Science.gov

Sample records for octadecyl glyceryl ether-alpha

  1. Amended final report on the safety assessment of glyceryl dilaurate, glyceryl diarachidate, glyceryl dibehenate, glyceryl dierucate, glyceryl dihydroxystearate, glyceryl diisopalmitate, glyceryl diisostearate, glyceryl dilinoleate, glyceryl dimyristate, glyceryl dioleate, glyceryl diricinoleate, glyceryl dipalmitate, glyceryl dipalmitoleate, glyceryl distearate, glyceryl palmitate lactate, glyceryl stearate citrate, glyceryl stearate lactate, and glyceryl stearate succinate.

    PubMed

    2007-01-01

    Glyceryl Dilaurate, Glyceryl Diarachidate, Glyceryl Dibehenate, Glyceryl Dierucate, Glyceryl Dihydroxystearate, Glyceryl Diisopalmitate, Glyceryl Diisostearate, Glyceryl Dilinoleate, Glyceryl Dimyristate, Glyceryl Dioleate, Glyceryl Diricinoleate, Glyceryl Dipalmitate, Glyceryl Dipalmitoleate, Glyceryl Distearate, Glyceryl Palmitate Lactate, Glyceryl Stearate Citrate, Glyceryl Stearate Lactate, and Glyceryl Stearate Succinate are diacylglycerols (also known as diglycerides or glyceryl diesters) that function as skin conditioning agents - emollients in cosmetics. Only Glyceryl Dilaurate (up to 5%), Glyceryl Diisostearate (up to 43%), Glyceryl Dioleate (up to 2%), Glyceryl Distearate (up to 7%), and Glyceryl Stearate Lactate (up to 5%) are reported to be in current use. Production proceeds from fully refined vegetable oils, which are further processed using hydrogenation and fractionation techniques, and the end products are produced by reacting selected mixtures of the partly hydrogenated, partly fractionated oils and fats with vegetable-derived glycerine to yield partial glycerides. In the final stage of the production process, the products are purified by deodorization, which effectively removes pesticide residues and lower boiling residues such as residues of halogenated solvents and aromatic solvents. Diglycerides have been approved by the Food and Drug Administration (FDA) for use as indirect food additives. Nominally, these ingredients are 1,3-diglycerides, but are easily isomerized to the 1,2-diglycerides form. The 1,3-diglyceride isomer is not a significant toxicant in acute, short-term, subchronic, or chronic animal tests. Glyceryl Dilaurate was a mild primary irritant in albino rabbits, but not a skin sensitizer in guinea pig maximization tests. Diacylglycerol Oil was not genotoxic in the Ames test, in mammalian Chinese hamster lung cells, or in a rodent bone marrow micronucleus assay. An eye shadow containing 1.5% Glyceryl Dilaurate did not induce skin

  2. Amended final report on the safety assessment of glyceryl dilaurate, glyceryl diarachidate, glyceryl dibehenate, glyceryl dierucate, glyceryl dihydroxystearate, glyceryl diisopalmitate, glyceryl diisostearate, glyceryl dilinoleate, glyceryl dimyristate, glyceryl dioleate, glyceryl diricinoleate, glyceryl dipalmitate, glyceryl dipalmitoleate, glyceryl distearate, glyceryl palmitate lactate, glyceryl stearate citrate, glyceryl stearate lactate, and glyceryl stearate succinate.

    PubMed

    2007-01-01

    Glyceryl Dilaurate, Glyceryl Diarachidate, Glyceryl Dibehenate, Glyceryl Dierucate, Glyceryl Dihydroxystearate, Glyceryl Diisopalmitate, Glyceryl Diisostearate, Glyceryl Dilinoleate, Glyceryl Dimyristate, Glyceryl Dioleate, Glyceryl Diricinoleate, Glyceryl Dipalmitate, Glyceryl Dipalmitoleate, Glyceryl Distearate, Glyceryl Palmitate Lactate, Glyceryl Stearate Citrate, Glyceryl Stearate Lactate, and Glyceryl Stearate Succinate are diacylglycerols (also known as diglycerides or glyceryl diesters) that function as skin conditioning agents - emollients in cosmetics. Only Glyceryl Dilaurate (up to 5%), Glyceryl Diisostearate (up to 43%), Glyceryl Dioleate (up to 2%), Glyceryl Distearate (up to 7%), and Glyceryl Stearate Lactate (up to 5%) are reported to be in current use. Production proceeds from fully refined vegetable oils, which are further processed using hydrogenation and fractionation techniques, and the end products are produced by reacting selected mixtures of the partly hydrogenated, partly fractionated oils and fats with vegetable-derived glycerine to yield partial glycerides. In the final stage of the production process, the products are purified by deodorization, which effectively removes pesticide residues and lower boiling residues such as residues of halogenated solvents and aromatic solvents. Diglycerides have been approved by the Food and Drug Administration (FDA) for use as indirect food additives. Nominally, these ingredients are 1,3-diglycerides, but are easily isomerized to the 1,2-diglycerides form. The 1,3-diglyceride isomer is not a significant toxicant in acute, short-term, subchronic, or chronic animal tests. Glyceryl Dilaurate was a mild primary irritant in albino rabbits, but not a skin sensitizer in guinea pig maximization tests. Diacylglycerol Oil was not genotoxic in the Ames test, in mammalian Chinese hamster lung cells, or in a rodent bone marrow micronucleus assay. An eye shadow containing 1.5% Glyceryl Dilaurate did not induce skin

  3. 21 CFR 582.1324 - Glyceryl monostearate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... Additives § 582.1324 Glyceryl monostearate. (a) Product. Glyceryl monostearate. (b) Conditions of use. This substance is generally recognized as safe when used in accordance with good manufacturing or...

  4. 21 CFR 582.1324 - Glyceryl monostearate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... Additives § 582.1324 Glyceryl monostearate. (a) Product. Glyceryl monostearate. (b) Conditions of use. This substance is generally recognized as safe when used in accordance with good manufacturing or...

  5. Octadecyl ferulate behavior in 1,2-dioleoylphosphocholine liposomes

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Octadecyl ferulate, a lipophilic derivative of ferulic acid having antioxidant properties, is found throughout the plant and fungi kingdoms. Octadecyl ferulate was prepared using solid acid catalyst, monitored using supercritical fluid chromatograph and purified to a 42% yield. Differential scanning...

  6. Octadecyl ferulate behavior in 1,2-Dioleoylphosphocholine liposomes

    NASA Astrophysics Data System (ADS)

    Evans, Kervin O.; Compton, David L.; Whitman, Nathan A.; Laszlo, Joseph A.; Appell, Michael; Vermillion, Karl E.; Kim, Sanghoon

    2016-01-01

    Octadecyl ferulate was prepared using solid acid catalyst, monitored using Supercritical Fluid Chromatography and purified to a 42% yield. Differential scanning calorimetry measurements determined octadecyl ferulate to have melting/solidification phase transitions at 67 and 39 °C, respectively. AFM imaging shows that 5-mol% present in a lipid bilayer induced domains to form. Phase behavior measurements confirmed that octadecyl ferulate increased transition temperature of phospholipids. Fluorescence measurements demonstrated that octadecyl ferulate stabilized liposomes against leakage, maintained antioxidant capacity within liposomes, and oriented such that the feruloyl moiety remained in the hydrophilic region of the bilayer. Molecular modeling calculation indicated that antioxidant activity was mostly influenced by interactions within the bilayer.

  7. 21 CFR 184.1324 - Glyceryl monostearate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... monopalmitate (C19H38O4, CAS Reg. No. 26657-96-5) and glyceryl esters of fatty acids present in commercial stearic acid. Glyceryl monostearate is prepared by glycerolysis of certain fats or oils that are derived from edible sources or by esterification, with glycerin, of stearic acid that is derived from...

  8. 21 CFR 184.1323 - Glyceryl monooleate.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... prepared by esterification of commerical oleic acid that is derived either from edible sources or from tall oil fatty acids meeting the requirements of § 172.862 of this chapter. It contains glyceryl monooleate (C21H40O4, CAS Reg. No. 25496-72-4) and glyceryl esters of fatty acids present in commercial oleic acid....

  9. 21 CFR 184.1323 - Glyceryl monooleate.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... prepared by esterification of commerical oleic acid that is derived either from edible sources or from tall oil fatty acids meeting the requirements of § 172.862 of this chapter. It contains glyceryl monooleate (C21H40O4, CAS Reg. No. 25496-72-4) and glyceryl esters of fatty acids present in commercial oleic acid....

  10. Octadecyl ferulate behavior in 1,2-Dioleoylphosphocholine liposomes.

    PubMed

    Evans, Kervin O; Compton, David L; Whitman, Nathan A; Laszlo, Joseph A; Appell, Michael; Vermillion, Karl E; Kim, Sanghoon

    2016-01-15

    Octadecyl ferulate was prepared using solid acid catalyst, monitored using Supercritical Fluid Chromatography and purified to a 42% yield. Differential scanning calorimetry measurements determined octadecyl ferulate to have melting/solidification phase transitions at 67 and 39°C, respectively. AFM imaging shows that 5-mol% present in a lipid bilayer induced domains to form. Phase behavior measurements confirmed that octadecyl ferulate increased transition temperature of phospholipids. Fluorescence measurements demonstrated that octadecyl ferulate stabilized liposomes against leakage, maintained antioxidant capacity within liposomes, and oriented such that the feruloyl moiety remained in the hydrophilic region of the bilayer. Molecular modeling calculation indicated that antioxidant activity was mostly influenced by interactions within the bilayer. PMID:26332862

  11. Monolithic stationary phases with incorporated fumed silica nanoparticles. Part II. Polymethacrylate-based monolithic column with "covalently" incorporated modified octadecyl fumed silica nanoparticles for reversed-phase chromatography.

    PubMed

    Aydoğan, Cemil; El Rassi, Ziad

    2016-05-01

    This study is concerned with the incorporation of surface modified fumed silica nanoparticles (FSNPs) into polymethacrylate based monolithic columns for use in reversed phase chromatography (RPC) of small solutes and proteins. First, FSNPs were modified with 3-(trimethoxysilyl)propylmethacrylate (TMSPM) to yield the "hybrid" methacryloyl fumed silica nanoparticle (MFSNP) monomer. The resulting MFSNP was then mixed with glyceryl monomethacrylate (GMM) and ethylene dimethacrylate (EDMA) in a binary porogenic solvent composed of cyclohexanol and dodecanol, and the in situ copolymerization of MFSNP, GMM and EDMA was performed in a stainless steel column of 4.6 mm i.d. The silanol groups of the hybrid monolith thus obtained were grafted with octadecyl ligands by perfusing the hybrid monolithic column with a solution of 4% w/v of dimethyloctadecylchlorosilane (DODCS) in toluene while the column was maintained at 110°C for 6h (in a heated HPLC oven). One of the originalities of this study was to demonstrate MFSNP as a novel derivatized "hybrid monomer" in making RPC monolithic columns with surface bound octadecyl ligands. In this respect, the RPC behavior of the monolithic column with "covalently" incorporated FNSPs having surface grafted octadecyl ligands was evaluated with alkylbenzenes, aniline derivatives and phenolic compounds. The results showed that the hybrid poly(GMA-EDMA-MFSNP) having surface bound octadecyl ligands exhibited hydrophobic interactions under reversed phase elution conditions. Furthermore, six standard proteins were baseline separated on the column using a 10min linear gradient elution at increasing ACN concentration in the mobile phase at a flow rate of 1.0mL/min using a 10 cm×4.6mm i.d. column. The relative standard deviations (RSDs) for the retention times of the tested solutes were lower than 2.1% and 2.4% under isocratic elution and gradient elution conditions, respectively. PMID:27059396

  12. Monolithic stationary phases with incorporated fumed silica nanoparticles. Part II. Polymethacrylate-based monolithic column with "covalently" incorporated modified octadecyl fumed silica nanoparticles for reversed-phase chromatography.

    PubMed

    Aydoğan, Cemil; El Rassi, Ziad

    2016-05-01

    This study is concerned with the incorporation of surface modified fumed silica nanoparticles (FSNPs) into polymethacrylate based monolithic columns for use in reversed phase chromatography (RPC) of small solutes and proteins. First, FSNPs were modified with 3-(trimethoxysilyl)propylmethacrylate (TMSPM) to yield the "hybrid" methacryloyl fumed silica nanoparticle (MFSNP) monomer. The resulting MFSNP was then mixed with glyceryl monomethacrylate (GMM) and ethylene dimethacrylate (EDMA) in a binary porogenic solvent composed of cyclohexanol and dodecanol, and the in situ copolymerization of MFSNP, GMM and EDMA was performed in a stainless steel column of 4.6 mm i.d. The silanol groups of the hybrid monolith thus obtained were grafted with octadecyl ligands by perfusing the hybrid monolithic column with a solution of 4% w/v of dimethyloctadecylchlorosilane (DODCS) in toluene while the column was maintained at 110°C for 6h (in a heated HPLC oven). One of the originalities of this study was to demonstrate MFSNP as a novel derivatized "hybrid monomer" in making RPC monolithic columns with surface bound octadecyl ligands. In this respect, the RPC behavior of the monolithic column with "covalently" incorporated FNSPs having surface grafted octadecyl ligands was evaluated with alkylbenzenes, aniline derivatives and phenolic compounds. The results showed that the hybrid poly(GMA-EDMA-MFSNP) having surface bound octadecyl ligands exhibited hydrophobic interactions under reversed phase elution conditions. Furthermore, six standard proteins were baseline separated on the column using a 10min linear gradient elution at increasing ACN concentration in the mobile phase at a flow rate of 1.0mL/min using a 10 cm×4.6mm i.d. column. The relative standard deviations (RSDs) for the retention times of the tested solutes were lower than 2.1% and 2.4% under isocratic elution and gradient elution conditions, respectively.

  13. 21 CFR 184.1323 - Glyceryl monooleate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... commerical oleic acid that is derived either from edible sources or from tall oil fatty acids meeting the...) and glyceryl esters of fatty acids present in commercial oleic acid. (b) The ingredient must be of a... this chapter; nonalcoholic beverages and beverage bases as defined in § 170.3(n)(3) of this...

  14. 21 CFR 184.1328 - Glyceryl behenate.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... glyceryl esters of behenic acid made from glycerin and behenic acid (a saturated C22 fatty acid). The... not more than 2.5 percent free fatty acids. (2) Behenic acid. Between 80 and 90 percent of the total fatty acid content. (3) Acid value. Not more than 4. (4) Saponification value. Between 145 and 165....

  15. 21 CFR 184.1328 - Glyceryl behenate.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... glyceryl esters of behenic acid made from glycerin and behenic acid (a saturated C22 fatty acid). The... not more than 2.5 percent free fatty acids. (2) Behenic acid. Between 80 and 90 percent of the total fatty acid content. (3) Acid value. Not more than 4. (4) Saponification value. Between 145 and 165....

  16. 21 CFR 184.1328 - Glyceryl behenate.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... glyceryl esters of behenic acid made from glycerin and behenic acid (a saturated C22 fatty acid). The... not more than 2.5 percent free fatty acids. (2) Behenic acid. Between 80 and 90 percent of the total fatty acid content. (3) Acid value. Not more than 4. (4) Saponification value. Between 145 and 165....

  17. 21 CFR 184.1328 - Glyceryl behenate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... glyceryl esters of behenic acid made from glycerin and behenic acid (a saturated C22 fatty acid). The... not more than 2.5 percent free fatty acids. (2) Behenic acid. Between 80 and 90 percent of the total fatty acid content. (3) Acid value. Not more than 4. (4) Saponification value. Between 145 and 165....

  18. 21 CFR 184.1328 - Glyceryl behenate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... chapter, the ingredient is used in food with no limitation other than current good manufacturing practice. The affirmation of this ingredient is generally recognized as safe (GRAS) as a direct human food... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Glyceryl behenate. 184.1328 Section 184.1328...

  19. 21 CFR 184.1323 - Glyceryl monooleate.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...), the ingredient is used in food with no limitation other than current good manufacturing practice. The affirmation of this ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Glyceryl monooleate. 184.1323 Section...

  20. 21 CFR 184.1329 - Glyceryl palmitostearate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 10 parts per million. (c) In accordance with § 184.1(b)(1), the ingredient is used in food with no... recognized as safe (GRAS) as a direct human food ingredient is based upon the following current good... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Glyceryl palmitostearate. 184.1329 Section...

  1. 21 CFR 184.1329 - Glyceryl palmitostearate.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is based upon the... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Glyceryl palmitostearate. 184.1329 Section 184.1329 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES...

  2. 21 CFR 184.1329 - Glyceryl palmitostearate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is based upon the... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Glyceryl palmitostearate. 184.1329 Section 184.1329 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED)...

  3. 21 CFR 184.1329 - Glyceryl palmitostearate.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is based upon the... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Glyceryl palmitostearate. 184.1329 Section 184.1329 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES...

  4. 21 CFR 184.1329 - Glyceryl palmitostearate.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is based upon the... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Glyceryl palmitostearate. 184.1329 Section 184.1329 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES...

