of phthalic anhydride and 4-phenylethynviphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pvrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

In vitro and in vivo antitumor effect of trachylobane-360, a diterpene from Xylopia langsdorffiana.

PubMed

Pita, João Carlos Lima Rodrigues; Xavier, Aline Lira; de Sousa, Tatyanna Kelvia Gomes; Mangueira, Vivianne Mendes; Tavares, Josean Fechine; de Oliveira Júnior, Robson José; Veras, Robson Cavalcante; Pessoa, Hilzeth de Luna Freire; da Silva, Marcelo Sobral; Morelli, Sandra; Ávila, Veridiana de Melo Rodrigues; da Silva, Teresinha Gonçalves; Diniz, Margareth de Fátima Formiga Melo; Castello-Branco, Marianna Vieira Sobral

2012-08-10

Trachylobane-360 (ent-7α-acetoxytrachyloban-18-oic acid) was isolated from Xylopia langsdorffiana. Studies have shown that it has weak cytotoxic activity against tumor and non-tumor cells. This study investigated the in vitro and in vivo antitumor effects of trachylobane-360, as well as its cytotoxicity in mouse erythrocytes. In order to evaluate the in vivo toxicological aspects related to trachylobane-360 administration, hematological, biochemical and histopathological analyses of the treated animals were performed. The compound exhibited a concentration-dependent effect in inducing hemolysis with HC₅₀ of 273.6 µM, and a moderate in vitro concentration-dependent inhibitory effect on the proliferation of sarcoma 180 cells with IC₅₀ values of 150.8 µM and 150.4 µM, evaluated by the trypan blue exclusion test and MTT reduction assay, respectively. The in vivo inhibition rates of sarcoma 180 tumor development were 45.60, 71.99 and 80.06% at doses of 12.5 and 25 mg/kg of trachylobane-360 and 25 mg/kg of 5-FU, respectively. Biochemical parameters were not altered. Leukopenia was observed after 5-FU treatment, but this effect was not seen with trachylobane-360 treatment. The histopathological analysis of liver and kidney showed that both organs were mildly affected by trachylobane-360 treatment. Trachylobane-360 showed no immunosuppressive effect. In conclusion, these data reinforce the anticancer potential of this natural diterpene.

Metabolomics reveals biotic and abiotic elicitor effects on the soft coral Sarcophyton ehrenbergi terpenoid content.

PubMed

Farag, Mohamed A; Al-Mahdy, Dalia A; Meyer, Achim; Westphal, Hildegard; Wessjohann, Ludger A

2017-04-05

The effects of six biotic and abiotic elicitors, i.e. MeJA (methyl jasmonate), SA (salicylic acid), ZnCl 2 , glutathione and β-glucan BG (fungal elicitor), and wounding, on the secondary metabolite accumulation in the soft coral Sarcophyton ehrenbergi were assessed. Upon elicitation, metabolites were extracted and analysed by ultra-performance liquid chromatography-mass spectrometry (UPLC-MS). Except for MeJA, no differences in photosynthetic efficiency were observed after treatments, suggesting the absence of a remarkable stress on primary production. Chemometric analyses of UPLC-MS data showed clear segregation of SA and ZnCl 2 elicited samples at 24 and 48 h post elicitation. Levels of acetylated diterpene and sterol viz., sarcophytonolide I and cholesteryl acetate, was increased in ZnCl 2 and SA groups, respectively, suggesting an activation of specific acetyl transferases. Post elicitation, sarcophytonolide I level increased 132 and 17-folds at 48 h in 0.1 mM SA and 1 mM ZnCl 2 groups, respectively. Interestingly, decrease in sarcophine, a major diterpene was observed only in response to ZnCl 2 , whereas no change was observed in sesquiterpene content following treatments. To the best of our knowledge, this study provides the first documentation for elicitation effects on a soft corals secondary metabolome and suggests that SA could be applied to increase diterpenoid levels in corals.

ELUTION OF URANIUM FROM RESIN

DOEpatents

McLEan, D.C.

1959-03-10

A method is described for eluting uranium from anion exchange resins so as to decrease vanadium and iron contamination and permit recycle of the major portion of the eluats after recovery of the uranium. Diminution of vanadium and iron contamination of the major portion of the uranium is accomplished by treating the anion exchange resin, which is saturated with uranium complex by adsorption from a sulfuric acid leach liquor from an ore bearing uranium, vanadium and iron, with one column volume of eluant prepared by passing chlorine into ammonium hydroxide until the chloride content is about 1 N and the pH is about 1. The resin is then eluted with 8 to 9 column volumes of 0.9 N ammonium chloride--0.1 N hydrochloric acid solution. The eluants are collected separately and treated with ammonia to precipitate ammonium diuranate which is filtered therefrom. The uranium salt from the first eluant is contaminated with the major portion of ths vanadium and iron and is reworked, while the uranium recovered from the second eluant is relatively free of the undesirable vanadium and irons. The filtrate from the first eluant portion is discarded. The filtrate from the second eluant portion may be recycled after adding hydrochloric acid to increase the chloride ion concentration and adjust the pH to about 1.

Cation exchange concentraion of the Americium product from TRUEX

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barney, G.S.; Cooper, T.D.; Fisher, F.D.

1991-06-01

A transuranic extraction (TRUEX) process has been developed to separate and recover plutonium, americium, and other transuranic (TRU) elements from acid wastes. The main objective of the process is to reduce the effluent to below the TRU limit for actinide concentrations (<100 nCi/g of material) so it can be disposed of inexpensively. The process yields a dilute nitric acid stream containing low concentrations of the extracted americium product. This solution also contains residual plutonium and trace amounts of iron. The americium will be absorbed into a cation exchange resin bed to concentrate it for disposal or for future use. Themore » overall objective of these laboratory tests was to determine the performance of the cation exchange process under expected conditions of the TRUEX process. Effects of acid, iron, and americium concentrations on americium absorption on the resin were determined. Distribution coefficients for americium absorption from acide solutions on the resin were measured using batch equilibrations. Batch equilibrations were also used to measure americium absorption in the presence of complexants. This data will be used to identify complexants and solution conditions that can be used to elute the americium from the columns. The rate of absorption was measured by passing solutions containing americium through small columns of resin, varying the flowrates, and measuring the concentrations of americium in the effluent. The rate data will be used to estimate the minimum bed size of the columns required to concentrate the americium product. 11 refs. , 10 figs., 2 tabs.« less

Comparative assessment of different recycling methods of orthodontic brackets for clinical use.

PubMed

de Oliveira Correia, Ayla M; de Souza Matos, Felipe; Pilli Jóias, Renata; de Mello Rode, Sigmar; Cesar, Paulo F; Paranhos, Luiz R

2017-06-01

This study aimed to assess bond strength of the resin/bracket interface, under in-vitro shear stress, of metal brackets recycled by different clinical protocols. Sixty stainless steel orthodontic brackets were bonded on acrylic resin. The Transbond XT™ resin was applied at the base of the bracket aided by a matrix, obtaining 1 mm of thickness, and photoactivated with a LED device (40 s; 500 mW/cm2). Samples were randomly divided into four groups (N.=15) according to the reconditioning/recycling protocol: aluminum oxide (AO) 90 µm; hydrofluoric acid 60 s (HA60); hydrofluoric acid 120 s (HA120); hydrofluoric acid 60 s + silane (HA60S). After recycling, the resin was applied at the base of the bracket for shear testing in a universal testing machine (0.5 mm/min). After reconditioning/recycling, the surfaces were analyzed by Scanning Electron Microscopy. Data obtained after the shear test were subjected to ANOVA and Tukey's test (P<0.05). The AO group presented higher values of shear bond strength compared to the other reconditioning/recycling protocols (P<0.05). The HA120 and HA60S groups presented statistically similar results, but HA120 presented strength below the recommended limit. The recycling technique by aluminum oxide sandblasting was more effective for reconditioning orthodontic brackets when compared to the other protocols. The reconditioning technique with 10% hydrofluoric acid followed by the application of silane bonding agent may be used as an alternative protocol.

Five New Guanacastane-Type Diterpenes from Cultures of the Fungus Psathyrella candolleana.

PubMed

Yin, Xia; Feng, Tao; Li, Zheng-Hui; Leng, Ying; Liu, Ji-Kai

2014-06-01

Five new guanacastane-type diterpenes, named guanacastepenes P-T (1-5), were isolated from cultures of the fungus Psathyrella candolleana. Their structures were elucidated on the basis of extensive spectroscopic methods. All of the compounds were tested for their 11β-hydroxysteroid dehydrogenase (11β-HSD1) inhibitory activity. Compound 3 exhibited inhibitory activity against both human and mouse isozymes of 11β-HSD1 with IC50 values of 6.2 and 13.9 μM, respectively.

Simplexins P–S, Eunicellin-Based Diterpenes from the Soft Coral Klyxum simplex

PubMed Central

Wu, Shwu-Li; Su, Jui-Hsin; Huang, Chiung-Yao; Tai, Chi-Jen; Sung, Ping-Jyun; Liaw, Chih-Chung; Sheu, Jyh-Horng

2012-01-01

Four new eunicellin-based diterpenes, simplexins P–S (1–4), and the known compound simplexin A (5), have been isolated from the soft coral Klyxum simplex. The structures of the new metabolites were determined on the basis of extensive spectroscopic analysis, particularly 1D and 2D NMR experiments. Compounds 1 and 3–5 were shown to exhibit cytotoxicity against a limited panel of cancer cell lines, 3 being the most cytotoxic. PMID:22822367

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

21 CFR 177.1500 - Nylon resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... condensation of adipic acid, 1,3-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Nylon resins. 177.1500 Section 177.1500 Food and...