  5. 21 CFR 172.852 - Glyceryl-lacto esters of fatty acids.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Glyceryl-lacto esters of fatty acids. 172.852... HUMAN CONSUMPTION Multipurpose Additives § 172.852 Glyceryl-lacto esters of fatty acids. Glyceryl-lacto esters of fatty acids (the lactic acid esters of mono- and diglycerides) may be safely used in food...

  6. 21 CFR 172.852 - Glyceryl-lacto esters of fatty acids.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Glyceryl-lacto esters of fatty acids. 172.852... § 172.852 Glyceryl-lacto esters of fatty acids. Glyceryl-lacto esters of fatty acids (the lactic acid... conditions: (a) They are manufactured from glycerin, lactic acid, and fatty acids conforming with §...

  7. 21 CFR 172.852 - Glyceryl-lacto esters of fatty acids.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Glyceryl-lacto esters of fatty acids. 172.852... HUMAN CONSUMPTION Multipurpose Additives § 172.852 Glyceryl-lacto esters of fatty acids. Glyceryl-lacto esters of fatty acids (the lactic acid esters of mono- and diglycerides) may be safely used in food...

  8. 21 CFR 172.852 - Glyceryl-lacto esters of fatty acids.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Glyceryl-lacto esters of fatty acids. 172.852... HUMAN CONSUMPTION Multipurpose Additives § 172.852 Glyceryl-lacto esters of fatty acids. Glyceryl-lacto esters of fatty acids (the lactic acid esters of mono- and diglycerides) may be safely used in food...

  9. Biodegradation of glyceryl trinitrate by Penicillium corylophilum Dierckx.

    PubMed Central

    Zhang, Y Z; Sundaram, S T; Sharma, A; Brodman, B W

    1997-01-01

    Penicillium corylophilum Dierckx, isolated from a contaminated water wet, double-base propellant, was able to completely degrade glyceryl trinitrate (GTN) in a buffered medium (pH 7.0) containing glucose and ammonium nitrate. In the presence of 12 mg of initial fungal inoculum, GTN (48.5 to 61.6 mumol) was quantitatively transformed in a stepwise process to glyceryl dinitrate (GDN) and glyceryl mononitrate (GMN) within 48 h followed by a decrease in the GDN content with a concomitant increase in the GMN level. GDN was totally transformed to GMN within 168 h, and the complete degradation of GMN was achieved within 336 h. The presence of glucose and ammonium nitrate in the growth medium was essential for completion of the degradation of GTN and its metabolites. Complete degradation of GTN by a fungal culture has not been previously reported in the literature. PMID:9143106

  10. Formation of inclusion complexes between high amylose starch and octadecyl ferulate via steam jet cooking.

    PubMed

    Kenar, James A; Compton, David L; Little, Jeanette A; Peterson, Steve C

    2016-04-20

    Amylose-ligand inclusion complexes represent an interesting approach to deliver bioactive molecules. However, ferulic acid has been shown not to form single helical inclusion complexes with amylose from high amylose maize starch. To overcome this problem a lipophilic ferulic acid ester, octadecyl ferulate, was prepared and complexed with amylose via excess steam jet cooking. Jet-cooking octadecyl ferulate and high amylose starch gave an amylose-octadecyl ferulate inclusion complex in 51.0% isolated yield. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) confirmed that a 61 V-type inclusion complex was formed. Amylose and extraction assays showed the complex to be enriched in amylose (91.9±4.3%) and contain 70.6±5.6mgg(-1) octadecyl ferulate, although, minor hydrolysis (∼4%) of the octadecyl ferulate was observed under the excess steam jet-cooking conditions utilized. This study demonstrates that steam jet cooking is a rapid and scalable process in which to prepare amylose-octadecyl ferulate inclusion complexes. PMID:26876851

  11. Preconcentration of milk proteins using octadecylated monolithic silica microchip.

    PubMed

    Alzahrani, Eman; Welham, Kevin

    2013-10-10

    Sample preparation is a bottleneck in systems for chemical analysis and it is a required step in order to remove interference and preconcentrate the target analytes. Much research in recent years has focused on porous monolithic materials since they are highly permeable to liquid flow and show high mass transfer compared with common packed beds. This study has focused on the use of a glass microchip containing an inorganic silica-based monolithic material modified with octadecyl groups for preconcentration of milk proteins from skimmed cows' milk that vary in molecular weight, hydrophobicity, and abundance. Comparison between the fabricated device and a commercial cartridge for the preconcentration of proteins in skimmed cows' milk showed the ability of the device to successfully enrich protein mixtures from the sample. The three replicate experiments showed that the RSD of the mass to charge ratio of milk proteins ranged from 0.01 to 0.46%. In addition, it was found that there were no significant differences between the observed and reported masses of the milk proteins and the relative percentage error of the molecular masses ranged between 0.03 and 0.90%. The fact that the small amounts of sample required and short sample preparation time suggest that this new microfluidic device may be a viable alternative to existing procedures for protein extraction from real samples. PMID:24070482

  12. Formation of inclusion complexes between high amylose starch and octadecyl ferulate via steam jet cooking

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Amylose can form inclusion complexes with guest molecules and represents an interesting approach to deliver bioactive molecules. However, ferulic acid has been shown not to form single helical inclusion complexes with amylose. To overcome this problem a ferulic acid ester, octadecyl ferulate, posses...

  13. Bioadhesive drug delivery systems. I. Characterisation of mucoadhesive properties of systems based on glyceryl mono-oleate and glyceryl monolinoleate.

    PubMed

    Nielsen, L S; Schubert, L; Hansen, J

    1998-07-01

    A group of fatty acid esters capable of forming liquid crystals has been identified as a new class of potential bioadhesive substances. The liquid crystals may act as a controlled release system. The experimental work was focused on the monoglycerides, glyceryl mono-oleate (GMO) and glyceryl monolinoleate (GML). The mucoadhesive properties of GMO and GML were demonstrated in vitro by a 'flushing' bioadhesion test system and a tensiometric method. The flushing system was validated with GMO. Mucoadhesion is influenced by the drug and excipient added, their concentrations, and the ability to form especially the cubic phase. It has been shown that the cubic phase is mucoadhesive when formed on wet mucosa, such as rabbit jejunum, and that drug added to the precursor formulation is incorporated in the cubic phase formed. Tensiometric measurements have shown that the unswollen monoglycerides have the greatest mucoadhesion, followed by the partly swollen lamellar phase and the fully swollen cubic phase. The values found for the work of adhesion were in the range 0.007-0.048 mJcm-2. The mechanism of mucoadhesion is unspecific and probably involves dehydration of the mucosa. The cubic phase of GMO and GML may be an interesting candidate for a bioadhesive drug delivery system.

  14. Superheated water as chromatographic eluent for parabens separation on octadecyl coated zirconia stationary phase.

    PubMed

    Dugo, Paola; Buonasera, Katia; Crupi, Maria Lucia; Cacciola, Francesco; Dugo, Giovanni; Mondello, Luigi

    2007-05-01

    In this study, the use of pure water at superheated temperatures, between 100 and 200 degrees C, as a mobile phase for RP separation is explored. Instrumental parameters, such as temperature, flow rate, preheating and cooling, have shown significant effects on the quality of the chromatographic peaks. The properties of superheated water as an eluent were investigated by observing the chromatographic behaviour of four parabens on a carbon-clad zirconia (ZR) phase with covalently bonded octadecyl groups. Results were compared with those obtained at 30 degrees C on a silica-based phase with octadecyl groups, using water and ACN as mobile phase. The optimized method was finally applied to analyse parabens in a commercial body cream. PMID:17595947

  15. Antifungal activity and isomerization of octadecyl p-coumarates from Ipomoea carnea subsp. fistulosa.

    PubMed

    Nidiry, Eugene Sebastian J; Ganeshan, Girija; Lokesha, Ankanahalli N

    2011-12-01

    Bioassay monitored HPLC assisted isolation and purification of the chief antifungal fraction of the leaves of Ipomoea carnea subsp. fistulosa (Convulvulaceae) were achieved using Colletotrichum gloeosporioides and Cladosporium cucumerinum as test organisms. The activity of the purified fraction was further confirmed by the dose dependent inhibition of the spore germination of Alternaria alternata and A. porri. The active fraction was identified as a mixture of (E)-octadecyl p-coumarate and (Z)-octadecyl p-coumarate. The two isomers were detected on an HPLC column with substantially different retention times, but once eluted from the column, one form was partly converted to the other in daylight. Conclusive evidence for the structures and their isomerization were obtained from the HPLC behavior, IR, UV, HRESIMS, CIMS and and NMR spectral data. Important 1H NMR and 13C NMR signals could be separately assigned for the isomers using 2D NMR techniques. PMID:22312731

  16. Chromatographic analysis of the neutral and phosphatide glyceryl ethers from various biological sources.

    PubMed

    Hack, M H; Helmy, F M

    1975-04-01

    A method of analysis is described which permits the facile evaluation of the neutral glyceryl ether lipids (mild alkaline hydrolysis) and total glyceryl ether lipid (Vitride reduction) thereby allowing an assessment of the phosphatide contribution. The alkyl and alk-enyl glyceryl ethers are chromatographically resolvable on Gelman glass-fiber type SG and Whatman SG-81 and detected by the periodic acid-Schiff and plasmal reaction, respectively. The attending problems and interpretation are discussed with examples from a number of unicellular organisms and animal tissues.

  17. Effect of tablet structure on controlled release from supersaturating solid dispersions containing glyceryl behenate.

    PubMed

    Keen, Justin M; Hughey, Justin R; Bennett, Ryan C; Jannin, Vincent; Rosiaux, Yvonne; Marchaud, Delphine; McGinity, James W

    2015-01-01

    The objective of this study was to evaluate the use of glyceryl behenate as a plasticizer and release modifier in solid dispersion systems containing itraconazole and carbamazepine. Amorphous solid dispersions of high molecular weight polyvinylpyrrolidone were prepared by hot-melt extrusion, the processing of which was improved by the inclusion of glyceryl behenate. Dispersions were milled and subsequently compressed into tablets. Solid dispersions were also prepared by KinetiSol Dispersing, which allowed for the manufacture of monolithic tablets of the same composition and shape as compressed tablets. Tablets without glyceryl behenate and all compressed tablets were observed to have an incomplete release profile likely due to drug crystallization within the tablet as this occurred at conditions in which dissolution concentrations were below saturation. Monolithic tablets formulated to be more hydrophobic, by including glyceryl behenate, allowed for sustained release below and above saturation conditions.

  18. [Secretagogue action of glyceryl guaiacolate in tracheal submucosal glands (author's transl)].

    PubMed

    Yanaura, S; Takeda, H; Misawa, M

    1982-01-01

    The effects of glyceryl guaiacolate on secretory activities of tracheal secretory cells and on behavior of mucus glycoprotein in these cells were investigated histologically and histochemically using isolated canine trachea. Following glyceryl guaiacolate treatment, the number of total glycoprotein-containing goblet cells (GC) did not change. The numbers of acid glycoprotein (AGP)-, neutral glycoprotein (NGP)-, and sulphated glycoprotein (SGP)-containing GC were also unaltered in a concentration range of 10(-7) to 10(-4)M. On the other hand the acinar inner diameter of the submucosal gland (SG) and the acinar inner diameter to wall ratio significantly increased, while thickness of acinus significantly decreased with 10(-6), 10(-5) and 10(-4)M glyceryl guaiacolate. AGP and SGP contents in glandular cells markedly decreased, while the ratio of the numbers of AGP- to NGP-containing glandular cell were the same, suggesting that glyceryl guaiacolate does not change the quality of mucus glycoprotein in GC and SG. Glyceryl guaiacolate produced a marked increase in total saccharide, protein, and N-acetylhexosamine concentrations in the incubation fluid. These findings suggest that glyceryl guaiacolate has no influence on the secretory activity of GC, but markedly stimulates the activity of SG. The secretagogue effect of the agent would be ascribable to stimulation of mucus discharge, but not stimulation of mucus synthesis. PMID:7061026

  19. Synthesis of octadecyl esters of histidine-containing tripeptides as potential regulators of plant growth

    SciTech Connect

    Ogrel, A.A.; Zvonkova, E.N.; Gafurov, R.G.

    1995-08-01

    Octadecyl esters of dipeptides and tripeptides of the type Phe-His, Val-His, Phe-Val-His and Val-Phe-His were synthesized using different methods. The minimum energy conformations of these peptides were calculated with computer minimization programs and compared with those of paclobutrazol, a well-known regulator of plant growth. It was demonstrated that the elongation of the peptide chain leads to a higher topochemical correspondence between paclobutrazol and the peptide derivatives than between paclobutrazol and amino acid derivatives. 9 refs., 2 figs., 3 tabs.

  20. Peptide washout and permeability from glyceryl monooleate buccal delivery systems.

    PubMed

    Lee, Jaehwi; Kellaway, Ian W

    2002-10-01

    Simultaneous evaluation of the permeation and washout of a peptide from the mucoadhesive liquid crystalline phases of glyceryl monooleate (GMO) has been investigated using a donor compartment flow-through diffusion cell. [D-Ala2, D-Leu5]enkephalin (DADLE) was incorporated into the cubic and lamellar liquid crystalline phases of GMO and applied to excised porcine buccal mucosa mounted in the donor compartment flow-through cell. Phosphate-buffered saline pH 7.4 (PBS) was pumped across the upper surface of the liquid crystalline phases to mimic salivary flow. The steady-state fluxes of DADLE and GMO from the cubic phase were significantly greater than that from the lamellar phase (P < 0.01). There was no statistical difference between the amounts of DADLE and GMO washed out from the lamellar and cubic phases (P > 0.05). The donor compartment flow-through diffusion cell was found to be a useful tool to evaluate the impact of salivary washout on mucoadhesive oral mucosal delivery systems.

  1. Targeting of lysosomes by liposomes modified with octadecyl-rhodamine B

    PubMed Central

    Koshkaryev, Alexander; Thekkedath, Ritesh; Pagano, Cinzia; Meerovich, Igor; Torchilin, Vladimir P.

    2014-01-01

    The use of lysosome-targeted liposomes may significantly improve a delivery of therapeutic enzymes into lysosomes for the treatment of lysosome-associated diseases. The aim of this research was to achieve a specific intracellular targeting of lysosomes, by using liposomes modified with the lysosomotropic octadecyl-rhodamine B (RhB) and loaded with a model compound, fluorescein isothiocyanate (FITC)–dextran (FD). Plain and RhB-modified liposomes were prepared by hydration of lipid films and loaded with FD or with 5-dodecanoylaminofluorescein di-β-D-galactopyranoside (C12FDG), a specific substrate for the intralysosomal β-galactosidase. The delivery of these liposomes and their content to lysosomes in HeLa cells was investigated by confocal microscopy, flow cytometry, and subcellular fractionation. Confocal microscopy demonstrated that RhB-liposomes co-localize well with the specific lysosomal markers, unlike plain liposomes. The comparison of the FITC fluorescence of the lysosomes isolated by subcellular fractionation also showed that the efficiency of FD delivery into lysosomes by RhB-modified liposomes was significantly higher compared with plain liposomes. These results were additionally confirmed by the flow cytometry of the intact cells treated with C12FDG-loaded liposomes that also demonstrated increased lysosomal targeting by RhB-modified liposomes. The modification of the liposomal surface with a lysosomotropic ligand, such as octadecyl-RhB, can significantly increase the delivery of liposomal loads to lysosomes. PMID:21275828

  2. Exposure to glyceryl trinitrate during gun powder production: plasma glyceryl trinitrate concentration, elimination kinetics, and discomfort among production workers.

    PubMed

    Gjesdal, K; Bille, S; Bredesen, J E; Bjørge, E; Halvorsen, B; Langseth, K; Lunde, P K; Silvertssen, E

    1985-01-01

    Plasma glyceryl trinitrate (GTN) concentration was studied in 12 volunteers producing gun powder. Serial blood samples were obtained from the cubital vein before and during work at two sites of production; high concentrations of GTN were detected in the plasma. Control specimens from a femoral vein contained much less GTN, indicating that blood in the cubital vein was enriched by dermally absorbed GTN. In the roll mill area concentrations of GTN in the cubital vein were higher than in the press area, but individual factors were also important since some workers consistently had higher concentration of GTN than others. Differences in absorption were more important than differences in the metabolism of GTN since only a small variation in disappearance rate was found after a sublingual test dose of GTN. Moderate changes in pulse rate and blood pressure were noted during the day. The major discomfort experienced was a headache that increased during working hours, but this was not significantly related to GTN concentrations in the air or in the blood from the cubital vein. The observations imply that major efforts should be made to reduce dermal contact with GTN during production work.