EFFECT OF THE DECHLORINATING AGENT, ASCORBIC ACID, ON THE MUTAGENICITY OF CHLORINATED WATER SAMPLES

EPA Science Inventory

XAD resin adsorption has been widely used to concentrate the organic compounds present in chlorinated drinking waters prior to mutagenicity testing. Previous work has shown that mutagenic artifcats can arise due to the reaction of residual chlorine with the resins. Althrough the ...

Amino acid sequences of peptides from a chymotryptic digest of a urea-soluble protein fraction (U.S.3) from oxidized wool

PubMed Central

Corfield, M. C.; Fletcher, J. C.

1969-01-01

1. A chymotryptic digest of the protein fraction U.S.3. from oxidized wool was separated into 51 peptide fractions by chromatography on a column of cation-exchange resin. 2. The less acidic fractions were separated into their component peptides by a combination of cation-exchange-resin chromatography, paper chromatography and paper electrophoresis. 3. The amino acid sequences of 34 of these peptides were elucidated, and those of 14 others partially determined. 4. Overlaps between the tryptic and chymotryptic peptides from fraction U.S.3 have enabled ten extended amino acid sequences to be deduced, the longest containing 20 amino acid residues. 5. The relevance of the results to the structures of the helical and non-helical regions of wool is discussed. PMID:5395876

Phosphazene additives

DOEpatents

Harrup, Mason K; Rollins, Harry W

2013-11-26

An additive comprising a phosphazene compound that has at least two reactive functional groups and at least one capping functional group bonded to phosphorus atoms of the phosphazene compound. One of the at least two reactive functional groups is configured to react with cellulose and the other of the at least two reactive functional groups is configured to react with a resin, such as an amine resin of a polycarboxylic acid resin. The at least one capping functional group is selected from the group consisting of a short chain ether group, an alkoxy group, or an aryloxy group. Also disclosed are an additive-resin admixture, a method of treating a wood product, and a wood product.

Analysis of potential hazards associated with 241Am loaded resins from nitrate media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schulte, Louis D.; Rubin, Jim; Fife, Keith William

2016-02-19

LANL has been contacted to provide possible assistance in safe disposition of a number of 241Am-bearing materials associated with local industrial operations. Among the materials are ion exchange resins which have been in contact with 241Am and nitric acid, and which might have potential for exothermic reaction. The purpose of this paper is to analyze and define the resin forms and quantities to the extent possible from available data to allow better bounding of the potential reactivity hazard of the resin materials. An additional purpose is to recommend handling procedures to minimize the probability of an uncontrolled exothermic reaction.

Selected resin acids in effluent and receiving waters derived from a bleached and unbleached kraft pulp and paper mill

USGS Publications Warehouse

Quinn, B.P.; Booth, M.M.; Delfino, J.J.; Holm, S.E.; Gross, T.S.

2003-01-01

Water samples were collected on three dates at 24 sites influenced by effluent from Georgia-Pacific's Palatka Pulp and Paper Mill Operation, a bleached and unbleached kraft mill near Palatka, Florida, USA. The sampling sites were located within the mill retention ponds, Rice Creek, and the St. John's River. Samples were analyzed by gas chromatography-mass spectrometry for abietic, dehydroabietic, and isopimaric acids, all of which are potentially toxic by-products of pulp production. Isopimaric acid concentrations greater than 12 mg/L were measured at the mill's effluent outfall but were less than 20 ??g/L at the end of Rice Creek. This result indicates that the waters of Rice Creek provide dilution or conditions conducive for degradation or sorption of these compounds. Large differences in resin acid concentrations were observed between sampling events. In two sampling events, the maximum observed concentrations were less than 2 mg/L for each analyte. In a third sampling event, all of the compounds were detected at concentrations greater than 10 mg/L. Data from the three sample dates showed that resin acid concentrations were below 20 ??g/L before the confluence of Rice Creek and the St. John's River in all cases.

Development of critical molecular weight-property specifications for high performance polymers used as adhesives and composites

NASA Technical Reports Server (NTRS)

Kranbuehl, D. E.

1982-01-01

The polyimide resin, LARC-160, was prepared from diethyl-3, 3', 4,4'-benzophenone tetracarboxylate, ethyl-5-norbornene-2,3-dicarboxylate and Jeffamine AP-22. The imidization reactions of NE and BTDE were studied by HPLC, C-13-NMR and IR. NE imidizes slowly at 12 C; BTDE imidizes when the resin is heated above 100 C. Both imidization reactions proceed directly to the imide. Neither amic acid is present in significant quantities at any stage of the imidization reactions. The monomer mixture was stored at 12 C for periods up to 14 months. The effects of resin aging at this temperature on the chemical composition of the resin monomer mixture and the imidized polymer formed on curing were investigated. Aging the resin monomer mixture has the effect of partially advancing the imidization reaction. The average size of the cured polymer increases slightly with resin age.

Chemical affinities between the solvent extractable and the bulk organic matter of fossil resin associated with an extinct podocarpaceae

USGS Publications Warehouse

Grimalt, J.O.; Simoneit, B.R.T.; Hatcher, P.G.

1989-01-01

Analyses by GC-MS and GC-IR of resin associated to Dacridiumites mawsonii deposits, an extinct species of Podocarpaceae occurring on the South Island of New Zealand during the Bortonian (Middle Eocene), have revealed that dehydroabietic acid is the predominant component of the solvent soluble fraction. Accordingly, this diterpenoid has been selected as the principal component material for spectroscopic comparison with the bulk resin using IR and CP/MAS 13C NMR. ?? 1989.

40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

Code of Federal Regulations, 2011 CFR

2011-07-01

... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

Code of Federal Regulations, 2010 CFR

2010-07-01

... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

CATALYTIC PROMOTION OF THE ADSORPTION OF VANADIUM ON AN ANIONIC EXCHANGE RESIN

DOEpatents

Bailes, R.H.; Ellis, D.A.

1958-08-26

An improvement in the process for the recovery of vanadium from acidic phosphatic solutions is presented. In this process the vanadium is first oxidized to the pentavaleat state, and is then separated by contacting such solutions with an anion exchange resin whereby adsorption of the complexed pentavalent vanadium is effected. The improvement lies in the fact that adsorp tion of the vanadium complex by the anion exchange resin is promoted and improved by providing fiuoride ions in solution to be contacted.

Synthesis of Neoclerodane Diterpenes and Their Pharmacological Effects

NASA Astrophysics Data System (ADS)

Lovell, Kimberly M.; Prevatt-Smith, Katherine M.; Lozama, Anthony; Prisinzano, Thomas E.

Salvinorin A is a neoclerodane diterpene that has been shown to be an agonist at kappa opioid receptors. Its unique structure makes it an attractive target for synthetic organic chemists due to its seven chiral centers and diterpene scaffold. This molecule is also interesting to pharmacologists because it is a non-serotonergic hallucinogen, and the first opioid ligand discovered that lacks a basic nitrogen. There have been several total synthesis approaches to salvinorin A, and these will be detailed within this chapter. Additionally, research efforts have concentrated on structure modification of the salvinorin A scaffold through semi-synthetic methods. Most modifications have focused on the manipulation of the acetate at C-2 and the furan ring. However, chemistry has also been developed to generate analogs at the C-1 ketone, the C-4 methyl ester, and the C-17 lactone. The synthetic methodologies developed for the salvinorin A scaffold will be described, as well as specific analogs with interesting biological activities.

Assessment of some diterpenoids in commercial distilled gin.

PubMed

Vichi, Stefania; Aumatell, Montserrat Riu; Buxaderas, Susana; López-Tamames, Elvira

2008-11-03

In the present study the qualitative and quantitative determination of diterpenoids in commercial distilled gin was carried out. This widely consumed juniper-based spirit is aromatized using Juniper (Juniperus communis) berries. Although juniper reportedly contains several diterpenic compounds, no studies have addressed the diterpenic composition of juniper-based spirits or beverages. With this objective, here we followed a multilevel factorial experimental design to optimize a direct immersion-solid phase microextraction (DI-SPME) method coupled to gas chromatography/mass spectrometry and analyzed eight commercial brands of gin. With total concentrations ranging from 10 to 190 microg L(-1), manool, manoyl oxide and trans-totarol were the most abundant diterpenoids of the 10 identified or tentatively identified at variable but not negligible concentrations in the distilled gin samples. The diterpenic composition allowed the brands to be differentiated. This indicates that these compounds contribute to the sensory characteristics of the distinct commercial brands, thus guaranteeing the authenticity and consequently the quality of the product.

Addition of phosphotungstic acid to ethanol for dehydration improves both the ultrastructure and antigenicity of pituitary tissue embedded in LR White acrylic resin.

PubMed

Sakai, Yuko; Hosaka, Masahiro; Hira, Yoshiki; Watanabe, Tsuyoshi

2005-12-01

Although hydrophilic acrylic resins including LR White have been widely utilized as embedding media for immunocytochemical use, the constituents of tissues are often extracted by the resin monomer during the infiltration process of the embedment, resulting in a discernible impairment of the ultrastructure when the tissue is weakly fixed only with aldehydes. To minimize the extraction by the resin monomer, the embedding procedure with LR White resin was reexamined in the present study. Among the treatments tested, a partial dehydration with 70% ethanol containing 2% phosphotungstic acid (PTA) well preserved the ultrastructure of the pituitary tissue without spoiling the antigenicity of LHbeta and other representative markers for the Golgi apparatus. In addition, treatment with 1% tannic acid (TA) prior to the dehydration described above synergistically improved both the ultrastructure and antigenicity of the tissue so that the orientation of the Golgi apparatus could be determined by double immunogold labeling with commercially available anti-GM130 and anti-TGN38 antibodies. The ultrathin sections from the LR White-embedded tissue treated with TA and dehydrated in 70% ethanol containing 2% PTA also enhanced contrast without conventional heavy-metal staining with uranyl acetate and lead citrate. Our findings further suggest that the precipitation of TA and PTA protected the tissue from being extracted during the embedment, probably because an insoluble complex was transiently formed with the constituents of the tissue. This simple modification of the LR White embedment can extend the application of post-embedding immunocytochemistry as an alternative to pre-embedding immunolabeling with frozen ultrathin sections.

Shear bond strength of a new self-adhering flowable composite resin for lithium disilicate-reinforced CAD/CAM ceramic material

PubMed Central

Sancakli, Hande Sar; Sancakli, Erkan; Eren, Meltem Mert; Ozel, Sevda; Yucel, Taner; Yildiz, Esra

2014-01-01

PURPOSE The purpose of this study was to evaluate and compare the effects of different surface pretreatment techniques on the surface roughness and shear bond strength of a new self-adhering flowable composite resin for use with lithium disilicate-reinforced CAD/CAM ceramic material. MATERIALS AND METHODS A total of one hundred thirty lithium disilicate CAD/CAM ceramic plates with dimensions of 6 mm × 4 mm and 3 mm thick were prepared. Specimens were then assigned into five groups (n=26) as follows: untreated control, coating with 30 µm silica oxide particles (Cojet™ Sand), 9.6% hydrofluoric acid etching, Er:YAG laser irradiation, and grinding with a high-speed fine diamond bur. A self-adhering flowable composite resin (Vertise Flow) was applied onto the pre-treated ceramic plates using the Ultradent shear bond Teflon mold system. Surface roughness was measured by atomic force microscopy. Shear bond strength test were performed using a universal testing machine at a crosshead speed of 1 mm/min. Surface roughness data were analyzed by one-way ANOVA and the Tukey HSD tests. Shear bond strength test values were analyzed by Kruskal-Wallis and Mann-Whitney U tests at α=.05. RESULTS Hydrofluoric acid etching and grinding with high-speed fine diamond bur produced significantly higher surface roughness than the other pretreatment groups (P<.05). Hydrofluoric acid etching and silica coating yielded the highest shear bond strength values (P<.001). CONCLUSION Self-adhering flowable composite resin used as repair composite resin exhibited very low bond strength irrespective of the surface pretreatments used. PMID:25551002

BisGMA/TEGDMA dental nanocomposites containing glyoxylic acid modified high-aspect ratio hydroxyapatite nanofibers with enhanced dispersion

PubMed Central

Chen, Liang; Xu, Changqi; Wang, Yong; Shi, Jian; Yu, Qingsong

2012-01-01

The purpose of this research was to investigate the influence of the glyoxylic acid (GA) modification of hydroxyapatite (HAP) nanofibers on their dispersion in bisphenol A glycidyl methacrylate (BisGMA)/triethylene glycol dimethacrylate (TEGDMA) dental composites and also investigate the mechanical properties, water absorption, and water solubility of the resulting dental resins and composites. Scanning/Transmission electron microscopy (STEM) images showed that microsized HAP nanofiber bundles could be effectively broken down to individual HAP nanofibers with an average length of ~15 μm after the surface modification process. Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and thermal gravimetric analysis (TGA) characterization confirmed glyoxylic acid was chemically grafted on the HAP nanofiber surface, hypothetically by reacting with the amine group on HAP nanofiber surface. The enhanced dispersion of HAP nanofibers in dental matrix led to increased biaxial flexural strength (BFS) compared with the corresponding dental resins and composites filled with untreated HAP nanofibers. In addition, impregnation of small mass fractions of the glyoxylic acid modified HAP nanofibers into the BisGMA/TEGDMA dental resins (5wt%, 10wt%) or composites (2wt%, 3wt%) could also substantially improve the BFS in comparison with the controls(pure resins or dental composites filled with silica particles alone). Larger mass fractions could not further increase the mechanical property or even degrade the BFS values. Water behavior testing results indicated that the addition of glyoxylic acid modified HAP nanofibers resulted in higher water absorption and water solubility values which is not preferred for clinical application. In summary, well dispersed HAP nanofibers and their dental composites with enhanced mechanical property have been successfully fabricated but the water absorption and water solubility of such dental composites need to be further improved. PMID:22689264

Antimicrobial activities of amphiphilic peptides covalently bonded to a water-insoluble resin.

PubMed Central

Haynie, S L; Crum, G A; Doele, B A

1995-01-01

A series of polymer-bound antimicrobial peptides was prepared, and the peptides were tested for their antimicrobial activities. The immobilized peptides were prepared by a strategy that used solid-phase peptide synthesis that linked the carboxy-terminal amino acid with an ethylenediamine-modified polyamide resin (PepsynK). The acid-stable, permanent amide bond between the support and the nascent peptide renders the peptide resistant to cleavage from the support during the final acid-catalyzed deprotection step in the synthesis. Select immobilized peptides containing amino acid sequences that ranged from the naturally occurring magainin to simpler synthetic sequences with idealized secondary structures were excellent antimicrobial agents against several organisms. The immobilized peptides typically reduced the number of viable cells by > or = 5 log units. We show that the reduction in cell numbers cannot be explained by the action of a soluble component. We observed no leached or hydrolyzed peptide from the resin, nor did we observe any antimicrobial activity in soluble extracts from the immobilized peptide. The immobilized peptides were washed and reused for repeated microbial contact and killing. These results suggest that the surface actions by magainins and structurally related antimicrobial peptides are sufficient for their lethal activities. PMID:7726486

BARIUM RECOVERY PROCESS

DOEpatents

Blanco, R.E.

1959-07-21

A method of separating barium from nuclear fission products is described. In accordance with the invention, barium may be recovered from an acidic solution of neutron-irradiated fissionable material by carrying ihe barium cut of solution as a sulfate with lead as a carrier and then dissolving the barium-containing precipitate in an aqueous solution of an aliphatic diamine chelating reagent. The barium values together with certain other metallic values present in the diamine solution are then absorbed onto a cation exchange resin and the barium is selectively eluted from the resin bed with concentrated nitric acid.

New Stable Cu(I) Catalyst Supported on Weakly Acidic Polyacrylate Resin for Green C-N Coupling: Synthesis of N-(Pyridin-4-yl)benzene Amines and N,N-Bis(pyridine-4-yl)benzene Amines.

PubMed

Kore, Nitin; Pazdera, Pavel

2016-12-22

A method for preparation of a new stable Cu(I) catalyst supported on weakly acidic polyacrylate resin without additional stabilizing ligands is described. A simple and efficient methodology for Ullmann Cu(I) catalyzed C-N cross coupling reactions using this original catalyst is reported. Coupling reactions of 4-chloropyridinium chloride with anilines containing electron donating (EDG) or electron withdrawing (EWG) groups, naphthalen-2-amine and piperazine, respectively, are successfully demonstrated.

Experiments on Anion Exchange with Amberlite Ir-120 Resin; ENSAYOS DE INTERCAMBIO ANIONICO CON RESINA AMBERLITA Ir-120

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cellini, R.F.; Palomino, J.V.

1956-01-01

The ion exchange of the uranyl ion on Amberlite Ir-120 resin was studied with different uranyl ion concentrations. Elution with sulfuric acid was investlgated and the elution curve for the experimental conditions was determined. From the concentrations of the ions of Cu/sup 2+/, Ni/sup 2+/, Fe/sup 3+/, Cd/sup 2+/, Mn/sup 2+/, and Cr/sup 3+/ the maximum exchange capacity was tested and elation curves with 4 N sulfuric acid were obtained. (tr-auth)

Process for the preparation of lactic acid and glyceric acid

DOEpatents

Jackson, James E [Haslett, MI; Miller, Dennis J [Okemos, MI; Marincean, Simona [Dewitt, MI

2008-12-02

Hexose and pentose monosaccharides are degraded to lactic acid and glyceric acid in an aqueous solution in the presence of an excess of a strongly anionic exchange resin, such as AMBERLITE IRN78 and AMBERLITE IRA400. The glyceric acid and lactic acid can be separated from the aqueous solution. Lactic acid and glyceric acid are staple articles of commerce.

The Resin-in-pulp Process and Its Application to Ores from Brosses "BRS 10"; LE PROCEDE "RESIN IN PULP" ET SON APPLICATION AUX MINERAIS DES BROSSES "BRS 10"

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kremer, M.

1959-03-01

The resin-in-pulp process is a technical variant of the recovery process of uranium in dilute solution by means of ion exchange resins. An anion resin, XE 123, of a welldefined grain size is placed in direct contact with the pulp produced by sulfuric acid attack on ore with a low uranium content. This process is of particular value in the treatment of pulps that cannot be filtered or decanted, such as those obtained with ore from Brosses. The preparation of the pulp, the elution of the uranium, and its fixation, as well as the various factors encountered in these operations,more » are discussed. (auth)« less

Separation and recovery of food coloring dyes using aqueous biphasic extraction chromatographic resins.

PubMed

Huddleston, J G; Willauer, H D; Boaz, K R; Rogers, R D

1998-06-26

Aqueous biphasic systems (ABS) and aqueous biphasic extraction chromatographic (ABEC) resins are currently under investigation for their utility in the removal of color from textile plant wastes. The structures of several widely used food colorings, suggest that these dyes would also be retained on the resins. In work currently in progress, we have begun to investigate the retention and resolution of several common food colorings including indigo carmine, amaranth, carminic acid. erythrosin B, tartrazine and quinoline yellow. The relationship between the uptake of these dyes on ABEC resins in terms of the binding strengths and capacities of the resins and their partitioning behavior in ABS is illustrated. Some possible theoretical and practical approaches to the prediction of the partitioning and retention behavior is discussed.