  3. STUDY OF DUAL MATRIX TABLETS CONTAINING HYPROMELLOSE OF DIFFERENT VISCOSITY DEGREE AND GLYCERYL DIBEHENATE.

    PubMed

    Mužíková, Jitka; Holubová, Katerina; Komersová, Alena; Lochar, Václav

    2016-01-01

    Studies are described on the compressibility of directly compressible tableting materials containing two viscosity types of hypromellose in two concentrations and tableting materials containing additional glyceryl dibehenate, also in two concentrations. Compressibility is evaluated by means of the energy profile of the compression process and determination of tensile strength of tablets. Dissolution test examines the rate of release of the active ingredient from matrix tablets, which is subsequently evaluated mathematically. Increased concentrations of both hypromelloses and an addition of glyceryl dibehenate into tablets with both types of hypromellose improved compressibility. The rate of drug release was decreased with increasing viscosity degree of hypromellose and its increasing concentration. An addition of glyceryl dibehenate exerted the same influence on release as increased concentrations of the pertinent hypromellose.

  4. 21 CFR 172.852 - Glyceryl-lacto esters of fatty acids.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Glyceryl-lacto esters of fatty acids. 172.852 Section 172.852 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) FOOD FOR HUMAN CONSUMPTION (CONTINUED) FOOD ADDITIVES PERMITTED FOR DIRECT ADDITION TO FOOD...

  5. Targeted therapy of colorectal neoplasia with rapamycin in peptide-labeled pegylated octadecyl lithocholate micelles

    PubMed Central

    Khondee, Supang; Rabinsky, Emily F.; Owens, Scott R.; Joshi, Bishnu P.; Qiu, Zhen; Duan, Xiyu; Zhao, Lili; Wang, Thomas D.

    2015-01-01

    Many powerful drugs have limited clinical utility because of poor water solubility and high systemic toxicity. Here, we formulated a targeted nanomedicine, rapamycin encapsulated in pegylated octadecyl lithocholate micelles labeled with a new ligand for colorectal neoplasia, LTTHYKL peptide. CPC;Apc mice that spontaneously develop colonic adenomas were treated with free rapamycin, plain rapamycin micelles, and peptide-labeled rapamycin micelles via intraperitoneal injection for 35 days. Endoscopy was performed to monitor adenoma regression in vivo. We observed complete adenoma regression at the end of therapy. The mean regression rate for peptide-labeled rapamycin micelles was significantly greater than that for plain rapamycin micelles, P<0.01. On immunohistochemistry, we observed a significant reduction in phospho-S6 but not β-catenin expression and reduced tumor cell proliferation, suggesting greater inhibition of downstream mTOR signaling. We observed significantly reduced renal toxicity for peptide-labeled rapamycin micelles compared to that of free drug, and no other toxicities were found on chemistries. Together, this unique targeted micelle represents a potential therapeutic for colorectal neoplasia with comparable therapeutic efficacy to rapamycin free drug and significantly less systemic toxicity. PMID:25483425

  6. Assessment of dermal glyceryl trinitrate and isosorbide dinitrate for patients with angina pectoris.

    PubMed Central

    Hubner, P J; Jones, P R; Galer, I A

    1985-01-01

    Dermal nitrate preparations are claimed to be useful in the treatment of angina, as their slow absorption by-passing the liver leads to a sustained action. Ten patients with angina were exercised on a treadmill after dermal application of 16.64 mg glyceryl trinitrate or 100 mg isosorbide dinitrate or placebo. Exercise duration was significantly increased at one and three hours for both nitrate preparations but not at six hours after application. The calculated workload achieved was significantly increased (p less than 0.01) at one and three hours for both preparations and at six hours (p less than 0.05) for isosorbide dinitrate. Headaches were common with glyceryl trinitrate cream. The dermal nitrate preparations studied had a duration of antianginal action similar to that of oral nitrate tablets. Aside from their value when the oral route cannot be used or absorption may be delayed, dermal nitrate preparations have no advantage over oral preparations for angina pectoris. PMID:3918653

  7. Prostaglandin E2-Glyceryl Ester: In Vivo Evidence for a Distinct Pharmacological Identity from Intraocular Pressure Studies.

    PubMed

    Woodward, David F; Poloso, Neil J; Wang, Jenny W

    2016-08-01

    Prostaglandin E2 (PGE2)-2-glyceryl ester is a cyclo-oxygenase 2 product of the endocannabinoid 2-arachidonyl glycerol. It is claimed as pharmacologically novel, but this is complicated by rapid and irreversible isomerization to the 1(3) ester. For ocular studies, enzymatic hydrolysis of the ester moiety creates an additional complication. PG-glyceryl esters were stabilized to isomerization and hydrolysis by replacing the noncarbonyl O with NH, to form the serinolamide and propanediolamide as stable analogs of PG-2-glyceryl and PG-2-1(3) glyceryl esters, respectively. Intraocular pressure was measured in conscious dogs and conscious laser-induced ocular hypertensive monkeys. Pharmacological studies involved stable transfectants for each of the human recombinant prostanoid receptors and the isolated feline iris for prostamide activity. PGE2-serinolamide and PGE2- propanediolamide were essentially inactive at all receptors except the EP3 receptor (EC50, ∼500 nM). This obliged elucidation of EP3 receptor involvement in the intraocular pressure response to these PGE2-glycyerl ester analogs. Since the EP3 receptor agonists sulprostone and GR 63799 did not lower monkey intraocular pressure, a role for EP3 receptors in mediating the effects of PGE2-serinolamide and PGE2-propanediolamide is not indicated. PGE2-glyceryl ester (0.01% and 0.1%) substantially lowered intraocular pressure in monkeys. PGE2-propanediolamide was more efficacious than PGE2-serinolamide in lowering intraocular pressure in monkey eyes, but both appeared equieffective in dog eyes. PGE2-serinolamide dose-dependently (0.01- 0.1%) lowered intraocular pressure in both species, but PGF2 α-serinolamide was inactive. In conclusion, stable PGE2-glyceryl ester analogs lowered intraocular pressure. These findings are consistent with the presence of a PGE2-glyceryl ester-specific recognition site in the eye. PMID:27217589

  8. Liquid chromatography of polyglycerol fatty esters and fatty ethers on porous graphitic carbon and octadecyl silica by using evaporative light scattering detection and mass spectrometry.

    PubMed

    Cassel, S; Chaimbault, P; Debaig, C; Benvegnu, T; Claude, S; Plusquellec, D; Rollin, P; Lafosse, M

    2001-06-01

    A liquid chromatographic method has been developed for the analysis of polyglycerol fatty esters and fatty ethers which are non-ionic surfactants. Two methods were compared using either octadecyl silica or porous graphitic carbon. The octadecyl silica system with a hydroorganic mobile phase enables to compare the hydrophobic behavior of the compounds. The porous graphitic carbon enables the separation of the diastereoisomers. Detection of these non-UV-absorbing compounds was achieved by evaporative light scattering detection. Identification of isomers was performed by mass spectrometry.

  9. A novel glyceryl monoolein-bearing cubosomes for gambogenic acid: Preparation, cytotoxicity and intracellular uptake.

    PubMed

    Luo, Qing; Lin, Tongyuan; Zhang, Cai Yuan; Zhu, Tingting; Wang, Lei; Ji, Zhaojie; Jia, Buyun; Ge, Tao; Peng, Daiyin; Chen, Weidong

    2015-09-30

    Lyotropic cubic liquid crystalline nanoparticles, also known as 'cubosomes', have been tested as effective carriers for a variety of drugs due to their ability to enhance delivery efficiency and reduced drug side effects. Cubosomes are colloidal carriers composed of biodegradable Glyceryl monooleate and F127. Being composed of well tolerable and physiological materials, these carriers are well tolerated, compatible and non-toxic. In this study, therefore, we developed a novel, water-soluble, glyceryl monooleate and F127 based multiblock copolymer for Gambogenic acid (GNA) by emulsion-evaporation and low temperature-solidification technique. Physicochemical properties, in vitro cytotoxicity, cellular uptake and in vivo pharmacokinetic of GNA-loaded cubosomes (GNA-Cubs) were investigated. The results revealed that GNA-Cubs were spherical or ellipsoidal monocellular by dynamic light scattering, meanwhile, 150-250nm in mean size with narrow polydispersity indexas determined by transmission electron microscopy. Small angle X-ray scattering indicated that GNA-Cubs retain the Pn3m cubic symmetry. Compared with GNA solution, GNA-Cubs exhibited markedly prolonged inhibitory activity in SMMC-7721 cells, as well as time-dependent increases in intra-cellular uptake. Furthermore, in vivo pharmacokinetic study showed that the Cmax values and the AUC of GNA-Cubs were higher than GNA solution approximately 1.2-fold and 9.1-fold, respectively. In conclusion, the results showed that the cubic liquid crystalline nanoparticles could be a potentially nanocarrier in the delivery of GNA for cancer therapy. PMID:26209071

  10. Development of a pressure-sensitive glyceryl tristearate capsule filled with a drug-containing hydrogel.

    PubMed

    Wilde, Lisa; Bock, Mona; Glöckl, Gunnar; Garbacz, Grzegorz; Weitschies, Werner

    2014-01-30

    The purpose of this work was to develop a new pressure-sensitive dosage form that breaks and releases its content in a fasted stomach at the predominant pressure at the pylorus. The content of the dosage form should be liquid so that the active pharmaceutical ingredient quickly reaches maximum absorption in the upper small intestine. For this purpose glyceryl tristearate capsules were developed, consisting of an extremely brittle shell, with a crushing behavior that can be controlled by modification of the shell thickness. The capsules were filled with a hydroxyethyl cellulose gel containing paracetamol. Dissolution testing using USP apparatus 2, performed for simulating the resting time in the stomach, did not show any release. Studies using a texture analyser showed a correlation between the glyceryl tristearate filling volume and the necessary force to break the capsule. Physiological conditions in dissolution testing, such as movement, pressure and discontinuous medium contact, were set in a stress test device and showed that the dosage forms did not break and release its pharmaceutical ingredient until a pressure of 300 mbar was applied which served as a threshold limit for physiological pressure occurring during gastric emptying of large solids. PMID:24333906

  11. Self-Assembly of Amphiphilic Block Copolymers Containing Poly(n-octadecyl acrylate) Block in Aqueous Solution

    NASA Astrophysics Data System (ADS)

    Akiba, Isamu; Akino, Yusuke; Masunaga, Hiroyasu; Sakurai, Kazuo

    2010-11-01

    Synchrotron small-angle X-ray scattering (SAXS) experiments were carried out for poly(acrylic acid)-block-poly(n-octadecyl acrylate) (PAA-b-PODA) and PAA-b-PODA-b-PAA micelles in aqueous solutions. SAXS results indicated that PAA-b-PODA and PAA-b-PODA-b-PAA formed core-shell micelles with disk-like morphology below melting temperature of PODA in aqueous solutions. The thickness of PAA-b-PODA (diblock copolymer) micelle was larger than that of PAA-b-PODA-b-PAA (triblock copolymer) micelle. The difference of sizes between these micelles was related to difference of molecular architectures of PAA-b-PODA and PAA-b-PODA-b-PAA. PAA-b-PODA micelle showed morphological transition from disk to spherical shape with elevating temperature. On the contrary, PAA-b-PODA-b-PAA micelle maintained disk-like shape above melting temperature, although enlargement of micelle thickness is caused.

  12. Bonding efficacy and side effects of the high purity glyceryl mono-methacrylate.

    PubMed

    Takahashi, Y; Itoh, K; Manabe, A; Tani, C; Hisamitsu, H

    2004-12-01

    The purpose of this study was to examine the efficacy of experimentally developed high purity glyceryl mono-methacrylate (GM) as a dentine primer and to evaluate the possibility of allergic reaction. The efficacy of experimental dentine primers was evaluated by measuring the polymerization contraction gap width and the tensile bond strength. Allergic reaction was evaluated by the guinea-pig maximization test. The skin reaction was evaluated according to the criteria of the International Contact Dermatitis Research Group. Contraction gap formation was completely prevented and the tensile bond strength was not significantly affected by priming with GM on high-purity GM. The allergic response decreased when high-purity GM was employed as the challenger. It was concluded that the clinical use of the high-purity GM is beneficial as the delayed allergic reaction could be avoided with no detrimental effect on the dentine bonding. PMID:15544652

  13. Preparation and evaluation of glyceryl monooleate-coated hollow-bioadhesive microspheres for gastroretentive drug delivery.

    PubMed

    Liu, Yuanfen; Zhang, Jianjun; Gao, Yuan; Zhu, Jiabi

    2011-07-15

    The purpose of this study was to produce hollow and bioadhesive microspheres to lengthen drug retention time in the stomach. In these microspheres, ethylcellulose was used as the matrix, Eudragit EPO was employed to modulate the release rate, and glyceryl monooleate (GMO) was the bioadhesive polymer in situ. The morphological characteristics of the microspheres were defined using scanning electron microscopy. The in vitro release test showed that the release rate of drug from the microspheres was pH-dependent, and was not influenced by the GMO coating film. The prepared microspheres demonstrated strong mucoadhesive properties with good buoyancy both in vitro and in vivo. Pharmacokinetic analysis indicated that the elimination half-life time of the hollow-bioadhesive microspheres was prolonged, and that the elimination rate was decreased. In conclusion, the hollow-bioadhesive synergic drug delivery system may be advantageous in the treatment of stomach diseases.

  14. Biotransformation of glyceryl trinitrate occurs concurrently with relaxation of rabbit aorta

    SciTech Connect

    Brien, J.F.; McLaughlin, B.E.; Breedon, T.H.; Bennett, B.M.; Nakatsu, K.; Marks, G.S.

    1986-05-01

    This study was conducted to test the hypothesis that biotransformation of glyceryl trinitrate (GTN) is involved in GTN-induced relaxation of vascular smooth muscle. Isolated rabbit aortic strips (RAS) were contracted submaximally with phenylephrine (PE) and then were incubated with 0.5 microM (/sup 14/C)GTN in a time course study. GTN-induced relaxation (inhibition of PE-induced tone) of RAS was monitored and tissue GTN and glyceryl-1,2- and 1,3-dinitrate (GDN) concentrations were measured by thin-layer chromatography and liquid scintillation spectrometry at 0.5, 1, 2 and 20 min after incubation. Biotransformation of GTN to GDN occurred during GTN-induced relaxation of RAS. The tissue GDN concentration was dependent on the time duration of incubation with GTN and was related to the magnitude of GTN-induced tissue relaxation. At the 20-min interval, the GDN concentration in the incubation medium indicated appreciable efflux of GDN metabolites from the RAS. In the biotransformation of GTN by RAS, there was about 4-fold preferential formation of 1,2-GDN compared with 1,3-GDN. RAS were made tolerant to GTN in vitro by incubation with 500 microM GTN for 1 hr. After washing, GTN-tolerant and nontolerant (incubation with vehicle for 1 hr) RAS were contracted submaximally with PE, and then were incubated with 0.5 microM (/sup 14/C)GTN for 2 min. GTN-induced relaxation of RAS and tissue GDN concentration were significantly less for GTN-tolerant tissue compared with nontolerant tissue. Tissue GTN concentration was similar for both GTN-tolerant and nontolerant RAS, which indicated that the tissue uptake of GTN was similar and that GTN biotransformation was diminished in tolerant tissue.(ABST

  15. A new sunscreen of the cinnamate class: synthesis and enzymatic hydrolysis evaluation of glyceryl esters of p-methoxycinnamic acid.

    PubMed

    de Freitas, Zaida Maria Faria; dos Santos, Elisabete Pereira; da Rocha, João Ferreira; Dellamora-Ortiz, Gisela Maria; Gonçalves, José Carlos Saraiva

    2005-05-01

    Glyceryl esters of p-methoxycinnamic acid, 1,3-dipalmitoyl-2-p-methoxycinnamoyl-1,2,3-propanetriol and 1,3-dioctanoyl-2-p-methoxycinnamoyl-1,2,3-propanetriol were synthesised in an attempt to increase substantivity and decrease eventual undesirable effects of sunscreens of this class. To assess if the glyceryl esters could present a higher stability towards hydrolysis by lipases in the stratum corneum, hydrolysis rates were determined in vitro using a commercial fungal lipase from Rhizomucor miehei. Results presented herein show that the glyceryl esters have similar lambda(max) and epsilon values to sunscreens of the cinnamate class. The ester 1,3-dipalmitoyl-2-p-methoxycinnamoyl-1,2,3-propanetriol presented a 2.8 times lower hydrolysis rate by lipase, in vitro, than the commercial sunscreen 2-ethylhexyl-p-methoxycinnamate (alkyl ester). This finding suggests that this triacylglycerol can possibly have a longer retention time in the skin and consequently promote a more intense and effective antisolar action than the commercial sunscreen.

  16. Silymarin glyceryl monooleate/poloxamer 407 liquid crystalline matrices: physical characterization and enhanced oral bioavailability.

    PubMed

    Lian, Ruyue; Lu, Yi; Qi, Jianping; Tan, Yanan; Niu, Mengmeng; Guan, Peipei; Hu, Fuqiang; Wu, Wei

    2011-12-01

    Silymarin, a mixture of flavonolignans extracted from the seeds of milk thistle, is used clinically as a hepatoprotector to treat liver injuries and chronic hepatitis. However, its therapeutic effect is compromised by its poor oral bioavailability due to the poor solubility and low permeability across intestinal epithelia. The main purpose of this study was to prepare silymarin glyceryl monooleate/poloxamer 407 liquid crystalline matrices (GMO/P407 LCM) to improve the oral bioavailability of silymarin. GMO/P407 LCMs were prepared by a melting/congealing method. The isotropic phenomenon observed under polarized light microscope confirmed the liquid crystalline structure at the junction of LCM and water. Both differential scanning calorimetry and X-ray diffraction analysis confirmed disappearance of silymarin crystallinity after incorporation into the LCMs. In vitro release of silymarin from LCMs was limited, whereas LCMs were readily degraded by lipase and released silymarin quickly and completely. Pharmacokinetic study in beagle dogs showed significantly increased peak concentration for silymarin GMO/P407 LCM, and, most importantly, a 3.46-fold increase in oral bioavailability as compared with Legalon®, a commercial silymarin formulation.

  17. Development and evaluation of liquid embolic agents based on liquid crystalline material of glyceryl monooleate.

    PubMed

    Du, Ling-Ran; Lu, Xiao-Jing; Guan, Hai-Tao; Yang, Yong-Jie; Gu, Meng-Jie; Zheng, Zhuo-Zhao; Lv, Tian-Shi; Yan, Zi-Guang; Song, Li; Zou, Ying-Hua; Fu, Nai-Qi; Qi, Xian-Rong; Fan, Tian-Yuan

    2014-08-25

    New type of liquid embolic agents based on a liquid crystalline material of glyceryl monooleate (GMO) was developed and evaluated in this study. Ternary phase diagram of GMO, water and ethanol was constructed and three isotropic liquids (ILs, GMO:ethanol:water=49:21:30, 60:20:20 and 72:18:10 (w/w/w)) were selected as potential liquid embolic agents, which could spontaneously form viscous gel cast when contacting with water or physiological fluid. The ILs exhibited excellent microcatheter deliverability due to low viscosity, and were proved to successfully block the saline flow when performed in a device to simulate embolization in vitro. The ILs also showed good cytocompatibility on L929 mouse fibroblast cell line. The embolization of ILs to rabbit kidneys was performed successfully under monitoring of digital subtraction angiography (DSA), and embolic degree was affected by the initial formulation composition and used volume. At 5th week after embolization, DSA and computed tomography (CT) confirmed the renal arteries embolized with IL did not recanalize in follow-up period, and an obvious atrophy of the embolized kidney was observed. Therefore, the GMO-based liquid embolic agents showed feasible and effective to embolize, and potential use in clinical interventional embolization therapy.

  18. Liquid crystalline phases and their dispersions in aqueous mixtures of glycerol monooleate and glyceryl monooleyl ether.

    PubMed

    Popescu, Georgeta; Barauskas, Justas; Nylander, Tommy; Tiberg, Fredrik

    2007-01-16

    The aqueous phase behavior of mixtures of 1-glycerol monooleate (GMO) and its ether analogue, 1-glyceryl monooleyl ether (GME) has been investigated by a combination of polarized microscopy, X-ray diffraction, and NMR techniques. Three phase diagrams of the ternary GMO/GME/water system have been constructed at 25, 40, and 55 degrees C. The results demonstrate that the increasing amount of GME favors the formation of the reversed phases, evidenced by the transformation of the lamellar and bicontinuous cubic liquid crystalline phases of the binary GMO/water system into reversed micellar or reversed hexagonal phases. For a particular liquid crystalline phase, increasing the GME content has no effect on the structural characteristics and hydration properties, thus suggesting ideal mixing with GMO. Investigations of dispersed nanoparticle samples using shear and a polymeric stabilizer, Pluronic F127, show the possibility of forming two different kinds of bicontinuous cubic phase nanoparticles by simply changing the GMO/GME ratio. Also NMR self-diffusion measurements confirm that the block copolymer, Pluronic F127, used to facilitate dispersion formation, is associated with nanoparticles and provides steric stabilization.

  19. A unique glyceryl diglycoside identified in the thermophilic, radiation-resistant bacterium Rubrobacter xylanophilus.

    PubMed

    Lamosa, Pedro; Lourenço, Eva C; d'Avó, Filipa; Nobre, Ana; Bandeiras, Tiago M; da Costa, Milton S; Ventura, M Rita; Santos, Helena

    2015-03-01

    The solute pool of the actinobacterium Rubrobacter xylanophilus has been investigated as a function of the growth temperature and concentration of NaCl in the medium (Empadinhas et al. Extremophiles 11: 667-673, 2007). Changing the carbon source from glucose to maltose in a minimal growth medium led to the accumulation of an unknown organic compound whose structure was investigated by NMR and confirmed by chemical synthesis in the present study as: (2R)-2-(1-O-α-D-mannopyranosyl)-3-(1-O-α-D-glucopyranosyl)-D-glycerate (MGlyG). In addition to this newly identified diglycoside, the solute pool of R. xylanophilus included trehalose, mannosylglycerate, di-myo-inositol phosphate and di-N-acetyl-glucosamine phosphate. The structure of MGlyG was established by NMR and confirmed by chemical synthesis. The availability of g-amounts of the synthetic material allowed us to perform stabilization tests on three model enzymes (malate dehydrogenase, staphylococcal nuclease, and lysozyme), and compare the efficacy of MGlyG with other natural glyceryl glycosides, such as α-D-mannosyl-D-glycerate, α-D-glucosyl-D-glycerate and α-D-glucosyl-(1 → 6)-α-D-glucosyl-(1 → 2)-D-glycerate.

  20. Glyceryl Trinitrate Inhibits Hypoxia/Reoxygenation-Induced Apoptosis in the Syncytiotrophoblast of the Human Placenta

    PubMed Central

    Belkacemi, Louiza; Bainbridge, Shannon A.; Dickinson, Michelle A.; Smith, Graeme N.; Graham, Charles H.

    2007-01-01

    Damage of the placenta resulting from ischemia-reperfusion is important to the pathophysiology of preeclampsia. Here we investigated whether low concentrations of glyceryl trinitrate (GTN), a nitric oxide mimetic with anti-apoptotic properties, inhibit hypoxia/reoxygenation-induced apoptosis in the syncytiotrophoblast of chorionic villous explants from human placentas. Compared with villi analyzed immediately after delivery or maintained under normoxic conditions, villi exposed to a 6-hour cycle of hypoxia/reoxygenation exhibited greater numbers of syncytiotrophoblasts with terminal dUTP nick-end labeling (TUNEL)-positive nuclei in the syncytiotrophoblast. This increased number of TUNEL-positive nuclei was paralleled by higher levels of 4-hydroxynonenal (marker of lipid peroxidation), nitrotyrosine residues, and active caspase-3 and polyADP-ribose polymerase expression. Morphological analysis of explants exposed to hypoxia/reoxygenation revealed apoptotic and aponecrotic features similar to those of chorionic villi from preeclamptic pregnancies. Treatment with GTN during the hy-poxia/reoxygenation cycle blocked the increases in the number of TUNEL-positive nuclei and in the levels of 4-hydroxynonenal, nitrotyrosine, and active caspase-3. Incubation with GTN also attenuated the hypoxia/reoxygenation-induced polyADP-ribose polymerase expression and the apoptotic and aponecrotic morphological alterations. These results suggest that small concentrations of nitric oxide protect chorionic villi from hypoxia/reoxygenation-induced damage and provide a rationale for the use of low doses of nitric oxide mimetics in the treatment and/or prevention of preeclampsia. PMID:17322376

  1. A novel method for the synthesis of glyceryl monocaffeate by the enzymatic transesterification and kinetic analysis.

    PubMed

    Sun, Shangde; Hu, Bingxue

    2017-01-01

    A novel enzymatic method for glyceryl monocaffeate (GMC) preparation by the transesterification of ethyl caffeate (EC) was investigated. The effects of reaction variables (reaction pressure, temperature, reaction time, enzyme load, and substrate ratio) on the enzymatic transesterification were studied and optimized using response surface methodology. HPLC-ESI-MS and HPLC-UV were used to monitor the transesterification. Thermodynamics, kinetic analyses and reaction mechanism were also evaluated. Results showed that, GMC can be successfully prepared by the enzymatic transesterification of EC with glycerol. Under the optimal conditions (enzyme load 22.54%, EC:glycerol=1:12.75 (mol/mol), 72.5°C, and 10.5h), EC conversion and GMC yield were 97.9±0.7% and 95.8±1.0%, respectively. The activation energies (Ea) for EC conversion and GMC formation were 44.23 and 46.51kJ/mol, respectively. The kinetic values for Vmax, Km(') and KIA were 2.18×10(-3)mol/(Lmin), 0.086mol/L, and 0.52mol/L, respectively. The transesterification mechanism with EC inhibition was also proposed. PMID:27507465

  2. Glyceryl trinitrate ointment did not reduce pain after stapled hemorrhoidectomy: a randomized controlled trial.

    PubMed

    Cross, Trent; Bartlett, Lynne; Mushaya, Chrispen; Ashour, Mohamed; Ho, Yik-Hong

    2012-01-01

    Medications, including topical 0.2% glyceryl trinitrate (GTN), can reduce anal spasm and pain after excisional hemorrhoidectomy. GTN after stapled hemorrhoidopexy was compared with routine postoperative management. Patients with symptomatic grade 3/4 hemorrhoids were recruited. After stapled hemorrhoidopexy, residual perianal skin tags were excised as appropriate. Those requiring double purse-string mucosectomy were excluded. Postoperative pain, pain duration, and complications were assessed. One hundred ten patients (74 men; mean age 50.6 years) were enrolled in the control group and 100 patients (57 men; mean age 49.8 years) in the GTN group. Maximum pain was higher in the GTN group (P  =  0.015). There were no differences between the two groups in residual perianal skin tags requiring excision, postoperative complications, recurrence rates, follow-up period, average pain, duration of pain, or satisfaction scores. Sixteen GTN patients were noncompliant due to side effects. None had persistent perianal skin tags. GTN did not reduce postoperative pain after stapled hemorrhoidectomy.

  3. Glyceryl Trinitrate Ointment Did Not Reduce Pain After Stapled Hemorrhoidectomy: A Randomized Controlled Trial

    PubMed Central

    Cross, Trent; Bartlett, Lynne; Mushaya, Chrispen; Ashour, Mohamed; Ho, Yik-Hong

    2012-01-01

    Medications, including topical 0.2% glyceryl trinitrate (GTN), can reduce anal spasm and pain after excisional hemorrhoidectomy. GTN after stapled hemorrhoidopexy was compared with routine postoperative management. Patients with symptomatic grade 3/4 hemorrhoids were recruited. After stapled hemorrhoidopexy, residual perianal skin tags were excised as appropriate. Those requiring double purse-string mucosectomy were excluded. Postoperative pain, pain duration, and complications were assessed. One hundred ten patients (74 men; mean age 50.6 years) were enrolled in the control group and 100 patients (57 men; mean age 49.8 years) in the GTN group. Maximum pain was higher in the GTN group (P  =  0.015). There were no differences between the two groups in residual perianal skin tags requiring excision, postoperative complications, recurrence rates, follow-up period, average pain, duration of pain, or satisfaction scores. Sixteen GTN patients were noncompliant due to side effects. None had persistent perianal skin tags. GTN did not reduce postoperative pain after stapled hemorrhoidectomy. PMID:23102076

  4. Modulation of drug release from glyceryl palmitostearate-alginate beads via heat treatment.

    PubMed

    Pongjanyakul, Thaned; Sungthongjeen, Srisagul; Puttipipatkhachorn, Satit

    2006-08-17

    Diclofenac calcium alginate (DCA) beads containing glyceryl palmitostearate (GPS) were prepared by ionotropic gelation method. The effect of GPS amount and heat treatment on characteristics of the DCA beads was investigated. Incorporation of GPS into the DCA beads increased particle size and entrapment efficiency of diclofenac sodium (DS), but decreased water uptake in distilled water, and DS release rate. The heat treatment caused the DCA beads to be irregular shape particles and to possess higher water uptake. A slower release rate of DS in distilled water was found because of interaction of DS and alginate polymer matrix, and a restriction of water sorption into the inside region of the beads, which caused by the shrinkage of the beads after heating. However, the heat treatment did not affect particle shape and water uptake in distilled water of the 3%GPS-DCA beads. Differential scanning calorimetric study showed that GPS in the DCA beads was resolidified to different polymorph after cooling. Furthermore, the micro-Raman spectra indicated the existence of DS in the GPS matrix particles in the beads due to the partition of DS into the melted GPS during heat treatment. This led to a decrease in release rate of DS in pH 6.8 phosphate buffer and a change in DS release pattern in distilled water. Thus, not only the calcium alginate matrix, but also the resolidified GPS matrix in the alginate beads controlled the DS release from the 3%GPS-DCA beads with heat treatment.

  5. Development and evaluation of liquid embolic agents based on liquid crystalline material of glyceryl monooleate.

    PubMed

    Du, Ling-Ran; Lu, Xiao-Jing; Guan, Hai-Tao; Yang, Yong-Jie; Gu, Meng-Jie; Zheng, Zhuo-Zhao; Lv, Tian-Shi; Yan, Zi-Guang; Song, Li; Zou, Ying-Hua; Fu, Nai-Qi; Qi, Xian-Rong; Fan, Tian-Yuan

    2014-08-25

    New type of liquid embolic agents based on a liquid crystalline material of glyceryl monooleate (GMO) was developed and evaluated in this study. Ternary phase diagram of GMO, water and ethanol was constructed and three isotropic liquids (ILs, GMO:ethanol:water=49:21:30, 60:20:20 and 72:18:10 (w/w/w)) were selected as potential liquid embolic agents, which could spontaneously form viscous gel cast when contacting with water or physiological fluid. The ILs exhibited excellent microcatheter deliverability due to low viscosity, and were proved to successfully block the saline flow when performed in a device to simulate embolization in vitro. The ILs also showed good cytocompatibility on L929 mouse fibroblast cell line. The embolization of ILs to rabbit kidneys was performed successfully under monitoring of digital subtraction angiography (DSA), and embolic degree was affected by the initial formulation composition and used volume. At 5th week after embolization, DSA and computed tomography (CT) confirmed the renal arteries embolized with IL did not recanalize in follow-up period, and an obvious atrophy of the embolized kidney was observed. Therefore, the GMO-based liquid embolic agents showed feasible and effective to embolize, and potential use in clinical interventional embolization therapy. PMID:24858389

  6. Glyceryl monooleate-based otic delivery system of ofloxacin: release profile and bactericidal activity.

    PubMed

    Adwan, Samer; Abu-Dahab, Rana; Al-Bakri, Amal G; Sallam, Alsayyed

    2015-05-01

    This study investigated the preparation and characterization of glyceryl monooleate- (GMO) based drug delivery system containing ofloxacin for the treatment of otitis externa. Acetate buffer (pH 4.5) containing dissolved ofloxacin was added to molten GMO as an aqueous phase, this resulted in the formation of a cubic and a reverse hexagonal phases. The release behavior of ofloxacin from the drug delivery system was studied using three different methods. The mechanism of drug release using paddles/dissolution apparatus and Franz diffusion cells followed Higuchi and Fickian diffusion models; whereas intrinsic release rate method showed zero-order kinetics. The intrinsic release rate was estimated and found to be 187.2 µg/cm(2)/h. The release mechanisms were similar irrespective of the loaded ofloxacin amount, however, the higher drug load displayed higher release rate. The drug delivery system was proven to be microbiologically effective by using agar diffusion method, against Staphylococcus aureus, and Pseudomonas aeruginosa. The GMO/ofloxacin formulation was stable for 6 months after preparation at room temperature as measured with respect to phase stability and antibacterial activity.