Separation of Be and Al for AMS using single-step column chromatography

NASA Astrophysics Data System (ADS)

Binnie, Steven A.; Dunai, Tibor J.; Voronina, Elena; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred

2015-10-01

With the aim of simplifying AMS target preparation procedures for TCN measurements we tested a new extraction chromatography approach which couples an anion exchange resin (WBEC) to a chelating resin (Beryllium resin) to separate Be and Al from dissolved quartz samples. Results show that WBEC-Beryllium resin stacks can be used to provide high purity Be and Al separations using a combination of hydrochloric/oxalic and nitric acid elutions. 10Be and 26Al concentrations from quartz samples prepared using more standard procedures are compared with results from replicate samples prepared using the coupled WBEC-Beryllium resin approach and show good agreement. The new column procedure is performed in a single step, reducing sample preparation times relative to more traditional methods of TCN target production.

Volatile components of horsetail (Hippuris vulgaris L.) growing in central Italy.

PubMed

Cianfaglione, Kevin; Papa, Fabrizio; Maggi, Filippo

2017-10-01

Hippuris vulgaris, also known as horsetail or marestail, is a freshwater macrophyte occurring in lakes, rivers, ponds and marshes. According to 'The IUCN Red List of Threatened Species', H. vulgaris is at a high risk of extinction in Italy in the medium-term future. In the present study, we analysed for the first time the volatile composition of H. vulgaris growing in central Italy. For the purpose, the essential oil was obtained by hydrodistillation and analysed by GC-MS. The chemical composition was dominated by aliphatic compounds such as fatty acids (26.0%), ketones (18.7%) and alkanes (11.4%), whereas terpenoids were poorer and mostly represented by diterpenes (7.4%). n-Hexadecanoic acid (25.5%), hexahydrofarnesyl acetone (17.5%) and trans-phytol (7.4%) were the major volatile constituents. These compounds are here proposed as chemotaxonomic markers of the species.

[Coffee as hepatoprotective factor].

PubMed

Szántová, Mária; Ďurkovičová, Zuzana

The mind about the coffee did change upon the recent studies and metaanalysis of the last years. Consensual protective effect of coffee on the progression of chronic liver diseases (NASH, viral hepatitis, liver cirrhosis, hepatocelullar carcinoma) was detected in experimental, clinical and large population studies together with decrease of mortality. Antioxidant, antifibrotic, insulinsensitizing and anticarcinogenic effect of coffee were detected. Modulation of genetic expression of key enzymes of fatty acid synthesis, modulation of mRNA included in autophagia, reduction of stress of endoplasmatic reticulum together with decrease of proinflammatory cytokines and decrease of fibrogenesis are main mechanisms. Chlorogenic acids, diterpens (cafestol, kahweol), caffein, polyfenols and melanoidins are key protective components of coffee. Inverse dose-dependent correlation of coffee consumption with liver diseases was found in clinical and population studies. Coffee is non-pharmacological tool of primary and secondary prevention of chronic liver diseases. Review of published data together with supposed mechanisms of hepatoprotection are given.Key words: coffee - hepatoprotective effect - metaanalysis.

[Contact allergy to epoxy resins plastics based on materials collected by the Nofer Institute of Occupational Medicine].

PubMed

Kieć-Swierczyńska, Marta; Krecisz, Beata

2003-01-01

Of the 5604 patients examined in 1984-2001 for suspected occupational dermatitis, 160 persons (2.8%) showed allergy to epoxy resins plastics. Allergy was more frequent in men (4.9%) than in women (1.2%); in 154 persons, allergy was of occupational etiology (in a group of 160 patients with allergy to epoxy resins, the following proportions were observed: bricklayers, platelayers--17.5%; fitters, turners, machinist millers--13.8%; plastics molders--13.1%; laminators--11.3%; electrical equipment assemblers--10.6%; painters--10.0%). Having compared the frequency of allergy to components of epoxy resins in the years 1984-1993 and 1994-2001, it was found that allergy to resin, reactive diluents and plasticizers was on increase, whereas allergy to amines and acid anhydrides hardeners was on decrease. In a group of 13 chemical compounds entering into the composition of epoxy resins, epoxy resin contributed to the largest number of positive patch tests (77.5% of epoxy-allergic persons). This was followed by triethylenetetramine (23.1%), ethylenediamine (13.1%), phthalic anhydride (8.1%), diethylenetetramine (6.9%) and phenylglycidylether (6.2%). In addition, three patients reacted to both epoxy resin and cycloaliphatic resin.

The Diterpene Sclareol Vascular Effect in Normotensive and Hypertensive Rats

PubMed Central

Campos, Debora Ribeiro; Celotto, Andrea Carla; Albuquerque, Agnes Afrodite S.; Ferreira, Luciana Garros; Monteiro, Ariadne Santana e Neves; Coelho, Eduardo Barbosa; Evora, Paulo Roberto Barbosa

2017-01-01

Background The diterpene Sclareol has antimicrobial action, cytotoxic and cytostatic effects and anti-tumor activities. However, researches on the cardiovascular system are scarce. Objective This study was designed to investigate the mechanisms involved in the Sclareol cardiovascular effect in normotensive and hypertensive rats. Methods The arterial hypertension was promoted using 2-kidneys 1-clip model in rats. The effect of sclareol on blood pressure was performed by using three dose (10, 20 and 40 mg/kg). Cumulative dose-response curves for Sclareol were determined for endothelium-intact and endothelium-denuded aortic rings in presence or absence of L-NAME and ODQ. The NOx levels were measure in the plasma sample. Results The Sclareol administration in vivo caused a significant reduction in blood pressure in both groups. In vitro the sclareol promoted relaxation in aorta, with endothelium, pre-contracted to Phe. The inhibitors of the nitric oxide synthase and soluble guanylate cyclase were as efficient as the removal of endothelium, in inhibiting the Sclareol-induced relaxation. Otherwise, it was no change of NOx. Also, for unknown reasons, the Sclareol is not selective for hypertensive animals. Conclusion The diterpene Sclareol showed in vivo hypotensive and in-vitro vasodilator effects;The chemiluminescence plasmatic NO analysis showed no significant difference between groups andThe Sclareol exhibit better effect on normotensive than hypertensive animals to reduce blood pressure. It is concluded that the diterpenes metabolites would be a promising source prototype for the development of new agents in the cardiovascular therapy. PMID:28678928

The Full-Size ABCG Transporters Nb-ABCG1 and Nb-ABCG2 Function in Pre- and Postinvasion Defense against Phytophthora infestans in Nicotiana benthamiana

PubMed Central

Shibata, Yusuke; Ojika, Makoto; Sugiyama, Akifumi; Yazaki, Kazufumi; Jones, David A.; Kawakita, Kazuhito

2016-01-01

The sesquiterpenoid capsidiol is the major phytoalexin produced by Nicotiana and Capsicum species. Capsidiol is produced in plant tissues attacked by pathogens and plays a major role in postinvasion defense by inhibiting pathogen growth. Using virus-induced gene silencing-based screening, we identified two Nicotiana benthamiana (wild tobacco) genes encoding functionally redundant full-size ABCG (PDR-type) transporters, Nb-ABCG1/PDR1 and Nb-ABCG2/PDR2, which are essential for resistance to the potato late blight pathogen Phytophthora infestans. Silencing of Nb-ABCG1/2 compromised secretion of capsidiol, revealing Nb-ABCG1/2 as probable exporters of capsidiol. Accumulation of plasma membrane-localized Nb-ABCG1 and Nb-ABCG2 was observed at the site of pathogen penetration. Silencing of EAS (encoding 5-epi-aristolochene synthase), a gene for capsidiol biosynthesis, reduced resistance to P. infestans, but penetration by P. infestans was not affected. By contrast, Nb-ABCG1/2-silenced plants showed reduced penetration defense, indicating that Nb-ABCG1/2 are involved in preinvasion defense against P. infestans. Plastidic GGPPS1 (geranylgeranyl diphosphate synthase) was also found to be required for preinvasion defense, thereby suggesting that plastid-produced diterpene(s) are the antimicrobial compounds active in preinvasion defense. These findings suggest that N. benthamiana ABCG1/2 are involved in the export of both antimicrobial diterpene(s) for preinvasion defense and capsidiol for postinvasion defense against P. infestans. PMID:27102667

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2011 CFR

2011-04-01

... (CONTINUED) FOOD FOR HUMAN CONSUMPTION (CONTINUED) INDIRECT FOOD ADDITIVES: POLYMERS Substances for Use Only... this section: (1) Acids: Adipic. Fatty acids, and dimers thereof, from natural sources. Fumaric...

21 CFR 177.2420 - Polyester resins, cross-linked.

Code of Federal Regulations, 2010 CFR

2010-04-01

... (CONTINUED) FOOD FOR HUMAN CONSUMPTION (CONTINUED) INDIRECT FOOD ADDITIVES: POLYMERS Substances for Use Only... this section: (1) Acids: Adipic. Fatty acids, and dimers thereof, from natural sources. Fumaric...

Effect of humic acid on ciprofloxacin removal by magnetic multifunctional resins

PubMed Central

Wang, Wei; Cheng, Jiade; Jin, Jing; Zhou, Qing; Ma, Yan; Zhao, Qingqing; Li, Aimin

2016-01-01

Background organic matter significantly influences the removal of emerging contaminants in natural water. In this work, the adsorption of ciprofloxacin (CPX) onto a series of magnetic multifunctional resins (GMA10-GMA90) in the presence and absence of humic acid (HA) was conducted to demonstrate the effect of HA. Both hydrophobic and ion exchange interactions contributed to CPX adsorption. Negative charge-assisted hydrogen bonds also participated in the adsorption process, resulting in the high adsorption amount of anionic CPX onto the negatively charged GMA30 under basic solutions. HA could impact CPX adsorption not only as a competitive adsorbate but also as an additional adsorbent. At pH 5.6, the additional adsorption sites provided by adsorbed HA molecules on the resins dominated and thus facilitated the adsorption process. While at pH 10, HA inhibited the adsorption of CPX by directly competing for ion exchange sites and coexisting with CPX in the solution. The ratio of the amount of CPX adsorbed by dissolved HA to that by the resin reached as high as 1.61 for GMA90. The adsorbed HA molecules onto the resins could provide additional adsorption sites for CPX as proven by the enhanced CPX adsorption in HA-preloading systems at pH 5.6. PMID:27464502

Relationship between water status in dentin and interfacial morphology in all-in-one adhesives.

PubMed

Yoshida, Eiji; Uno, Sigeru; Nodasaka, Yoshinobu; Kaga, Msayuki; Hirano, Susumu

2007-05-01

All-in-one adhesive systems have been recently developed to simplify bonding procedures. The adhesives containing acidic resin monomers generate a relatively thin bonding zone between dentin and composite. This zone may be left acidic and permeable when polymerization is poor. In this study, the effect of water contained in dentin on the quality of the bonding interface was morphologically investigated for all-in-one adhesives. Intact coronal dentin (hydrated dentin), desiccated coronal dentin (dehydrated dentin), caries-affected dentin (CAD) and resin composites were used for adherends to assess the effects of water contained in dentin on the ultra-structures of bonding interfaces created with two all-in-one adhesives and a resin composite. The bonding interfaces were observed under TEM without demineralization. Voids of various sizes were found at the bottom of the adhesive resin layers along the bonding interface of hydrated dentin, while dehydrated dentin, CAD and resin composites did not generate voids. The results showed that the voids were possibly formed by water that had penetrated from the underlying dentin. When the adherend contains little water, the formation of voids will not occur. It was verified that a phenomenon of void formation would not occur in a clinical situation in which caries-affected dentin is mainly subjected to adhesive practices.

Effect of humic acid on ciprofloxacin removal by magnetic multifunctional resins

NASA Astrophysics Data System (ADS)

Wang, Wei; Cheng, Jiade; Jin, Jing; Zhou, Qing; Ma, Yan; Zhao, Qingqing; Li, Aimin

2016-07-01

Background organic matter significantly influences the removal of emerging contaminants in natural water. In this work, the adsorption of ciprofloxacin (CPX) onto a series of magnetic multifunctional resins (GMA10-GMA90) in the presence and absence of humic acid (HA) was conducted to demonstrate the effect of HA. Both hydrophobic and ion exchange interactions contributed to CPX adsorption. Negative charge-assisted hydrogen bonds also participated in the adsorption process, resulting in the high adsorption amount of anionic CPX onto the negatively charged GMA30 under basic solutions. HA could impact CPX adsorption not only as a competitive adsorbate but also as an additional adsorbent. At pH 5.6, the additional adsorption sites provided by adsorbed HA molecules on the resins dominated and thus facilitated the adsorption process. While at pH 10, HA inhibited the adsorption of CPX by directly competing for ion exchange sites and coexisting with CPX in the solution. The ratio of the amount of CPX adsorbed by dissolved HA to that by the resin reached as high as 1.61 for GMA90. The adsorbed HA molecules onto the resins could provide additional adsorption sites for CPX as proven by the enhanced CPX adsorption in HA-preloading systems at pH 5.6.

High-temperature resins

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1982-01-01

The basic chemistry, cure processes, properties, and applications of high temperature resins known as polyimides are surveyed. Condensation aromatic polymides are prepared by reacting aromatic diamines with aromatic dianhydrides, aromatic tetracarboxylic acids, or with dialkyl esters of aromatic tetracarboxylic acids, depending on the intended end use. The first is for coatings or films while the latter two are more suitable for polyimide matrix resins. Prepreg solutions are made by dissolving reactants in an aprotic solvent, and advances in the addition of a diamine on the double bond and radical polymerization of the double bond are noted to have yielded a final cure product with void-free characteristics. Attention is given to properties of the Skybond, Pyralin, and NR-150B polyimide prepreg materials and characteristics of aging in the NP-150 polyimides. Finally, features of the NASA-developed PMR polyimides are reviewed.

21 CFR 175.300 - Resinous and polymeric coatings.

Code of Federal Regulations, 2014 CFR

2014-04-01

... triglycerides or fatty acids derived from the oils listed in paragraph (b)(3)(i) of this section to form esters.... Maleic anhydride adduct of butadiene styrene. Polybutadiene. (iv) Natural fossil resins, as the basic... with: Maleic anhydride. o-, m-, and p-substituted phenol-form-alde-hydes listed in paragraph (b)(3)(vi...

21 CFR 175.320 - Resinous and polymeric coatings for polyolefin films.

Code of Federal Regulations, 2014 CFR

2014-04-01

... film over one or both sides of a base film produced from one or more of the basic olefin polymers complying with § 177.1520 of this chapter. The base polyolefin film may contain optional adjuvant substances... Limitations (i) Resins and polymers: Acrylic acid polymer and its ethyl or methyl esters Acrylamide...

Simultaneous separation and purification of chlorogenic acid, epicatechin, hyperoside and phlorizin from thinned young Qinguan apples by successive use of polyethylene and polyamide resins.

PubMed

Sun, Lijun; Liu, Dongjie; Sun, Jiaojiao; Yang, Xingbin; Fu, Minghai; Guo, Yurong

2017-09-01

The method for separating and purifying chlorogenic acid (CA), epicatechin (EC), hyperoside (HY) and phlorizin (PH) simutaneously from young Qinguan apples by successive use of X-5 and polyamide resins has been developed in this study. The order of adsorption capacities of X-5 for the four phenolics was PH>HY>EC>CA, and the adsorption equilibriums of the four phenolics onto X-5 resin conformed to Langmuir isotherms preferentially. The adsorption kinetics of EC and CA onto X-5 conformed to the pseudo-first-order model, while that of HY and PH accorded with the pseudo-second-order model. Interestingly, the values of equilibrium adsorption capacities (Q e ) calculated in the preferential kinetics models were closer to that of theoretical maximum adsorption capacities (Q 0 ) calculated by Langmuir isotherms. Through dynamic adsorption and desorption using X-5 and polyamide resins with ethanol solution as strippant, CA, EC, HY and PH were obtained with purities of 96.21%, 95.34%, 95.36% and 97.36%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

The conifer biomarkers dehydroabietic and abietic acids are widespread in Cyanobacteria

PubMed Central

Costa, Maria Sofia; Rego, Adriana; Ramos, Vitor; Afonso, Tiago B.; Freitas, Sara; Preto, Marco; Lopes, Viviana; Vasconcelos, Vitor; Magalhães, Catarina; Leão, Pedro N.

2016-01-01

Terpenes, a large family of natural products with important applications, are commonly associated with plants and fungi. The diterpenoids dehydroabietic and abietic acids are defense metabolites abundant in resin, and are used as biomarkers for conifer plants. We report here for the first time that the two diterpenoid acids are produced by members of several genera of cyanobacteria. Dehydroabietic acid was isolated from two cyanobacterial strains and its identity was confirmed spectroscopically. One or both of the diterpenoids were detected in the cells of phylogenetically diverse cyanobacteria belonging to four cyanobacterial ‘botanical orders’, from marine, estuarine and inland environments. Dehydroabietic acid was additionally found in culture supernatants. We investigated the natural role of the two resin acids in cyanobacteria using ecologically-relevant bioassays and found that the compounds inhibited the growth of a small coccoid cyanobacterium. The unexpected discovery of dehydroabietic and abietic acids in a wide range of cyanobacteria has implications for their use as plant biomarkers. PMID:26996104

Direct injection analysis of fatty and resin acids in papermaking process waters by HPLC/MS.

PubMed

Valto, Piia; Knuutinen, Juha; Alén, Raimo

2011-04-01

A novel HPLC-atmospheric pressure chemical ionization/MS (HPLC-APCI/MS) method was developed for the rapid analysis of selected fatty and resin acids typically present in papermaking process waters. A mixture of palmitic, stearic, oleic, linolenic, and dehydroabietic acids was separated by a commercial HPLC column (a modified stationary C(18) phase) using gradient elution with methanol/0.15% formic acid (pH 2.5) as a mobile phase. The internal standard (myristic acid) method was used to calculate the correlation coefficients and in the quantitation of the results. In the thorough quality parameters measurement, a mixture of these model acids in aqueous media as well as in six different paper machine process waters was quantitatively determined. The measured quality parameters, such as selectivity, linearity, precision, and accuracy, clearly indicated that, compared with traditional gas chromatographic techniques, the simple method developed provided a faster chromatographic analysis with almost real-time monitoring of these acids. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The conifer biomarkers dehydroabietic and abietic acids are widespread in Cyanobacteria

NASA Astrophysics Data System (ADS)

Costa, Maria Sofia; Rego, Adriana; Ramos, Vitor; Afonso, Tiago B.; Freitas, Sara; Preto, Marco; Lopes, Viviana; Vasconcelos, Vitor; Magalhães, Catarina; Leão, Pedro N.

2016-03-01

Terpenes, a large family of natural products with important applications, are commonly associated with plants and fungi. The diterpenoids dehydroabietic and abietic acids are defense metabolites abundant in resin, and are used as biomarkers for conifer plants. We report here for the first time that the two diterpenoid acids are produced by members of several genera of cyanobacteria. Dehydroabietic acid was isolated from two cyanobacterial strains and its identity was confirmed spectroscopically. One or both of the diterpenoids were detected in the cells of phylogenetically diverse cyanobacteria belonging to four cyanobacterial ‘botanical orders’, from marine, estuarine and inland environments. Dehydroabietic acid was additionally found in culture supernatants. We investigated the natural role of the two resin acids in cyanobacteria using ecologically-relevant bioassays and found that the compounds inhibited the growth of a small coccoid cyanobacterium. The unexpected discovery of dehydroabietic and abietic acids in a wide range of cyanobacteria has implications for their use as plant biomarkers.