  7. Steady-state maternal and fetal plasma concentrations of glyceryl trinitrate (GTN) in the preterm sheep.

    PubMed

    Bustard, Mark A; Farley, Anne E; Bennett, Brian M; Smith, Graeme N

    2003-09-01

    The administration of glyceryl trinitrate (GTN; nitroglycerin) is increasing during preterm pregnancies, yet its disposition and, importantly, the extent of fetal exposure remain to be elucidated. When used as a tocolytic (pharmacological agent that stops uterine contractions), it is administered transdermally (24-48 h). Here, we quantified the maternal and fetal steady-state plasma concentrations of maternal intravenous GTN in preterm sheep and continuously monitored maternal and fetal vascular parameters to observe possible dose-dependent vascular effects. Preterm (120 days gestation) pregnant sheep (n = 6) were instrumented with maternal femoral arterial (MA) and venous (MV) and fetal femoral arterial (FA) and umbilical venous (UV) polyethylene blood-sampling catheters. During maternal GTN infusion (3.0 micro g.kg-1.min-1, 60-min duration) the steady-state GTN concentrations ([GTN]) were as follows: MA, 98.6 +/- 9.0 nM; UV, 17.4 +/- 7.6 nM; and FA, <5 nM. There were no changes in maternal and fetal mean arterial pressure and heart rate or in uterine activity. Overall, the steady-state [GTN] was established by 5 min, and the UV/MA ratio of [GTN] was 0.18. The FA [GTN] (<5 nM) indicates that the fetus cleared essentially all GTN in the UV, and the maternal and fetal heart rate and mean arterial pressure appear to be independent of maternal GTN infusion. PMID:14614525

  8. RNA Sequencing of Trigeminal Ganglia in Rattus Norvegicus after Glyceryl Trinitrate Infusion with Relevance to Migraine

    PubMed Central

    Hougaard Pedersen, Sara; Maretty, Lasse; Ramachandran, Roshni; Sibbesen, Jonas Andreas; Yakimov, Victor; Elgaard-Christensen, Rikke; Hansen, Thomas Folkmann; Krogh, Anders; Olesen, Jes; Jansen-Olesen, Inger

    2016-01-01

    Introduction Infusion of glyceryl trinitrate (GTN), a donor of nitric oxide, induces immediate headache in humans that in migraineurs is followed by a delayed migraine attack. In order to achieve increased knowledge of mechanisms activated during GTN-infusion this present study aims to investigate transcriptional responses to GTN-infusion in the rat trigeminal ganglia. Methods Rats were infused with GTN or vehicle and trigeminal ganglia were isolated either 30 or 90 minutes post infusion. RNA sequencing was used to investigate transcriptomic changes in response to the treatment. Furthermore, we developed a novel method for Gene Set Analysis Of Variance (GSANOVA) to identify gene sets associated with transcriptional changes across time. Results 15 genes displayed significant changes in transcription levels in response to GTN-infusion. Ten of these genes showed either sustained up- or down-regulation in the 90-minute period after infusion. The GSANOVA analysis demonstrate enrichment of pathways pointing towards an increase in immune response, signal transduction, and neuroplasticity in response to GTN-infusion. Future functional in-depth studies of these mechanisms are expected to increase our understanding of migraine pathogenesis. PMID:27213950

  9. Steady-state maternal and fetal plasma concentrations of glyceryl trinitrate (GTN) in the preterm sheep.

    PubMed

    Bustard, Mark A; Farley, Anne E; Bennett, Brian M; Smith, Graeme N

    2003-09-01

    The administration of glyceryl trinitrate (GTN; nitroglycerin) is increasing during preterm pregnancies, yet its disposition and, importantly, the extent of fetal exposure remain to be elucidated. When used as a tocolytic (pharmacological agent that stops uterine contractions), it is administered transdermally (24-48 h). Here, we quantified the maternal and fetal steady-state plasma concentrations of maternal intravenous GTN in preterm sheep and continuously monitored maternal and fetal vascular parameters to observe possible dose-dependent vascular effects. Preterm (120 days gestation) pregnant sheep (n = 6) were instrumented with maternal femoral arterial (MA) and venous (MV) and fetal femoral arterial (FA) and umbilical venous (UV) polyethylene blood-sampling catheters. During maternal GTN infusion (3.0 micro g.kg-1.min-1, 60-min duration) the steady-state GTN concentrations ([GTN]) were as follows: MA, 98.6 +/- 9.0 nM; UV, 17.4 +/- 7.6 nM; and FA, <5 nM. There were no changes in maternal and fetal mean arterial pressure and heart rate or in uterine activity. Overall, the steady-state [GTN] was established by 5 min, and the UV/MA ratio of [GTN] was 0.18. The FA [GTN] (<5 nM) indicates that the fetus cleared essentially all GTN in the UV, and the maternal and fetal heart rate and mean arterial pressure appear to be independent of maternal GTN infusion.

  10. Formation of "solvent-free" black lipid bilayer membranes from glyceryl monooleate dispersed in squalene.

    PubMed

    White, S H

    1978-09-01

    A simple technique for forming "black" lipid bilayer membranes containing negligible amounts of alkyl solvent is described. The membranes are formed by the method of Mueller et al (Circulation. 1962. 26:1167.) from glyceryl monooleate (GMO) dispersed in squalene. The squalene forms an annulus to satisfy the boundary conditions of the planar bilayer but does not appear to dissolve noticeably in the bilayer itself. The specific geometric capacitance (Cg) of the membranes at 20 degrees C formed by this technique is 0.7771 +/- 0.0048 muF/cm2. Theoretical estimates of Cg for solvent-free bilayers range from 0.75 to 0.81 muF/cm2. Alkane-free GMO bilayers formed from n-octadecane by the solvent freeze-out method of White (Biochim. Biophys. Acta. 1974. 356:8) have values of Cg = 0.7903 +/- 0.0013 muF/cm2 at 20.5 degrees C. The agreement between the various values of Cg strongly suggests that the bilayers are free of squalene. DC potentials applied to the bilayers have no detectable effect on the value of Cg, as expected for solvent-free films. The ability to form bilayers essentially free of the solvent used in the forming solution makes it possible to determine the area per molecule of the surface active lipid in the bilayer. The area per molecule of GMO at 20 degrees C is estimated to be 37.9 +/- 0.2 A2.

  11. Kinetic characterization of swelling of liquid crystalline phases of glyceryl monooleate.

    PubMed

    Lee, Jaehwi; Choi, Sung-Up; Yoon, Mi-Kyeong; Choi, Young Wook

    2003-10-01

    Research in this paper focuses on the kinetic evaluation of swelling of the liquid crystalline phases of glyceryl monooleate (GMO). Swelling of the lamellar and cubic liquid crystalline phases of GMO was studied using two in vitro methods, a total immersion method and a Franz cell method. The swelling of the lamellar phase and GMO having 0 %w/w initial water content was temperature dependent. The swelling ratio was greater at 20 degrees C than 37 degrees C. The water uptake increased dramatically with decreasing initial water content of the liquid crystalline phases. The swelling rates obtained using the Franz cell method with a moist nylon membrane to mimic buccal drug delivery situation were slower than the total immersion method. The swelling was studied by employing first-order and second-order swelling kinetics. The swelling of the liquid crystalline phases of GMO could be described by second-order swelling kinetics. The initial stage of the swelling (t < 4 h) followed the square root of time relationship, indicating that this model is also suitable for describing the water uptake by the liquid crystalline matrices. These results obtained from the current study demonstrate that the swelling strongly depends on temperature, the initial water content of the liquid crystalline phases and the methodology employed for measuring the swelling of GMO.

  12. Cubic liquid crystalline glyceryl monooleate matrices for oral delivery of enzyme.

    PubMed

    Shah, Manish H; Paradkar, Anant

    2005-04-27

    In situ cubic phase transforming system of glyceryl monooleate (GMO) has been prepared which offers protection to the metaloenzyme, seratiopeptidase (STP), in gastric environment and provides delayed and controlled release with no initial burst after oral administration. Effect of magnesium trisilicate (MTS) on floating, proteolytic activity and drug release was studied. Gelucire 43/01 was incorporated in the system to provide prolonged lag time. The drug-loaded matrices required 100 mg of MTS to overcome floatability of GMO matrix. Plain GMO matrices showed 85.3% loss of proteolytic activity in acidic medium, whereas matrices containing MTS showed retention of activity (111.6%). The hydrophobic nature of MTS induced formation of cubic phase at faster rate and the existence of cubic phase was confirmed by polarizing light microscopy. Furthermore, MTS provided alkaline microenvironment, which prevented acid-catalyzed hydrolysis and protein unfolding. The magnesium ions restored the activity of STP. The release of STP was decreased with increasing amount of MTS in the matrix. Gelucire did not affect proteolytic activity. The water uptake of matrices with gelucire was decelerated due to formation of hexagonal phase. However, the rate of STP release from these matrices was very slow due to incorporation of gelucire into lipid bilayers, which provided resistance to movement of STP. Thus, microenvironment-controlled in situ cubic phase transforming GMO matrices provided protection to STP and controlled release.

  13. Preparation of multiparticulate vaginal tablet using glyceryl monooleate for sustained progesterone delivery.

    PubMed

    Biradar, Shailesh V; Dhumal, Ravindra S; Shah, Manish H; Paradkar, Anant R; Yamamura, Shigeo

    2009-01-01

    Most of the sustained release vaginal formulations are in the form of bioadhesive gels and tablets. Though proved efficient, their presence in the vagina for a longer time as a bulk produces discomfort and interference with body functioning including sexual activities. Hence, they lack complete patient compliance. In this study, multiparticulate vaginal tablets were prepared by utilizing progesterone (PRO) loaded dry powder precursor of cubic phase (DPPCP) of glyceryl monooleate (GMO). DPPCP were obtained by spray drying GMO with magnesium trisilicate (MTS) and have presented PRO sustained release in simulated vaginal fluid (SVF) for 14 hours. The effect of hydrophilic and hydrophobic tableting excipients on compression, phase, bioadhesion and drug release properties of prepared tablets was evaluated. The effervescent hydrophilic tablet (EHT) prepared with hydrophilic excipients showed rapid disintegration but, diminished sustaining ability owing to transformation into lamellar phase whereas the multiparticulate hydrophobic tablet (MHT) obtained from hydrophobic excipients presented both rapid disintegration and sustained release in SVF by virtue of cubic phase retention. During bioadhesivity testing, fast disintegration of MHT with formation of uniform and viscous bioadhesive layer on cow mucosa was observed even with a small volume of SVF. As MHT may not produce discomfort and interference, it will be preferred over bioadhesive gel or tablet.

  14. Computational and Biological Evaluation of N-octadecyl-N′-propylsulfamide, a Selective PPARα Agonist Structurally Related to N-acylethanolamines

    PubMed Central

    Serrano, Antonia; Cano, Carolina; Suardíaz, Margarita; Decara, Juan; Suarez, Juan; de Fonseca, Fernando Rodríguez; Macías-González, Manuel

    2014-01-01

    To further understand the pharmacological properties of N-oleoylethanolamine (OEA), a naturally occurring lipid that activates peroxisome proliferator-activated receptor alpha (PPARα), we designed sulfamoyl analogs based on its structure. Among the compounds tested, N-octadecyl-N′-propylsulfamide (CC7) was selected for functional comparison with OEA. The performed studies include the following computational and biological approaches: 1) molecular docking analyses; 2) molecular biology studies with PPARα; 3) pharmacological studies on feeding behavior and visceral analgesia. For the docking studies, we compared OEA and CC7 data with crystallization data obtained with the reference PPARα agonist GW409544. OEA and CC7 interacted with the ligand-binding domain of PPARα in a similar manner to GW409544. Both compounds produced similar transcriptional activation by in vitro assays, including the GST pull-down assay and reporter gene analysis. In addition, CC7 and OEA induced the mRNA expression of CPT1a in HpeG2 cells through PPARα and the induction was avoided with PPARα-specific siRNA. In vivo studies in rats showed that OEA and CC7 had anorectic and antiobesity activity and induced both lipopenia and decreases in hepatic fat content. However, different effects were observed when measuring visceral pain; OEA produced visceral analgesia whereas CC7 showed no effects. These results suggest that OEA activity on the PPARα receptor (e.g., lipid metabolism and feeding behavior) may be dissociated from other actions at alternative targets (e.g., pain) because other non cannabimimetic ligands that interact with PPARα, such as CC7, do not reproduce the full spectrum of the pharmacological activity of OEA. These results provide new opportunities for the development of specific PPARα-activating drugs focused on sulfamide derivatives with a long alkyl chain for the treatment of metabolic dysfunction. PMID:24651609

  15. Computational and biological evaluation of N-octadecyl-N'-propylsulfamide, a selective PPARα agonist structurally related to N-acylethanolamines.

    PubMed

    Moreno-Santos, Inmaculada; Pavón, Francisco Javier; Romero-Cuevas, Miguel; Serrano, Antonia; Cano, Carolina; Suardíaz, Margarita; Decara, Juan; Suarez, Juan; de Fonseca, Fernando Rodríguez; Macías-González, Manuel

    2014-01-01

    To further understand the pharmacological properties of N-oleoylethanolamine (OEA), a naturally occurring lipid that activates peroxisome proliferator-activated receptor alpha (PPARα), we designed sulfamoyl analogs based on its structure. Among the compounds tested, N-octadecyl-N'-propylsulfamide (CC7) was selected for functional comparison with OEA. The performed studies include the following computational and biological approaches: 1) molecular docking analyses; 2) molecular biology studies with PPARα; 3) pharmacological studies on feeding behavior and visceral analgesia. For the docking studies, we compared OEA and CC7 data with crystallization data obtained with the reference PPARα agonist GW409544. OEA and CC7 interacted with the ligand-binding domain of PPARα in a similar manner to GW409544. Both compounds produced similar transcriptional activation by in vitro assays, including the GST pull-down assay and reporter gene analysis. In addition, CC7 and OEA induced the mRNA expression of CPT1a in HpeG2 cells through PPARα and the induction was avoided with PPARα-specific siRNA. In vivo studies in rats showed that OEA and CC7 had anorectic and antiobesity activity and induced both lipopenia and decreases in hepatic fat content. However, different effects were observed when measuring visceral pain; OEA produced visceral analgesia whereas CC7 showed no effects. These results suggest that OEA activity on the PPARα receptor (e.g., lipid metabolism and feeding behavior) may be dissociated from other actions at alternative targets (e.g., pain) because other non cannabimimetic ligands that interact with PPARα, such as CC7, do not reproduce the full spectrum of the pharmacological activity of OEA. These results provide new opportunities for the development of specific PPARα-activating drugs focused on sulfamide derivatives with a long alkyl chain for the treatment of metabolic dysfunction.

  16. Quantification of glyceryl trinitrate effect through analysis of the synthesised ascending aortic pressure waveform

    PubMed Central

    Jiang, X J; O'Rourke, M F; Jin, W Q L; Liu, L S; Li, C W; Tai, P C; Zhang, X C; Liu, S Z

    2002-01-01

    Objective: To establish through analysis of the radial pressure pulse waveform the dose dependent effects of glyceryl trinitrate (GTN) on properties of different blood vessels. Design: Radial pulse waveform was measured in randomised order before, during a five hour application of a GTN patch delivering 0.104–0.625 mg/h, and for two hours after patch removal. The radial pressure waveform (Millar applanation tonometer) was convolved into an ascending aortic wave using a generalised transfer function (SphygmoCor process) enabling measurement of aortic systolic, diastolic, pulse, mean, and augmented pressure and left ventricular ejection duration in addition to standard brachial cuff pressures. Setting: Fu Wai and Ren Ming hospitals in Beijing, China. Patients: 46 recumbent hospitalised patients aged 56 (9) years, awaiting electrophysiological or other diagnostic studies, fasting, and with other treatments suspended. Major outcome measures: Conventional brachial pressure measures and data from the synthesised aortic pulse. Results: There was no consistent change in heart rate or brachial pressures except for a decrease in systolic and pulse pressures (p < 0.01) at dose > 0.416 mg/h. In contrast, there were substantial and significant (p < 0.0001) decreases in aortic systolic, pulse, and augmented pressures at all doses, mean pressure (p < 0.001) at doses > 0.416 mg/h, and ejection duration (p < 0.001) at doses > 0.208 mg/h. Conclusions: Pulse waveform analysis exposes dose dependent effects of GTN on the aortic waveform, suggesting muscular conduit arterial dilatation with reduced wave reflection at the lowest dose, arteriolar dilatation and decreased peripheral resistance at the highest dose, and venous dilatation at the intermediate dose. PMID:12117838

  17. Cubic, sponge, and lamellar phases in the glyceryl monooleyl ether-propylene glycol-water system.

    PubMed

    Engström, Sven; Wadsten-Hindrichsen, Pia; Hernius, Bettina

    2007-09-25

    The phase behavior of 1-glyceryl monooleyl ether (GME) in mixtures of propylene glycol (PG) and water was investigated by visual inspection, polarization microscopy, small-angle X-ray diffraction, and conductance measurements. A phase diagram, based on over 200 samples of the ternary system GME-PG-water, was constructed at 20 degrees C. Without PG, GME forms a reverse micellar phase with up to 10 wt % water and a reverse hexagonal liquid-crystalline phase between 10 and 25 wt % water, a phase that can coexist with excess water. If PG is added in amounts exceeding about 10 wt %, then cubic and lamellar liquid-crystalline phases start to form. A cubic phase, belonging to space group Pn3m, can coexist with excess PG-water mixtures. If even more PG is added, then the cubic phase is transformed into a sponge phase. A lamellar phase forms at water contents between 10 and 15 wt % and with widely differing PG/GME weight ratios. We postulate that the phase behavior is caused by the fact that PG makes the interfacial region between self-assembled GME and PG-water less negatively curved, which in turn allows for the formation of the new phases. The phase behavior obtained for the GME system shows a striking similarity with the phase behavior of the corresponding system in which the GME has been replaced by the ester, 1-glycerol monooleate (GMO), differing only in one extra carbonyl oxygen. The major difference is the lower amount of water present in the GME phases, an effect that is mainly due to the more hydrophobic character of GME compared to that of GMO.

  18. Chitosan and glyceryl monooleate nanostructures containing gemcitabine: potential delivery system for pancreatic cancer treatment.

    PubMed

    Trickler, William J; Khurana, Jatin; Nagvekar, Ankita A; Dash, Alekha K

    2010-03-01

    The objectives of this study are to enhance cellular accumulation of gemcitabine with chitosan/glyceryl monooleate (GMO) nanostructures, and to provide significant increase in cell death of human pancreatic cancer cells in vitro. The delivery system was prepared by a multiple emulsion solvent evaporation method. The nanostructure topography, size, and surface charge were determined by atomic force microscopy (AFM), and a zetameter. The cellular accumulation, cellular internalization and cytotoxicity of the nanostructures were evaluated by HPLC, confocal microscopy, or MTT assay in Mia PaCa-2 and BxPC-3 cells. The average particle diameter for 2% and 4% (w/w) drug loaded delivery system were 382.3 +/- 28.6 nm, and 385.2 +/- 16.1 nm, respectively with a surface charge of +21.94 +/- 4.37 and +21.23 +/- 1.46 mV. The MTT cytotoxicity dose-response studies revealed the placebo at/or below 1 mg/ml has no effect on MIA PaCa-2 or BxPC-3 cells. The delivery system demonstrated a significant decrease in the IC50 (3 to 4 log unit shift) in cell survival for gemcitabine nanostructures at 72 and 96 h post-treatment when compared with a solution of gemcitabine alone. The nanostructure reported here can be resuspended in an aqueous medium that demonstrate increased effective treatment compared with gemcitabine treatment alone in an in vitro model of human pancreatic cancer. The drug delivery system demonstrates capability to entrap both hydrophilic and hydrophobic compounds to potentially provide an effective treatment option in human pancreatic cancer. PMID:20238190

  19. Spray dried glyceryl monooleate-magnesium trisilicate dry powder as cubic phase precursor.

    PubMed

    Shah, Manish H; Biradar, Shailesh V; Paradkar, Anant R

    2006-10-12

    Glyceryl monooleate (GMO) is a polar amphiphilic lipid, which forms different sequential lyotropic liquid crystals upon hydration. GMO has been utilized for various delivery systems and routes of administrations. Owing to sticky and waxy nature of GMO, preparation of oral solid dosage form utilizing GMO is still a challenge for pharmaceutical researchers. Therefore, the objective of the present work was to fabricate dry powder precursors using GMO, which upon hydration in situ forms cubic phase and can be wisely used for fabrication of oral solid dosage forms. In addition to this, dry powder precursor was evaluated for drug loading, in vitro release behavior and in vivo performance of model drug diclofenac sodium (DiNa). The dry powder precursor was obtained by spray-drying GMO with DiNa using magnesium trisilicate (MTS) as adsorbent. The percent drug entrapment of various batches of powder precursor was in the range of 84-93% indicating high content uniformity. SEM and image analysis showed that as the amount of MTS in powder precursor was increased, the particle size decreased. Furthermore, the viscosity of powder precursor was function of amount of MTS. The rate of water uptake of powder precursor was higher due to uniform layer of GMO on the MTS surface, which led to faster transformation of lamellar phase into cubic phase. The polarizing light microscopy confirmed that cubic phase was formed upon hydration of powder precursor. The drug released from powder precursor was initially governed by the cubic phase formed and in later stage it depends upon dynamic swelling behavior of hexagonally packed cylindrical aggregates. The drug loaded powder precursor was found to have more effective and prolonged anti-inflammatory and analgesic activity as compared to pure drug. Thus the dry powder precursor of cubic phase was prepared in which drug release was entirely governed by the mesophases formed.

  20. Acute and chronic effects of glyceryl trinitrate therapy on insulin and glucose regulation in humans.

    PubMed

    Jedrzkiewicz, Sean; Parker, John D

    2013-05-01

    This study examined the effect of acute and sustained transdermal glyceryl trinitrate (GTN) therapy on insulin and glucose regulation. Totally, 12 males (18-30 years) underwent a glucose tolerance test at baseline (visit 1), 90 minutes after acute transdermal GTN 0.6 mg/h (visit 2), following 7 days of continuous GTN (visit 3), and 2 to 3 days after stopping GTN (visit 4). At each visit, plasma glucose and insulin concentrations were measured before and 30, 60, 90, and 120 minutes after a 75-g oral glucose load. Indices of glucose metabolism that were examined included the insulin sensitivity index, the homeostasis model assessment of insulin resistance (HOMA-IR), and the insulinogenic index. The acute administration of GTN had no effect on glucose and insulin responses (visit 2). However, after 7 days of GTN exposure (visit 3) there was an increase in the mean glucose concentration measured after the oral glucose load. On visit 1, the mean glucose concentration (± standard deviation) following the 75 g oral glucose challenge was 5.7 ± 0.5 µmol/L. On visit 3, after 7 days of transdermal GTN therapy, the mean glucose concentration after the oral glucose was significantly higher; 6.2 ± 0.5 µmol/L (P < .015; 95% confidence intervals 0.25-0.77). There was also an increase in the HOMA-IR index; on visit 1, the median HOMA-IR (interquartile range) was 5.2 (3.9) versus 6.9 (6.8) on visit 3 (P < .015). Other indices of glucose metabolism did not change. These observations document that GTN therapy modifies glucose metabolism causing evidence of increased insulin resistance during sustained therapy in normal humans.

  1. Analysis of responses to glyceryl trinitrate and sodium nitrite in the intact chest rat.

    PubMed

    Nossaman, Bobby D; Pankey, Edward A; Badejo, Adeleke R; Casey, David B; Uppu, Satvika; Murthy, Subramanyam N; Kadowitz, Philip J

    2012-05-15

    Responses to glyceryl trinitrate/nitroglycerin (GTN), S-nitrosoglutathione (GSNO), and sodium nitrite were compared in the intact chest rat. The iv injections of GTN, sodium nitrite, and GSNO produced dose-dependent decreases in pulmonary and systemic arterial pressures. In as much as cardiac output was not reduced, the decreases in pulmonary and systemic arterial pressures indicate that GTN, sodium nitrite, and GSNO have significant vasodilator activity in the pulmonary and systemic vascular beds in the rat. Responses to GTN were attenuated by cyanamide, but not allopurinol, whereas responses to nitrite formed by the metabolism of GTN were attenuated by allopurinol and cyanamide. The results with allopurinol and cyanamide suggest that only mitochondrial aldehyde dehydrogenase is involved in the bioactivation of GTN, sodium nitrite, and GSNO, whereas both pathways are involved in the bioactivation of nitrite anion in the intact rat. The comparison of vasodilator activity indicates that GSNO and GTN are more than 1000-fold more potent than sodium nitrite in decreasing pulmonary and systemic arterial pressures in the rat. Following administration of 1H-[1,2,4]-oxadizaolo[4,3-]quinoxaline-1-one (ODQ), responses to GTN were significantly attenuated, indicating that responses are mediated by the activation of soluble guanylyl cyclase. These data suggest that the reduction of nitrite to nitric oxide formed from the metabolism of GTN, cannot account for the vasodilator activity of GTN in the intact rat and that another mechanism; perhaps the formation of an S-NO, may mediate the vasodilator response to GTN in this species.

  2. Glyceryl monooleate-coated bioadhesive hollow microspheres of riboflavin for improved gastroretentivity: optimization and pharmacokinetics.

    PubMed

    Upadhyay, Mayank Shekhar; Pathak, Kamla

    2013-06-01

    The bioadhesive hollow microspheres of riboflavin were developed as a site-specific gastroretentive system to prolong the residence time of drug in the stomach and, consequently, to enhance the bioavailability. Hollow microspheres (M1-M9) prepared by the emulsion solvent diffusion method using ethyl cellulose and Eudragit E100 as shell-forming polymers were designed using 3(2) full factorial design. The optimized formulation (M5) with 93.23 ± 0.6 % entrapment efficiency and 75.39 ± 3.4 % cumulative drug release at 8 h was subjected to coating with a bioadhesive layer of glyceryl monooleate (GMO) to obtain BM5. It exhibited excellent in vitro buoyancy for 12 h (100 %), in vitro bioadhesion (88.33 ± 2.35 %), and presented micromeritic properties amenable to processing steps. Scanning electron microscopy depicted a spherical shape and hollow cavity of microspheres and evidenced smooth surface coating of GMO. The compatibility of drug and excipients and the absence of interaction were determined using differential scanning calorimetry and diffuse reflectance spectroscopy, respectively. The in vitro release from BM5 (novel release apparatus) demonstrated that drug release was not hindered by the bioadhesive coating layer of GMO. The pharmacokinetic study provided convincing evidence for the increased absorption of riboflavin and bioavailability (Fr = 178.47 %) from bioadhesive hollow microspheres. Conclusively, the study demonstrated the superiority of the synergistic approach of floating and bioadhesive system over either floating or bioadhesive system for the prolongation of gastric residence time of riboflavin to improve its absorption.

  3. Effect of HLB of additives on the properties and drug release from the glyceryl monooleate matrices.

    PubMed

    Shah, Manish H; Paradkar, Anant

    2007-08-01

    Glyceryl monooleate (GMO) is an amphiphilic surfactant, which as such can solubilize hydrophilic, lipophilic and amphiphilic drug molecules in its different polarity regions. Addition of additives with different polarities in GMO leads to change in phase behavior and related properties of GMO. Effect of the additives with different hydrophilic lipophilic balance (HLB; 1.5, 3, 4, 5, 7, 10 and 11) in GMO matrices on its phase transformation, rheological properties, mechanical properties, wetting and release behavior was investigated. Polarizing light microscopy showed that the GMO matrices incorporated with lower HLB additive (1.5, 3, 4 and 5) form cubic phase at higher rate while lamellar phase was prominent for matrices with additive of HLB 7, 10 and 11. The diametrical crushing strength and viscosity was decreased with increased HLB of additive. Lower HLB additives enhanced contact angle as compared to plain matrices and high HLB additives induced change in solid-liquid interface from hydrophobic to hydrophilic leading to decline in contact angle. Percent swelling of matrices was increased linearly with increase in HLB of additives. Tensiometric method was used for determination of bioadhesive strength of hydrated matrices and it was observed that matrices with additives of HLB 10 presented highest bioadhesion due to higher rate of hydration and formation of lamellar phase. As the HLB of additives in matrix increased, release was shifted from anomalous (non-Fickian) diffusion and/or partially erosion-controlled release to Fickian diffusion. Initial lag was observed for drug released from matrices with additive of HLB 1.5, 3, 4 and 5. Thus incorporation of the additives of different HLB changed molecular packing, which significantly affected drug release pattern.

  4. Glyceryl monooleate cubic phase gel as chemical stability enhancer of cefazolin and cefuroxime.

    PubMed

    Sadhale, Y; Shah, J C

    1998-11-01

    The primary objective of this study was to determine the ability of the glyceryl monooleate (GMO) cubic phase gel to protect drugs from chemical instability reactions such as hydrolysis and oxidation. Stability was assessed on cefazolin incorporated in cubic phase gel and in solution at two different concentrations (200 and 50 micrograms/g), at 22, 37, and 50 degrees C. Degradation profiles, plotting percent cefazolin remaining on a logarithmic scale versus time, were constructed and the degradation rate constants calculated from the slopes. At both concentrations, degradation of cefazolin was found to be slower in the cubic phase gel than in solution at 22 and 37 degrees C, but not at 50 degrees C. The degradation rate constants were 3- to 18-fold lower in the gel than in solution at low concentration of cefazolin. At 22 and 37 degrees C, the kinetics of degradation at high concentration of cefazolin was not first-order but showed a lag phase followed by an exponential loss of cefazolin, typical of oxidation. The potential oxidation of the thioether moiety of cefazolin was confirmed by its 18-fold higher stability in the presence of ethylenediaminetetraacetic acid (EDTA) and nitrogen in solution. Cefuroxime, a cephalosporin which degrades solely via beta-lactam hydrolysis, degraded twice as fast in solution as it did in the gel. The enhanced stability of cefazolin and cefuroxime in the GMO cubic phase gel shows its potential as a chemical stability enhancer and this is the first report to demonstrate oxidation, in addition to beta-lactam hydrolysis, as a mechanism for degradation of cefazolin.

  5. Chitosan and glyceryl monooleate nanostructures containing gemcitabine: potential delivery system for pancreatic cancer treatment.

    PubMed

    Trickler, William J; Khurana, Jatin; Nagvekar, Ankita A; Dash, Alekha K

    2010-03-01

    The objectives of this study are to enhance cellular accumulation of gemcitabine with chitosan/glyceryl monooleate (GMO) nanostructures, and to provide significant increase in cell death of human pancreatic cancer cells in vitro. The delivery system was prepared by a multiple emulsion solvent evaporation method. The nanostructure topography, size, and surface charge were determined by atomic force microscopy (AFM), and a zetameter. The cellular accumulation, cellular internalization and cytotoxicity of the nanostructures were evaluated by HPLC, confocal microscopy, or MTT assay in Mia PaCa-2 and BxPC-3 cells. The average particle diameter for 2% and 4% (w/w) drug loaded delivery system were 382.3 +/- 28.6 nm, and 385.2 +/- 16.1 nm, respectively with a surface charge of +21.94 +/- 4.37 and +21.23 +/- 1.46 mV. The MTT cytotoxicity dose-response studies revealed the placebo at/or below 1 mg/ml has no effect on MIA PaCa-2 or BxPC-3 cells. The delivery system demonstrated a significant decrease in the IC50 (3 to 4 log unit shift) in cell survival for gemcitabine nanostructures at 72 and 96 h post-treatment when compared with a solution of gemcitabine alone. The nanostructure reported here can be resuspended in an aqueous medium that demonstrate increased effective treatment compared with gemcitabine treatment alone in an in vitro model of human pancreatic cancer. The drug delivery system demonstrates capability to entrap both hydrophilic and hydrophobic compounds to potentially provide an effective treatment option in human pancreatic cancer.

  6. Mitochondrial aldehyde dehydrogenase mediates vasodilator responses of glyceryl trinitrate and sodium nitrite in the pulmonary vascular bed of the rat.

    PubMed

    Badejo, Adeleke M; Hodnette, Chris; Dhaliwal, Jasdeep S; Casey, David B; Pankey, Edward; Murthy, Subramanyam N; Nossaman, Bobby D; Hyman, Albert L; Kadowitz, Philip J

    2010-09-01

    It has been reported that mitochondrial aldehyde dehydrogenase (ALDH2) catalyzes the formation of glyceryl dinitrate and inorganic nitrite from glyceryl trinitrate (GTN), leading to an increase in cGMP and vasodilation in the coronary and systemic vascular beds. However, the role of nitric oxide (NO) formed from nitrite in mediating the response to GTN in the pulmonary vascular bed is uncertain. The purpose of the present study was to determine if nitrite plays a role in mediating vasodilator responses to GTN. In this study, intravenous injections of GTN and sodium nitrite decreased pulmonary and systemic arterial pressures and increased cardiac output. The decreases in pulmonary arterial pressure under baseline and elevated tone conditions and decreases in systemic arterial pressure in response to GTN and sodium nitrite were attenuated by cyanamide, an ALDH2 inhibitor, whereas responses to the NO donor, sodium nitroprusside (SNP), were not altered. The decreases in pulmonary and systemic arterial pressure in response to GTN and SNP were not altered by allopurinol, an inhibitor of xanthine oxidoreductase, whereas responses to sodium nitrite were attenuated. GTN was approximately 1,000-fold more potent than sodium nitrite in decreasing pulmonary and systemic arterial pressures. These results suggest that ALDH2 plays an important role in the bioactivation of GTN and nitrite in the pulmonary and systemic vascular beds and that the reduction of nitrite to vasoactive NO does not play an important role in mediating vasodilator responses to GTN in the intact chest rat.

  7. Octadecyl bonded silica membrane disk modified with Cyanex302 for separation and flame atomic absorption spectrometric determination of nickel from tap water and industrial effluent.

    PubMed

    Karve, Manjusha; Rajgor, Reeta V

    2009-07-15

    A simple and reliable method based upon impregnation of Cyanex302 on octadecyl bonded silica membrane disk has been developed for separation and atomic absorption spectrometric determination of nickel. The influence of various parameters like aqueous phase pH, flow rate and volume of eluent were investigated systematically to optimize the conditions for quantitative sorption and desorption of nickel. The break through volume for nickel was greater than 1.0 dm(3), enrichment factor more than 100 and a detection limit of 2.1 microg dm(-3) was achieved. The method applied for detection of nickel in tap water and effluent sample had a relative standard deviation (R.S.D.) of 0.4%.