Rapid removal of copper with magnetic poly-acrylic weak acid resin: quantitative role of bead radius on ion exchange.

PubMed

Fu, Lichun; Shuang, Chendong; Liu, Fuqiang; Li, Aimin; Li, Yan; Zhou, Yang; Song, Haiou

2014-05-15

A novel magnetic weak acid resin NDMC was self-synthesized for the removal of Cu(2+) from aqueous solutions. NDMC showed superior properties on the removal of Cu(2+) compared to commercial resins C106 and IRC-748, which was deeply investigated by adsorption isotherms and kinetic tests. The equilibrium adsorption amount of Cu(2+) onto NDMC (267.2mg/g) was almost twice as large as that onto IRC-748 (120.0mg/g). The adsorption kinetics of Cu(2+) onto the three resins fitted well with the pseudo-second-order equation. The initial adsorption rate h of NDMC was about 4 times that of C106 and nearly 8 times that of IRC-748 at the initial concentration of 500mg/L. External surface area was determined to be the key factor in rate-controlling by further analyzing the adsorption thermodynamics, kinetics parameters and physicochemical properties of the resins. NDMC resin with the smallest bead radius possessed the largest external surface and therefore exhibited the fastest kinetics. The adsorption amount of Cu(2+) onto NDMC was not influenced as the concentration of Na(+) increased from 1.0 to 10.0mM/L. Dilute HCl solution could effectively desorb Cu(2+). NDMC demonstrated high stability during 10 adsorption/desorption cycles, showing great potential in the rapid removal of Cu(2+) from wastewater. Copyright © 2014 Elsevier B.V. All rights reserved.

Direct Tensile Strength and Characteristics of Dentin Restored with All-Ceramic, Resin-Composite, and Cast Metal Prostheses Cemented with Resin Adhesives

PubMed Central

Piemjai, Morakot; Nakabayashi, Nobuo

2015-01-01

A dentin-cement-prosthesis complex restored with either all-porcelain, cured resin-composite, or cast base metal alloy and cemented with either of the different resin cements was trimmed into a mini-dumbbell shape for tensile testing. The fractured surfaces and characterization of the dentin-cement interface of bonded specimens were investigated using a Scanning Electron Microscope. A significantly higher tensile strength of all-porcelain (12.5 ± 2.2 MPa) than that of cast metal (9.2 ± 3.5 MPa) restorations was revealed with cohesive failure in the cement and failure at the prosthesis-cement interface in Super-Bond C&B group. No significant difference in tensile strength was found among the types of restorations using the other three cements with adhesive failure on the dentin side and cohesive failure in the cured resin. SEM micrographs demonstrated the consistent hybridized dentin in Super-Bond C&B specimens that could resist degradation when immersed in hydrochloric acid followed by NaOCl solutions whereas a detached and degraded interfacial layer was found for the other cements. The results suggest that when complete hybridization of resin into dentin occurs tensile strength at the dentin-cement is higher than at the cement-prosthesis interfaces. The impermeable hybridized dentin can protect the underlying dentin and pulp from acid demineralization, even if detachment of the prosthesis has occurred. PMID:26539520

Screening of Catalyst and Important Variable for The Esterification of Acrylic Acid with 2 Ethylhexanol

NASA Astrophysics Data System (ADS)

Ahmad, M. A. A.; Chin, S. Y.

2017-06-01

The global demand of 2-ethylhexyl acrylate (2EHA) market has witnessed a significant growth in the past few years and this growth is anticipated to increase in the coming years. 2EHA is one of the basic organic building blocks that mainly used in the production of coatings, adhesives, superabsorbents, thickeners and plastic additives. Homogenous acid-catalysed esterification of acrylic acid (AA) with 2-ethylhexanol (2EH) is commonly used for the production of 2EHA. The homogeneous catalysts such as sulfuric and para-toluene sulfonic acid have resulted the costly and complicated downstream process that generates acidic, corrosive and non-environmental friendly waste. Therefore, it is importance to develop a cheaper process that employing heterogeneous catalysts and alternative raw material from wastewater containing acrylic acid. In this research, the study for the esterification of AA with 2EH catalysed by ion-exchange resin was conducted. The best sulfonic acid functional cation-exchange resin among SK104, SK1B, PK208, PK216, PK228, RCP145, and RCP160 was screened. PK208 outperformed the other resins and it was used subsequently in the parametric studies. The effect of important parameters (initial concentration of acrylic acid (AA), temperature, molar ratio of reactant (AA and 2EH), catalyst loading, and polymerisation inhibitor loading) was studied using 2 factorial design to determine the significant parameters to the esterification. It was found that the initial concentration of AA and temperature were most significantly affecting the esterification of AA with 2EH.

[Effect of hydrofluoric acid concentration on the surface morphology and bonding effectiveness of lithium disilicate glass ceramics to resin composites].

PubMed

Hailan, Qian; Lingyan, Ren; Rongrong, Nie; Xiangfeng, Meng

2017-12-01

This study aimed at determining the influence of hydrofluoric acid (HF) in varied concentrations on the surface morphology of lithium disilicate glass ceramics and bond durability between resin composites and post-treated lithium disilicate glass ceramics. After being sintered, ground, and washed, 72 as-prepared specimens of lithium disilicate glass ceramics with dimensions of 11 mm×13 mm×2 mm were randomly divided into three groups. Each group was treated with acid solution [32% phosphoric acid (PA) or 4% or 9.5% HF] for 20 s. Then, four acidified specimens from each group were randomly selected. One of the specimens was used to observe the surface morphology using scanning electron microscopy, and the others were used to observe the surface roughness using a surface roughness meter (including Ra, Rz, and Rmax). After treatment with different acid solutions in each group, 20 samples were further treated with silane coupling agent/resin adhesive/resin cement (Monobond S/Multilink Primer A&B/Multilink N), followed by bonding to a composite resin column (Filtek™ Z350) with a diameter of 3 mm. A total of 20 specimens in each group were randomly divided into two subgroups, which were used for measuring the microshear bond strength, with one of them subjected to cool-thermal cycle for 20 000 times. The surface roughness (Ra, Rz, and Rmax) of lithium disilicate glass ceramics treated with 4% or 9.5% HF was significantly higher than that of the ceramic treated with PA (P<0.05). The lithium disilicate glass ceramics treated with 9.5% HF also demonstrated better surface roughness (Rz and Rmax) than that of the ceramics treated with 4% HF. Cool-thermal cycle treatment reduced the bond strength of lithium disilicate glass ceramics in all groups (P<0.05). After cool-thermal cycle, the lithium disilicate glass ceramics treated with HF had higher bond strength than that of the ceramics treated with PA. The lithium disilicate glass ceramics treated with 4% HF had higher bond strength than that of the ceramics treated with 9.5% HF (P<0.05). During cool-thermal cycle, the lithium disilicate glass ceramics treated with 4% HF demonstrated higher reduction in bond strength than that of the samples treated with 9.5% HF (P<0.05). The concentration of HF significantly affected the surface morphology of lithium disilicate glass ceramics and the bond durability between resin composites and post-treated lithium disilicate glass ceramics. The bond strength between resin composites and post-treated lithium disilicate glass ceramic was more efficiently maintained by treatment with 9.5% HF.

Impact of natural organic matter properties on the kinetics of suspended ion exchange process.

PubMed

Bazri, Mohammad Mahdi; Mohseni, Madjid

2016-03-15

Removal kinetics of four standard organic matter isolates under the application of strongly basic ion exchange resins (IEX) in suspended mode was studied under commercial application conditions. Suwannee River natural organic matter (SRNOM), SR fulvic acid (SRFA), and Pony Lake fulvic acid (PLFA) were greatly removed (>90%) and highly preferred by IEX resins (α > 5, over Cl(-), and HCO3(-)) while SR humic acid (SRHA) was the least preferred organic structure among the four isolates studied (α ≈ 1). Moreover, the efficacy of removal for fulvic acids (i.e., SRFA, PLFA) was consistent over consecutive reuse of IEX resins (i.e., loading cycles) whereas it decreased for SRNOM and SRHA over the course of operation. The stoichiometric correlation between the chloride released from the resins as a result of organic molecules uptake indicated that ion exchange was the dominant mechanism. Results obtained indicated that molecular weight and charge density of isolates played a major role in the performance of ion exchange process for organic matter removal. Furthermore, various empirical and physical models were evaluated using the experimental data and pore diffusion was found to be the rate-liming step during the uptake of organic matters; hence, it was used as the appropriate model to predict the kinetics of removal. Consequently, free liquid diffusivities and effective pore diffusion coefficients of organic molecules were estimated and findings were in agreement with the literature data that were obtained from spectrophotometric methods. Copyright © 2015 Elsevier Ltd. All rights reserved.

Matrix effect and optimization of LC-MSn determination of trachylobane-360 in mice blood.

PubMed

Pita, João Carlos Lima Rodrigues; Gomes, Isis Fernandes; Dos Santos, Socrates Golzio; Tavares, Josean Fechine; da Silva, Marcelo Sobral; Diniz, Margareth de Fátima Formiga Melo; Sobral, Marianna Vieira

2014-11-01

Xylopia langsdorffiana A. St.-Hil. & Tul. (Annonaceae) is popularly known as "pimenteira-da-terra". Various constituents have been isolated from this species, including diterpenes, such as 8(17), 12E, 14-labdatrien-18-oic acid, ent-atisan-7α, 16α-diol (xylodiol), ent-7α-hydroxytrachyloban-18-oic acid (trachylobane-318) and ent-7α-acetoxytrachyloban-18-oic acid, a crystalline solid with a molecular weight of 360 and molecular formula of C22H32O4 (trachylobane-360). When administered intraperitoneally to mice, trachylobane-360 (T-360) significantly inhibits growth of the solid tumor sarcoma 180 transplanted in mice, without causing alterations in biochemical, hematological and histopathological parameters that are frequently associated with the clinical use of antineoplastic. Furthermore, this diterpene blocks voltage-dependent calcium channels (Cav), showing spasmolytic activity. The present study shows that variables such as extraction solvent (methanol, acetonitrile and chloroform), centrifugation force (1000, 7000 and 14,000×g), and centrifugation time (5, 15 and 25min), are important in the liquid-liquid extraction of T-360 from male Swiss mice blood in HPLC-MSn studies. The study confirms matrix influence on recovery and detection of T-360. The recovery for T-360 was 37.02% using chloroform as better extractor solvent, while centrifuged at 14,000×g for 15min demonstrated the importance of the parameters chosen for the extraction/recovery process of analyte. The effect of mice blood matrix for T-360 was -51.23%. This method was optimized by repeating the extraction procedure and acidification of samples. These conditions were essential in increasing recovery (49.47%) by decreasing the matrix effect (-37.60%). The efficiency of the process, after optimization with two extractions and acidification, increased by 14.19% when compared to the initial method, from 18.05% to 32.24%. According to Marchi et al. (2010), the matrix effect does not necessarily need to be reduced or eliminated, but it does need to be identified and quantified. Therefore, these findings are essential for the subsequent evaluation of the pharmacokinetic parameters of this promising natural product. Copyright © 2014 Elsevier B.V. All rights reserved.

Dental Cements for Luting and Bonding Restorations: Self-Adhesive Resin Cements.

PubMed

Manso, Adriana P; Carvalho, Ricardo M

2017-10-01

Self-adhesive resin cements combine easy application of conventional luting materials with improved mechanical properties and bonding capability of resin cements. The presence of functional acidic monomers, dual cure setting mechanism, and fillers capable of neutralizing the initial low pH of the cement are essential elements of the material and should be understood when selecting the ideal luting material for each clinical situation. This article addresses the most relevant aspects of self-adhesive resin cements and their potential impact on clinical performance. Although few clinical studies are available to establish solid clinical evidence, the information presented provides clinical guidance in the dynamic environment of material development. Copyright © 2017 Elsevier Inc. All rights reserved.

PEEK surface treatment effects on tensile bond strength to veneering resins.

PubMed

Stawarczyk, Bogna; Jordan, Peter; Schmidlin, Patrick R; Roos, Malgorzata; Eichberger, Marlis; Gernet, Wolfgang; Keul, Christine

2014-11-01

Polyetheretherketone (PEEK) can be used as a framework material for fixed dental prostheses. However, information about the durable bond to veneering resins is still scarce. The purpose of this study was to investigate the effect of chemical treatments of PEEK on tensile bond strength (TBS) to veneering resins with special emphasis on surface free energy (SFE) and surface roughness (SR). Seven-hundred fifty PEEK specimens were fabricated and divided into the following 3 pretreatment groups (n=250/group): etching with sulfuric acid for 60 seconds, etching with piranha acid for 30 seconds, and an unetched control. After pretreatment, SFE was determined by using contact angle measurements and SR with a profilometer (n=10/group). The topography of pretreated PEEK surfaces was examined with scanning electron microscopy. Remaining specimens (n=240 per group) were conditioned with visio.link or Signum PEEK Bond, or were left untreated as the control group. Half of each group was veneered with Sinfony or VITA VM LC (n=40/group), and TBS was measured after storage in distilled water at 37°C for either 24 hours or 60 days. Data were analyzed by 4-way and 1-way ANOVA followed by the Scheffé post hoc test and chi-square test (α=.05). PEEK specimens etched with sulfuric acid resulted in higher SFE and SR than specimens without pretreatment or etching with piranha acid. Etching with sulfuric acid or piranha acid led to no general recommendations with respect to TBS. Conditioning with visio.link or Signum PEEK Bond significantly increased the TBS (P<.001). PEEK veneered with Sinfony showed significantly higher TBS values than those veneered with VITA VM LC (P<.001). Sufficient TBS for bonding to veneering resin can only be achieved when additional adhesive materials were applied. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Natural products with hypoglycemic, hypotensive, hypocholesterolemic, antiatherosclerotic and antithrombotic activities.

PubMed

Wang, H X; Ng, T B

1999-01-01

This article reviews compounds of botanical origin which are capable of lowering plasma levels of glucose and cholesterol and blood pressure, as well as compounds inhibiting atherosclerosis and thrombosis. Hypoglycemic natural products comprise flavonoids, xanthones, triterpenoids, alkaloids, glycosides, alkyldisulfides, aminobutyric acid derivatives, guanidine, polysaccharides and peptides. Hypotensive compounds include flavonoids, diterpenes, alkaloids, glycosides, polysaccharides and proteins. Among natural products with hypocholesterolemic activity are beta-carotene, lycopene, cycloartenol, beta-sitosterol, sitostanol, saponin, soybean protein, indoles, dietary fiber, propionate, mevinolin (beta-hydroxy-beta-methylglutaryl coenzyme A reductase inhibitor) and polysaccharides. Heparins, flavonoids, tocotrienols, beta-hydroxy-beta-methylglutaryl coenzyme A reductase inhibitors (statins), garlic compounds and fungal proteases exert antithrombotic action. Statins and garlic compounds also possess antiatherosclerotic activity.

Prevention of water-contamination of ethanol-saturated dentin and hydrophobic hybrid layers

PubMed Central

Sauro, Salvatore; Watson, Timothy F; Mannocci, Francesco; Tay, Franklin R; Pashley, David H

2013-01-01

SUMMARY Purpose This in vitro study evaluated the amount and the distribution of outward fluid flow that occurred when an experimental etch-and-rinse hydrophobic adhesive was applied to ethanol-saturated dentin before and after oxalate pretreatment. Materials and methods Measurements of dentin permeability were performed under a constant pulpal pressure of 20 cm H2O in deep and middle dentin. A lucifer yellow solution was placed in the pulp chamber to determine the distribution of the water contamination of the hybrid layers. Results The distribution of fluorescence in dentin specimens that were not pretreated with oxalate revealed that the dye permeated around the resin tags and filled the hybrid layer. Dentin specimens pretreated with oxalate prior to resin bonding, showed 80–83% less (p<0.05) water contamination compared to controls. The dentin permeability results obtained before and after oxalate pretreatment showed that oxalate decreased dentin permeability by 98% (p<0.05) compared to acid-etched controls. This prevented outward fluid movement during bonding resulting in better resin sealing of dentin due to the formation of a double seal of resin tags over calcium oxalate crystals in the tubules. Conclusion Outward dentinal fluid flow may contaminate hybrid layers during adhesive bonding procedures. Pretreatment of acid-etched dentin with 3% oxalic acid prior to bonding procedures can prevent outward fluid flow during bonding and water contamination of the hydrophobic hybrid layers. PMID:19701507

A new rearranged abietane diterpene and other constituents from Clerodendrum philipinum.

PubMed

Van Oanh, Ha; Sinh, Pham Xuan; An, Nguyen Thai; Hung, Ta Manh; Huong, Tran Thi Lan; Que, Do Thi Nguyet; Thao, Nguyen Phuong; Cuong, Nguyen Xuan; Dat, Nguyen Tien; Minh, Chau Van; Kiem, Phan Van

2009-03-01

From the methanolic extract of the roots of Clerodendrum philipinum, a new rearranged abietane diterpene (1) and eight known compounds were isolated by various chromatography methods. Their structures were identified by means of spectroscopic methods, including 1D- and 2D-NMR, as 17(15-->16),18(4-->3)-bisabeo-11,12,14,16-tetrahydroxy-3,5,8,11,13,15-abietahexaen-7-one (1), binankadsurin A, clerodenoside A, martynoside, acteoside, isoacteoside, astragalin, p3-sitosterol, and daucosterol. Binankadsurin A was found for the first time from a Clerodendrum species.

Two Bacterial Diterpene Synthases from Allokutzneria albata for Bonnadiene and for Phomopsene and Allokutznerene.

PubMed

Lauterbach, Lukas; Rinkel, Jan; Dickschat, Jeroen Sidney

2018-05-14

Two diterpene synthases from Allokutzneria albata were studied for their products, resulting in the identification of the new compound bonnadiene from the first enzyme. Although phylogenetically unrelated to fungal phomopsene synthase, the second enzyme produced a mixture of phomopsene and a biosynthetically linked new compound, allokutznerene, besides spiroviolene. Both enzymes were deeply studied for their mechanisms by isotopic labelling experiments, metal cofactor variation and site-directed mutagenesis. Oxidation products of phomopsene and allokutznerene are also discussed. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Furanolabdane diterpenes from Hypoestes purpurea.

PubMed

Shen, Chien-Chang; Ni, Ching-Li; Huang, Yu-Ling; Huang, Ray-Ling; Chen, Chien-Chih

2004-11-01

Four new furanolabdane diterpenes, hypopurin A (1), hypopurin B (2), hypopurin C (3), and hypopurin D (4), together with eight lignans, alpha-O-methylcubebin, beta-O-methylcubebin, hinoquinin, helioxanthin, 7-hydroxyhinokinin, dehydroxycubebin, justicidine E, and (-)-hibalactone, as well as two triterpenes, lupeol and betulin, were isolated from the dried aerial part of Hypoestes purpurea. The structures of 1-4 were elucidated mainly on the basis of NMR and MS. Compound 1 was found to be moderately cytotoxic toward the KB cell line with an IC(50) value of 9.4 microM.