  8. Lysosome-targeted octadecyl-rhodamine B-liposomes enhance lysosomal accumulation of glucocerebrosidase in Gaucher’s cells in vitro

    PubMed Central

    Thekkedath, Ritesh; Koshkaryev, Alexander; Torchilin, Vladimir P

    2013-01-01

    Aim We hypothesized that liposomes modified with lysosomotropic octadecyl-rhodamine B (Rh) and loaded with therapeutic glucocerebroside velaglucerase alfa (VPRIV™) will improve lysosomal delivery of the enzyme into Gaucher’s cells. Materials & methods Confocal microscopy and flow cytometry were used to evaluate the ability of Rh-modified liposomes loaded with VPRIV to improve the lysosomal targeting in monocyte-derived macrophages and Gaucher’s fibroblasts. Results Confocal microscopy demonstrated that Rh-modified liposomes localized primarily in the lysosomes. As confirmed by flow cytometry using specific substrate 5-(pentafluorobenzoylamino)fluorescein diglucoside, intralysosomal accumulation of VPRIV in the cells treated with Rh-modified liposomes was significantly increased (up to 68%) relative to the cells treated with plain liposomes or free VPRIV. Conclusion Rh-modified lysosomotropic liposomes can improve lysosomal accumulation of liposomal enzymes both in nonphagocytic Gaucher’s fibroblasts and phagocytic monocyte-derived macrophages. PMID:23199221

  9. The second harmonic generation and the photoelectric property studies on a new dye, (E)- N-octadecyl-4-[2-(4-dimethylaminophenyl) enamine] pyridinium iodide

    NASA Astrophysics Data System (ADS)

    Zhai, Jin; Huang, Chun-Hui; Wei, Tian-Xin; Yu, An-Chi; Zhao, Xin-Sheng

    1999-03-01

    According to quantum chemistry calculation, a Schiff-base (E)- N-octadecyl-4-[2-(4-dimethylaminophenyl) enamine] pyridinium iodide with a large dipole moment difference between the excited state and the ground state (Δ μ), is designed and synthesized as a second-order non-linear optical material. Its second-order susceptibility ( χ(2)zzz) is evaluated to be 279.4 pm V -1, which is larger than that of the hemicyanine which is known as one of the best dyes in the second harmonic generation (SHG) behavior. Its LB film formation properties were studied. The photoelectric conversion property is not as good as expected. According to the experiments and the results of the quantum chemistry calculation, an explanation of this phenomenon is proposed.

  10. ORAL 1-O-OCTADECYL-2-O-BENZYL-SN-GLYCERO-3-CIDOFOVIR TARGETS THE LUNG AND IS EFFECTIVE AGAINST A LETHAL RESPIRATORY CHALLENGE WITH ECTROMELIA VIRUS IN MICE

    PubMed Central

    Hostetler, Karl Y.; Beadle, James R.; Trahan, Julissa; Aldern, Kathy A.; Owens, Gelita; Schriewer, Jill; Melman, Lora; Buller, R. Mark

    2007-01-01

    Hexadecyloxypropyl-cidofovir (HDP-CDV) has been shown to be orally active against lethal infection with orthopoxviruses including, mousepox, cowpox, vaccinia and rabbitpox. The alkoxyalkyl group provides oral absorption and reduces greatly the amount of drug reaching the kidney, the site of CDV’s dose limiting toxicity. However, the amount of HDP-CDV detected in lung, an important site of early poxvirus replication, is low and the reduction of viral titers in surviving animals is reduced moderately compared with the liver where poxvirus titers are virtually undetectable. We synthesized a novel glycerol ester of CDV, 1-O-octadecyl-2-O-benzyl-sn-glycero-3-CDV (ODBG-CDV), and compared its oral pharmacokinetics with that of HDP-CDV. Surprisingly, ODBG-CDV levels in lung are much higher and liver levels are reduced, suggesting that the compound is transported in small intestinal lymph instead the portal vein. ODBG-CDV has excellent in vitro activity in cells infected with ectromelia virus (ECTV). In mice infected with a lethal aerosol or intranasal challenge of ECTV, HDP-CDV and ODBG-CDV are equally effective in preventing death from disease. Other drugs esterified to 1-O-octadecyl-2-O-benzyl-sn-glycerol or 1-O-octadecyl-2-O-benzyl-sn-glycerol-3-phosphate may provide lung targeting for treatment of microbial or neoplastic diseases while reducing first pass removal by the liver during oral absorption. PMID:17123638

  11. Liquid crystalline systems of phytantriol and glyceryl monooleate containing a hydrophilic protein: Characterisation, swelling and release kinetics.

    PubMed

    Rizwan, S B; Hanley, T; Boyd, B J; Rades, T; Hook, S

    2009-11-01

    Swelling and phase behaviour of phytantriol and glyceryl monooleate (GMO) matrices with varying water loadings were investigated. Release of a model protein, FITC-Ova was subsequently examined. Polarised light microscopy and small angle X-ray scattering analysis showed that the addition of FITC-Ova only altered the liquid crystalline structure of phytantriol matrices at low water loadings, and that postrelease study, the phase structure of matrices at both low and high loading reflected that of the binary system. Addition of FITC-Ova to GMO matrices also altered the liquid crystalline structure when compared to the respective binary system at low but not at high loading. All samples analysed after the release study had transformed to the reverse hexagonal phase (H(II)). Swelling studies revealed a faster and more extensive swelling of GMO when compared to phytantriol. Release of FITC-Ova from phytantriol matrices was faster and occurred to a greater extent most likely due to the conversion of GMO matrices into the H(II) phase. No effect on release as a function of initial water content was observed for either lipid. We have confirmed that phytantriol based liquid crystalline matrices can sustain the release of a hydrophilic protein, suggesting its suitability as a potential sustained antigen-delivery system.

  12. Glyceryl trinitrate and caprylic acid for the mitigation of the Desulfovibrio vulgaris biofilm on C1018 carbon steel.

    PubMed

    Li, Y; Zhang, P; Cai, W; Rosenblatt, J S; Raad, I I; Xu, D; Gu, T

    2016-02-01

    Microbiologically influenced corrosion (MIC), also known as biocorrosion, is caused by corrosive biofilms. MIC is a growing problem, especially in the oil and gas industry. Among various corrosive microbes, sulfate reducing bacteria (SRB) are often the leading culprit. Biofilm mitigation is the key to MIC mitigation. Biocide applications against biofilms promote resistance over time. Thus, it is imperative to develop new biodegradable and cost-effective biocides for large-scale field applications. Using the corrosive Desulfovibrio vulgaris (an SRB) biofilm as a model biofilm, this work demonstrated that a cocktail of glyceryl trinitrate (GTN) and caprylic acid (CA) was very effective for biofilm prevention and mitigation of established biofilms on C1018 carbon steel coupons. The most probable number sessile cell count data and confocal laser scanning microscope biofilm images proved that the biocide cocktail of 25 ppm (w/w) GTN + 0.1% (w/w) CA successfully prevented the D. vulgaris biofilm establishment on C1018 carbon steel coupons while 100 ppm GTN + 0.1% CA effectively mitigated pre-established D. vulgaris biofilms on C1018 carbon steel coupons. In both cases, the cocktails were able to reduce the sessile cell count from 10(6) cells/cm(2) to an undetectable level. PMID:26745983

  13. Calcitonin gene-related peptide (CGRP) levels during glyceryl trinitrate (GTN)-induced headache in healthy volunteers.

    PubMed

    Kruuse, C; Iversen, H K; Jansen-Olesen, I; Edvinsson, L; Olesen, J

    2010-04-01

    The role of nitric oxide (NO) in migraine has been studied in the experimental glyceryl trinitrate (GTN)-infusion headache model. We hypothesized that GTN-induced headache may activate the trigeminovascular system and be associated with increased levels of sensory neuropeptides, including calcitonin gene-related peptide (CGRP). CGRP, vasoactive intestinal peptide (VIP), neuropeptide Y (NPY) and somatostatin plasma levels were measured before and after placebo/sumatriptan injection and during GTN-induced headache. Following a double-blind randomized cross-over design, 10 healthy volunteers received subcutaneous sumatriptan 6 mg or placebo. This was succeeded by 20 min of GTN (0.12 µg kg(-1) min(-1)) infusion. At baseline no subject reported headache (using verbal rating scale from 0 to 10) and the jugular CGRP-like immunoreactivity (-LI) level was 18.6 ± 2.5 pmol/l. After a 20-min intravenous infusion of GTN 0.12 µg kg(-1) min(-1), median peak headache intensity was 4 (range 2-6) (P < 0.05), while jugular CGRP-LI levels were unchanged (19.0 ± 2.8 pmol/l; P > 0.05). There were no changes in VIP-, NPY- or somatostatin-LI. In conclusion, the NO donor GTN appears not to induce headache via immediate CGRP release.

  14. Enhanced rectal absorption of insulin in rabbits from hollow-type suppositories containing insulin and glyceryl-1-monooctanoate.

    PubMed

    Watanabe, Y; Matsumoto, Y; Hori, N; Funato, H; Matsumoto, M

    1991-11-01

    The absorption of two kinds of insulin (from porcine or bovine pancreas) from the rectum of rabbits after the administration of hollow-type suppositories containing insulin and glyceryl-1-monooctanoate (GMO) as an absorption-enhancing agent was investigated. Two types of suppositories were employed: type I containing insulin in an aqueous solution (approx. 25 IU/mg/100 microliters citric buffer solution at pH 3.0) in the cavity of the suppository and GMO mixed with a base material (Witepsol H-15), and type II containing insulin in a crystalline form in the same amount as in type I. Without GMO, the insulin and glucose levels in plasma were unchanged, whereas a marked increase in the plasma levels of insulin and a decrease of glucose concentrations were found following coadministration of insulin and GMO by the type I suppository. Similar enhancement of rectal absorption of insulin was obtained from porcine and bovine sources. In the case of the crystalline insulin, despite the use of the same amount of GMO, porcine insulin was more efficiently absorbed than bovine insulin by the type II suppository. GMO enhances the absorption of insulin in an aqueous solution or a crystalline form, and the dissolution rate of insulin may be an important factor in the rectal absorption of insulin.

  15. Buccal permeation of [D-Ala(2), D-Leu(5)]enkephalin from liquid crystalline phases of glyceryl monooleate.

    PubMed

    Lee, J; Kellaway, I W

    2000-02-15

    The ex vivo buccal permeability of a [D-Ala(2), D-Leu(5)]enkephalin (DADLE) and glyceryl monooleate (GMO) was examined from the cubic and lamellar liquid crystalline phases of GMO and aqueous phosphate-buffered saline (pH 7.4, PBS) solution across excised porcine buccal mucosa mounted in a Franz cell. GMO was released in vitro from the liquid crystalline phases indicating the erosion of the liquid crystal matrices. GMO released from the liquid crystalline matrices permeated the porcine buccal mucosa with fluxes of 0.10+/-0.03 and 0.07+/-0.00%/cm(2) per h for the cubic and lamellar phases, respectively. The flux of DADLE (1.21+/-0.32 and 1. 15+/-0.11%/cm(2) per h for the cubic and lamellar phases, respectively) from the liquid crystalline phases was significantly enhanced by the GMO compared with PBS solution (0.43+/-0.08%/cm(2) per h) during the initial permeation phase (t<3 h). Our results suggest that the cubic and lamellar liquid crystalline phases can be considered as promising buccal drug carriers for peptide drugs as well as acting as permeation enhancers.

  16. 4-alkoxyethoxy-N-octadecyl-1,8-naphthalimide fluorescent sensor for human serum albumin and other major blood proteins: design, synthesis and solvent effect.

    PubMed

    Wei, Song; Sun, Yang; Tan, Chunlei; Yan, Sen; Guo, Ping; Hu, Xiaoyun; Fan, Jun

    2013-01-01

    A series of 4-alkoxyethoxy-N-octadecyl-1,8-naphthalimides with intense blue fluorescence were designed and synthesized as polarity and spectrofluorimetric probes for the determination of proteins. In solvents of different polarities, the Stokes shifts of two dyes increased with increasing solvent polarity and fluorescence quantum yields decreased significantly, suggesting that electronic transiting from ground to excited states was π-π(*) in character. Dipole moment changes were estimated from solvent-dependent Stokes shift data using a solvatochromic method based on bulk solvent polarity functions and the microscopic solvent polarity parameter (E(T)N). These results were generally consistent with semi-empirical molecular orbital calculations and were found to be quite reliable based on the fact that the correlation of the solvatochromic Stokes shifts with E(T)N was superior to that obtained using bulk solvent polarity functions. Fluorescence data revealed that the fluorescence quenching of human serum albumin (HSA) by dyes was the result of the formation of a Dye-HSA complex. The method was applied to the determination of total proteins (HSA + immunoglobulins) in human serum samples and results were in good agreement with those reported by the research institute.

  17. Chromatographic retention behaviour of monosubstituted benzene derivatives on porous graphitic carbon and octadecyl-bonded silica studied using molecular modelling and quantitative structure-retention relationships.

    PubMed

    De Matteis, Cristina I; Simpson, David A; Euerby, Melvin R; Shaw, P Nicholas; Barrett, David A

    2012-03-16

    The retention behaviour of a series of 28 monosubstituted benzenes, representing a diverse range of functional groups and substituent shape, were investigated using porous graphitic carbon (PGC) and octadecyl-bonded silica (ODS) stationary phases. For the majority of analytes retention on PGC was greater than on ODS, and in most cases this effect occurred at both pH 2.5 and 7.0. The main trends observed on PGC (in comparison with ODS) were: (i) similar or reduced retention of low polarity molecules such as the hydrocarbon and halogenated analytes; (ii) increased retention of conjugated analytes with extended planarity; (iii) increased retention of polar and charged species; and (iv) substantial increases in retention for selected polar and negatively charged analytes, including some ionised and unionised acid analytes. Poor retention of positively charged analytes was observed on both stationary phases. Molecular modelling studies have explored the geometry of π-π stacking interactions in retention on PGC and have highlighted the strong retention of large conjugated analytes, with extended planar conformations, which can interact with the graphite surface with cofacial geometry. Quantitative structure-retention relationships showed the importance of hydrophobic (π) and electronic factors (e.g. mean polarisability and LUMO energy) in retention on PGC, whilst retention on ODS was correlated to hydrophobicity (logP and π). PMID:22305358

  18. Solid phase extraction of copper (II) by sorption on octadecyl silica membrane disk modified with a new Schiff base and determination with atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mashhadizadeh, Mohammad Hossein; Pesteh, Mahnaz; Talakesh, Mahzad; Sheikhshoaie, Iran; Ardakani, Mohammad Mazloum; Karimi, Mohammad Ali

    2008-08-01

    A simple, selective and reliable method for rapid extraction and determination of trace amounts of Cu (II) ions from aqueous samples using octadecyl-bonded silica membrane disks modified with bis-(3-methoxy salicylaldehyde)-1,6-diaminohexane and flame atomic absorption spectrometry (FAAS) is presented. Extraction efficiency, the influence of pH, flow rates, amount of ligand, and type and least amount of eluant were investigated. The linear dynamic range of the proposed method for Cu (II) ions was found in a wide concentration range of 1.0 (± 0.2)-150 (± 2) μg l - 1 . The detection limit and preconcentration factor of this method were found 30.0 (± 0.7) ng l - 1 and 100 respectively. The reproducibility of the procedure is at the most 2.0%. The effects of various cationic interferences on the percent recovery of copper ion were studied. The method was used to the recovery of copper ion from different synthetic, alloys and biological samples.

  19. Lysophosphatidylcholine attenuates the cytotoxic effects of the antineoplastic phospholipid 1-O-octadecyl-2-O-methyl-rac-glycero-3- phosphocholine.

    PubMed

    Boggs, K P; Rock, C O; Jackowski, S

    1995-05-12

    A colony-stimulating factor 1-dependent cell line was used to determine the relationship between the inhibition of phospholipid synthesis and the cytotoxic activity of the antineoplastic ether lipid, 1-O-octadecyl-2-O-methyl-rac-glycero-3-phosphocholine (ET-18-OCH3). ET-18-OCH3 inhibited choline incorporation into phosphatidylcholine as well as total phospholipid synthesis. Exposure to ET-18-OCH3 at the G1/S boundary led to the accumulation of cells in G2, whereas the addition of ET-18-OCH3 in the G1 phase of the cell cycle prevented entry into the S phase. In both cases, ET-18-OCH3 treatment triggered DNA fragmentation and morphological changes associated with apoptosis within 10 h. The addition of lysophosphatidylcholine provided an exogenous source of cellular phospholipid and prevented ET-18-OCH3-dependent accumulation of cells in G2 and apoptosis. However, lysophosphatidylcholine did not overcome the ET-18-OCH3-dependent G1 block, although the growth-arrested cells remained viable. These data indicate that restoring phosphatidylcholine synthesis by supplementation with lysophosphatidylcholine overrides the cytotoxic but not the cytostatic activity of ET-18-OCH3.

  20. Pharmacokinetics and enhanced oral bioavailability in beagle dogs of cyclosporine A encapsulated in glyceryl monooleate/poloxamer 407 cubic nanoparticles.