Hydrophilicity of dentin bonding systems influences in vitro Streptococcus mutans biofilm formation

PubMed Central

Brambilla, Eugenio; Ionescu, Andrei; Mazzoni, Annalisa; Cadenaro, Milena; Gagliani, Massimo; Ferraroni, Monica; Tay, Franklin; Pashley, David; Breschi, Lorenzo

2014-01-01

Objectives To evaluate in vitro Streptococcus mutans (S. mutans) biofilm formation on the surface of five light-curing experimental dental bonding systems (DBS) with increasing hydrophilicity. The null hypothesis tested was that resin chemical composition and hydrophilicity does not affect S. mutans biofilm formation. Methods Five light-curing versions of experimental resin blends with increasing hydrophilicity were investigated (R1, R2, R3, R4 and R5). R1 and R2 contained ethoxylated BisGMA/TEGDMA or BisGMA/TEGDMA, respectively, and were very hydrophobic, were representative of pit-and-fissure bonding agents. R3 was representative of a typical two-step etch- and-rinse adhesive, while R4 and R5 were very hydrophilic resins analogous to self-etching adhesives. Twenty-eight disks were prepared for each resin blend. After a 24 h-incubation at 37 °C, a multilayer monospecific biofilm of S. mutans was obtained on the surface of each disk. The adherent biomass was determined using the MTT assay and evaluated morphologically with confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). Results R2 and R3 surfaces showed the highest biofilm formation while R1 and R4 showed a similar intermediate biofilm formation. R5 was more hydrophilic and acidic and was significantly less colonized than all the other resins. A significant quadratic relationship between biofilm formation and hydrophilicity of the resin blends was found. CLSM and SEM evaluation confirmed MTT assay results. Conclusions The null hypothesis was rejected since S. mutans biofilm formation was influenced by hydrophilicity, surface acidity and chemical composition of the experimental resins. Further studies using a bioreactor are needed to confirm the results and clarify the role of the single factors. PMID:24954666

Coffee Consumption Increases the Antioxidant Capacity of Plasma and Has No Effect on the Lipid Profile or Vascular Function in Healthy Adults in a Randomized Controlled Trial.

PubMed

Agudelo-Ochoa, Gloria M; Pulgarín-Zapata, Isabel C; Velásquez-Rodriguez, Claudia M; Duque-Ramírez, Mauricio; Naranjo-Cano, Mauricio; Quintero-Ortiz, Mónica M; Lara-Guzmán, Oscar J; Muñoz-Durango, Katalina

2016-03-01

Coffee, a source of antioxidants, has controversial effects on cardiovascular health. We evaluated the bioavailability of chlorogenic acids (CGAs) in 2 coffees and the effects of their consumption on the plasma antioxidant capacity (AC), the serum lipid profile, and the vascular function in healthy adults. Thirty-eight men and 37 women with a mean ± SD age of 38.5 ± 9 y and body mass index of 24.1 ± 2.6 kg/m(2) were randomly assigned to 3 groups: a control group that did not consume coffee or a placebo and 2 groups that consumed 400 mL coffee/d for 8 wk containing a medium (MCCGA; 420 mg) or high (HCCGA; 780 mg) CGA content. Both were low in diterpenes (0.83 mg/d) and caffeine (193 mg/d). Plasma caffeic and ferulic acid concentrations were measured by GC, and the plasma AC was evaluated with use of the ferric-reducing antioxidant power method. The serum lipid profile, nitric oxide (NO) plasma metabolites, vascular endothelial function (flow-mediated dilation; FMD), and blood pressure (BP) were evaluated. After coffee consumption (1 h and 8 wk), caffeic and ferulic acid concentrations increased in the coffee-drinking groups, although the values of the 2 groups were significantly different (P < 0.001); caffeic and ferulic acid concentrations were undetectable in the control group. At 1 h after consumption, the plasma AC in the control group was significantly lower than the baseline value (-2%) and significantly increased in the MCCGA (6%) and HCCGA (5%) groups (P < 0.05). After 8 wk, no significant differences in the lipid, FMD, BP, or NO plasma metabolite values were observed between the groups. Both coffees, which contained CGAs and were low in diterpenes and caffeine, provided bioavailable CGAs and had a positive acute effect on the plasma AC in healthy adults and no effect on blood lipids or vascular function. The group that did not drink coffee showed no improvement in serum lipid profile, FMD, BP, or NO plasma metabolites. This trial was registered at registroclinico.sld.cu as RPCEC00000168. © 2016 American Society for Nutrition.

A Robust Epoxy Resins @ Stearic Acid-Mg(OH)2 Micronanosheet Superhydrophobic Omnipotent Protective Coating for Real-Life Applications.

PubMed

Si, Yifan; Guo, Zhiguang; Liu, Weimin

2016-06-29

Superhydrophobic coating has extremely high application value and practicability. However, some difficult problems such as weak mechanical strength, the need for expensive toxic reagents, and a complex preparation process are all hard to avoid, and these problems have impeded the superhydrophobic coating's real-life application for a long time. Here, we demonstrate one kind of omnipotent epoxy resins @ stearic acid-Mg(OH)2 superhydrophobic coating via a simple antideposition route and one-step superhydrophobization process. The whole preparation process is facile, and expensive toxic reagents needed. This omnipotent coating can be applied on any solid substrate with great waterproof ability, excellent mechanical stability, and chemical durability, which can be stored in a realistic environment for more than 1 month. More significantly, this superhydrophobic coating also has four protective abilities, antifouling, anticorrosion, anti-icing, and flame-retardancy, to cope with a variety of possible extreme natural environments. Therefore, this omnipotent epoxy resins @ stearic acid-Mg(OH)2 superhydrophobic coating not only satisfies real-life need but also has great application potential in many respects.

Decontamination of spent ion-exchangers contaminated with cesium radionuclides using resorcinol-formaldehyde resins.

PubMed

Palamarchuk, Marina; Egorin, Andrey; Tokar, Eduard; Tutov, Mikhail; Marinin, Dmitry; Avramenko, Valentin

2017-01-05

The origin of the emergence of radioactive contamination not removable in the process of acid-base regeneration of ion-exchange resins used in treatment of technological media and liquid radioactive waste streams has been determined. It has been shown that a majority of cesium radionuclides not removable by regeneration are bound to inorganic deposits on the surface and inside the ion-exchange resin beads. The nature of the above inorganic inclusions has been investigated by means of the methods of electron microscopy, IR spectrometry and X-ray diffraction. The method of decontamination of spent ion-exchange resins and zeolites contaminated with cesium radionuclides employing selective resorcinol-formaldehyde resins has been suggested. Good prospects of such an approach in deep decontamination of spent ion exchangers have been demonstrated. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of CO2 laser on root caries inhibition around composite restorations: an in vitro study.

PubMed

de Melo, Jociana Bandeira; Hanashiro, Fernando Seishim; Steagall, Washington; Turbino, Miriam Lacalle; Nobre-dos-Santos, Marinês; Youssef, Michel Nicolau; de Souza-Zaroni, Wanessa Christine

2014-03-01

The aim of the present study was to investigate the in vitro effect of CO2 laser on the inhibition of root surface demineralization around composite resin restorations. For this purpose, 30 blocks obtained from human molar roots were divided into three groups: group 1 (negative control), cavity prepared with cylindrical diamond bur + acid etching + adhesive + composite resin restoration; group 2, cavity prepared with cylindrical diamond bur + CO2 laser (5.0 J/cm(2)) + acid etching + adhesive + composite resin; and group 3, cavity prepared with cylindrical diamond bur + CO2 laser (6.0 J/cm(2)) + acid etching + adhesive + composite resin. After this procedure, the blocks were submitted to thermal and pH cycling. Root surface demineralization around the restorations was measured by microhardness analysis. The hardness results of the longitudinally sectioned root surface were converted into percentage of mineral volume, which was used to calculate the mineral loss delta Z (ΔZ). The percentage of mineral volume, ΔZ, and the percentage of demineralization inhibition of the groups were statistically analyzed by using analysis of variance and Tukey-Kramer test. The percentage of mineral volume was higher in the irradiated groups up to 80 μm deep. The ΔZ was significantly lower in the irradiated groups than in the control group. The percentage of reduction in demineralization ranged from 19.73 to 29.21 in position 1 (50 μm), and from 24.76 to 26.73 in position 2 (100 μm), when using 6 and 5 J/cm(2), respectively. The CO2 laser was effective in inhibiting root demineralization around composite resin restorations.

Thermal and Mechanical Characteristics of Polymer Composites Based on Epoxy Resin, Aluminium Nanopowders and Boric Acid

NASA Astrophysics Data System (ADS)

Nazarenko, O. B.; Melnikova, T. V.; Visakh, P. M.

2016-01-01

The epoxy polymers are characterized by low thermal stability and high flammability. Nanoparticles are considered to be effective fillers of polymer composites for improving their thermal and functional properties. In this work, the epoxy composites were prepared using epoxy resin ED-20, polyethylene polyamine as a hardener, aluminum nanopowder and boric acid fine powder as flame-retardant filler. The thermal characteristics of the obtained samples were studied using thermogravimetric analysis and differential scanning calorimetry. The mechanical characteristics of epoxy composites were also studied. It was found that an addition of all fillers enhances the thermal stability and mechanical characteristics of the epoxy composites. The best thermal stability showed the epoxy composite filled with boric acid. The highest flexural properties showed the epoxy composite based on the combination of boric acid and aluminum nanopowder.

21 CFR 175.320 - Resinous and polymeric coatings for polyolefin films.

Code of Federal Regulations, 2012 CFR

2012-04-01

... coating is applied as a continuous film over one or both sides of a base film produced from one or more of the basic olefin polymers complying with § 177.1520 of this chapter. The base polyolefin film may... as are provided: List of substances Limitations (i) Resins and polymers: Acrylic acid polymer and its...