    PubMed

    Lai, Jie; Lu, Yi; Yin, Zongning; Hu, Fuqiang; Wu, Wei

    2010-01-01

    Efforts to improve the oral bioavailability of cyclosporine A (CyA) remains a challenge in the field of drug delivery. In this study, glyceryl monooleate (GMO)/poloxamer 407 cubic nanoparticles were evaluated as potential vehicles to improve the oral bioavailability of CyA. Cubic nanoparticles were prepared via the fragmentation of a bulk GMO/poloxamer 407 cubic phase gel by sonication and homogenization. The cubic inner structure formed was verified using Cryo-TEM. The mean diameters of the nanoparticles were about 180 nm, and the entrapment efficiency of these particles for CyA was over 85%. The in vitro release of CyA from these nanoparticles was less than 5% at 12 h. The results of a pharmacokinetic study in beagle dogs showed improved absorption of CyA from cubic nanoparticles as compared to microemulsion-based Neoral((R)); higher C(max) (1371.18 +/- 37.34 vs 969.68 +/- 176.3 ng mL(-1)), higher AUC(0-t) (7757.21 +/- 1093.64 vs 4739.52 +/- 806.30 ng h mL(-1)) and AUC(0-infinity) (9004.77 +/- 1090.38 vs 5462.31 +/- 930.76 ng h mL(-1)). The relative oral bioavailability of CyA cubic nanoparticles calculated on the basis of AUC(0-infinity) was about 178% as compared to Neoral((R)). The enhanced bioavailability of CyA is likely due to facilitated absorption by cubic nanoparticles rather than improved release.

  1. Glyceryl monooleyl ether-based liquid crystalline nanoparticles as a transdermal delivery system of flurbiprofen: characterization and in vitro transport.

    PubMed

    Uchino, Tomonobu; Murata, Akiko; Miyazaki, Yasunori; Oka, Toshihiko; Kagawa, Yoshiyuki

    2015-01-01

    Liquid crystalline nanoparticles (LCNs) were prepared using glyceryl monooleyl ether (GME) by the modified film rehydration method. Hydrogenated lecithin (HL), 1,3-butylene glycol (1,3-BG), and Poloxamer 407 were used as additives. The prepared LCN formulations were evaluated based on particle size, small-angle X-ray diffraction (SAXS) analysis, (1)H- and (19)F-NMR spectra, and in vitro skin permeation across Yucatan micropig skin. The composition (weight percent) of the LCN formulations were GME-HL-1,3-BG (4 : 1 : 15), 4% GME-based LCN and GME-HL-1,3-BG (8 : 1 : 15), 8% GME-based LCN and their mean particle sizes were 130-175 nm. Flurbiprofen 5 and 10 mg was loaded into 4% GME-based LCN and 8% GME-based LCN systems, respectively. The results of SAXS and NMR suggested that both flurbiprofen-loaded formulations consist of particles with reverse type hexagonal phase (formation of hexosome) and flurbiprofen molecules were localized in the lipid domain through interaction of flurbiprofen with the lipid components. Flurbiprofen transport from the LCN systems across the Yucatan micropig skin was increased compared to flurbiprofen in citric buffer (pH=3.0). The 8% GME-based LCN systems was superior to the 4% GME-based LCN for flurbiprofen transport. Since the internal hexagonal phase in the 8% GME-based LCN systems had a higher degree of order compared to the 4% GME-based LCN in SAXS patterns, the 8% GME-based LCN system had a larger surface area, which might influence flurbiprofen permeation. These results indicated that the GME-based LCN system is effective in improving the skin permeation of flurbiprofen across the skin.

  2. Glyceryl monooleyl ether-based liquid crystalline nanoparticles as a transdermal delivery system of flurbiprofen: characterization and in vitro transport.

    PubMed

    Uchino, Tomonobu; Murata, Akiko; Miyazaki, Yasunori; Oka, Toshihiko; Kagawa, Yoshiyuki

    2015-01-01

    Liquid crystalline nanoparticles (LCNs) were prepared using glyceryl monooleyl ether (GME) by the modified film rehydration method. Hydrogenated lecithin (HL), 1,3-butylene glycol (1,3-BG), and Poloxamer 407 were used as additives. The prepared LCN formulations were evaluated based on particle size, small-angle X-ray diffraction (SAXS) analysis, (1)H- and (19)F-NMR spectra, and in vitro skin permeation across Yucatan micropig skin. The composition (weight percent) of the LCN formulations were GME-HL-1,3-BG (4 : 1 : 15), 4% GME-based LCN and GME-HL-1,3-BG (8 : 1 : 15), 8% GME-based LCN and their mean particle sizes were 130-175 nm. Flurbiprofen 5 and 10 mg was loaded into 4% GME-based LCN and 8% GME-based LCN systems, respectively. The results of SAXS and NMR suggested that both flurbiprofen-loaded formulations consist of particles with reverse type hexagonal phase (formation of hexosome) and flurbiprofen molecules were localized in the lipid domain through interaction of flurbiprofen with the lipid components. Flurbiprofen transport from the LCN systems across the Yucatan micropig skin was increased compared to flurbiprofen in citric buffer (pH=3.0). The 8% GME-based LCN systems was superior to the 4% GME-based LCN for flurbiprofen transport. Since the internal hexagonal phase in the 8% GME-based LCN systems had a higher degree of order compared to the 4% GME-based LCN in SAXS patterns, the 8% GME-based LCN system had a larger surface area, which might influence flurbiprofen permeation. These results indicated that the GME-based LCN system is effective in improving the skin permeation of flurbiprofen across the skin. PMID:25948327

  3. Topical glyceryl trinitrate treatment of chronic patellar tendinopathy: a randomised, double-blind, placebo-controlled clinical trial

    PubMed Central

    Steunebrink, Mirjam; Zwerver, Johannes; Brandsema, Ruben; Groenenboom, Petra; van den Akker-Scheek, Inge; Weir, Adam

    2012-01-01

    Objectives To assess if continuous topical glyceryl trinitrate (GTN) treatment improves outcome in patients with chronic patellar tendinopathy when compared with eccentric training alone. Methods Randomised double-blind, placebo-controlled clinical trial comparing a 12-week programme of using a GTN or placebo patch in combination with eccentric squats on a decline board. Measurements were performed at baseline, 6, 12 and 24 weeks. Primary outcome measure was the Victorian Institute of Sports Assessment-Patella (VISA-P) questionnaire. Secondary outcome measures were patient satisfaction and pain scores during sports. Generalised estimated equation was used to analyse the treatment, time and treatment×time effect. Analyses were performed following the intention-to-treat principle. Results VISA-P scores for both groups improved over the study period to 75.0±16.2 and 80.7±22.1 at 24 weeks. Results showed a significant effect for time (p<0.01) but no effect for treatment×time (p=0.80). Mean Visual Analogue Scores pain scores during sports for both groups increased over the study period to 6.6±3 and 7.8±3.1. Results showed a significant effect for time (p<0.01) but no effect for treatment×time (p=0.38). Patient satisfaction showed no difference between GTN and placebo groups (p=0.25) after 24 weeks, but did show a significant difference over time (p=0.01). Three patients in the GTN group reported some rash. Conclusion It seems that continuous topical GTN treatment in addition to an eccentric exercise programme does not improve clinical outcome compared to placebo patches and an eccentric exercise programme in patients with chronic patellar tendinopathy. PMID:22930695

  4. Ictal lack of binding to brain parenchyma suggests integrity of the blood–brain barrier for 11C-dihydroergotamine during glyceryl trinitrate-induced migraine

    PubMed Central

    Schankin, Christoph J.; Maniyar, Farooq H.; Seo, Youngho; Kori, Shashidar; Eller, Michael; Chou, Denise E.; Blecha, Joseph; Murphy, Stephanie T.; Hawkins, Randall A.; Sprenger, Till; VanBrocklin, Henry F.

    2016-01-01

    See Dreier (doi: 10.1093/aww112) for a scientific commentary on this article. For many decades a breakdown of the blood–brain barrier has been postulated to occur in migraine. Hypothetically this would facilitate access of medications, such as dihydroergotamine or triptans, to the brain despite physical properties otherwise restricting their entry. We studied the permeability of the blood–brain barrier in six migraineurs and six control subjects at rest and during acute glyceryl trinitrate-induced migraine attacks using positron emission tomography with the novel radioligand 11C-dihydroergotamine, which is chemically identical to pharmacologically active dihydroergotamine. The influx rate constant Ki, average dynamic image and time activity curve were assessed using arterial blood sampling and served as measures for receptor binding and thus blood–brain barrier penetration. At rest, there was binding of 11C-dihydroergotamine in the choroid plexus, pituitary gland, and venous sinuses as expected from the pharmacology of dihydroergotamine. However, there was no binding to the brain parenchyma, including the hippocampus, the area with the highest density of the highest-affinity dihydroergotamine receptors, and the raphe nuclei, a postulated brainstem site of action during migraine, suggesting that dihydroergotamine is not able to cross the blood–brain barrier. This binding pattern was identical in migraineurs during glyceryl trinitrate-induced migraine attacks as well as in matched control subjects. We conclude that 11C-dihydroergotamine is unable to cross the blood–brain barrier interictally or ictally demonstrating that the blood–brain barrier remains tight for dihydroergotamine during acute glyceryl trinitrate-induced migraine attacks. PMID:27234268

  5. Fourier transform infrared spectroscopy and solid-state nuclear magnetic resonance studies of octadecyl modified metal oxides obtained from different silane precursors.

    PubMed

    Kailasam, Kamalakannan; Natile, Marta Maria; Glisenti, Antonella; Müller, Klaus

    2009-03-20

    Octadecyl (C(18)) modified metal oxide substrates, including titania, zirconia, hafnia, and alumina, are prepared using two types of silylating reagents, n-octadecyltrihydridosilane and n-octadecyltrichlorosilane. Fourier transform infrared (FTIR) and solid-state (29)Si nuclear magnetic resonance (NMR) measurements are performed to examine the cross-linking of the silanes. Solid-state (13)C NMR spectroscopy provides information about the conformation and mobility of surface-immobilized alkyl chains. Variable temperature FTIR investigations are carried out to study the influence of the organosilane precursors and metal oxides on the conformational order of the alkyl modified systems. It is found that grafting by means of n-octadecyltrichlorosilane yields higher grafting densities than surface modification with n-octadecyltrihydridosilane. Combined pyridine adsorption and diffuse reflectance infrared Fourier transform (DRIFT) measurements are performed on the titania and hafnia substrates to evaluate potential surface heterogeneities, i.e. Lewis and Brønsted sites. Differences in the alkyl chain conformational order within the series of C(18) modified metal oxides are explained by the presence of island structures. The reduced C(18) conformational order for the samples grafted with n-octadecyltrihydridosilane is traced back to the lower grafting density which in turn points to a lower reactivity of this silylating reagent. The most striking result is the higher conformational order of the C(18) chains grafted in the present surface modified metal oxides when compared with silica-based systems. This finding is attributed to the lower porosity of the metal oxide supports along with more closely packed chains on the surface.

  6. Effect of amine counterion type on the retention of basic compounds on octadecyl silane bonded silica-based and polybutadiene-coated zirconia phases.

    PubMed

    Yang, Xiqin; Dai, Jun; Carr, Peter W

    2003-07-01

    In a previous paper, we compared the mixed-mode retention characteristics of cationic solutes on octadecyl silane-bonded silica (ODS) and polybutadiene-coated zirconia (PBD-ZrO2) phases. It is well recognized that both reversed-phase and ion-exchange interactions contribute to the retention of cations on ODS phases. The reversed-phase interaction results from the bonded hydrocarbon chain; the ion-exchange interaction originates in the ionized residual silanol groups. These two types of interactions also exist on the PBD-ZrO2 phase. The polybutadiene contributes to the reversed-phase interaction and the ionized zirconol, but primarily, the adsorbed Lewis base anions, such as phosphate or fluoride, contribute to the ion-exchange interaction. We have shown that on ODS phases, reversed-phase interactions are much more important, whereas the opposite is true of PBD-ZrO2 phases. In this work, we investigate the effect of several amine mobile phase counterions on the retention of cationic solutes on ODS and PBD-ZrO2 phases. The effects of the chain length and the type of amine (1 degree, 2 degrees, 3 degrees) counterion on the retention of basic compounds were studied. In contrast to older studies of type A silica-based phases, the results show that the chain length and type of the amine blocker do not have a large effect on the retention of basic compounds with the newer type B silica-based materials. However, on the PBD-ZrO2 phase, very striking differences in retention were observed with different amine counterions. We show that the molecular geometry of the amine counterion has a significant effect on the retention of basic solutes on the PBD-ZrO2 phase. PMID:12964764

  7. Novel RAFT amphiphilic brush copolymer steric stabilisers for cubosomes: poly(octadecyl acrylate)-block-poly(polyethylene glycol methyl ether acrylate).

    PubMed

    Chong, Josephine Y T; Mulet, Xavier; Postma, Almar; Keddie, Daniel J; Waddington, Lynne J; Boyd, Ben J; Drummond, Calum J

    2014-09-21

    Copolymers, particularly Pluronics®, are typically used to sterically stabilise colloidal nanostructured particles composed of a lyotropic liquid crystalline bicontinuous cubic phase (cubosomes). There is a need to design and assess new functionalisable stabilisers for these colloidal drug delivery systems. Six amphiphilic brush copolymers, poly(octadecyl acrylate)-block-poly(polyethylene glycol methyl ether acrylate) (P(ODA)-b-P(PEGA-OMe)), synthesised by reversible addition-fragmentation chain transfer (RAFT), were assessed as novel steric stabilisers for cubosomes. It was found that increasing the density of PEG on the nanostructured particle surface by incorporating a PEG brush design (i.e., brush copolymer), provided comparable and/or increased stabilisation effectiveness compared to a linear PEG structure, Pluronic® F127, which is extensively used for steric stabilisation of cubosomes. Assessment was conducted both prior to and following the removal of the dodecyl trithiocarbonate end-group, by free radical-induced reduction. The reduced (P(ODA)-b-P(PEGA-OMe) copolymers were more effective steric stabilisers for phytantriol and monoolein colloidal particle dispersions than their non-reduced analogues. High throughput characterisation methodologies, including an accelerated stability assay (ASA) and synchrotron small angle X-ray scattering (SAXS), were implemented in this study for the rapid assessment of steric stabiliser effectiveness and lyotropic liquid crystalline phase identification. Phytantriol cubosomes stabilised with P(ODA)-b-P(PEGA-OMe) copolymers exhibited a double diamond cubic phase (Q(2)(D)), whilst monoolein cubosomes exhibited a primitive cubic phase (Q(2)(P)), analogous to those formed using Pluronic® F127. PMID:25058647

  8. Thin-film octadecyl-silica glass coating for automated 96-blade solid-phase microextraction coupled with liquid chromatography-tandem mass spectrometry for analysis of benzodiazepines.

    PubMed

    Mirnaghi, Fatemeh S; Monton, Maria Rowena N; Pawliszyn, Janusz

    2012-07-13

    A thin-film octadecyl (C18)-silica glass coating was developed as the extraction phase for an automated 96-blade solid-phase microextraction (SPME) system coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Various factors (e.g., sol-gel composition and aging time, coating preparation speed, coating thickness, and drying conditions) affecting the quality of C18-silica glass thin-film coating were studied and optimized. The results showed that the stability and durability of the coating are functions of the coating thickness and drying conditions. Coating thickness is controlled by sol-gel composition, aging time and the withdrawal speed in the dipping method. Automated sample preparation was achieved using a robotic autosampler that enabled simultaneous preparation of 96 samples in a 96-well plate format. Under the optimum SPME conditions the proposed system requires a total of 140 min for preparation of all 96 samples (i.e., 30 min preconditioning, 40 min equilibrium extraction, 40 min desorption and 30 min carry over step). The performance of the C18-silica glass 96-blade SPME system was evaluated for high-throughput analysis of benzodiazepines from phosphate-buffered saline solution (PBS) and human plasma, and the reusability, repeatability, and validity of the system were evaluated. When analysing spiked PBS and human plasma, the inter-blade reproducibility for four benzodiazepines was obtained in the ranges of 4-8% and 9-11% RSD (relative standard deviation), respectively, and intra-blade reproducibility were in the ranges of 3-9% and 8-13% RSD, respectively. The limits of detection and quantitation for plasma analysis were in the ranges of 0.4-0.7 ng/mL and 1.5-2.5 ng/mL for all four analytes.

  9. Pure short-chain glycerol fatty acid esters and glycerylic cyclocarbonic fatty acid esters as surface active and antimicrobial coagels protecting surfaces by promoting superhydrophilicity.

    PubMed

    Valentin, Romain; Alignan, Marion; Giacinti, Géraldine; Renaud, François N R; Raymond, Bernard; Mouloungui, Zéphirin

    2012-01-01

    Pure glycerol fatty acid esters and glycerylic cyclocarbonic fatty acid esters have an amphiphilic structure, giving these biomolecules a broad range of physico-chemical and biological properties. Physico-chemical properties depend on chain lengths, odd or even carbon numbers on the chain, and glyceryl or cyclocarbonic polar heads. The spectrum of melting-point values for these molecules is large. Surface-activity is very important and through determination of the critical aggregation concentration (CAC), some fatty-acid esters are considered as solvo-surfactant biomolecules. Coupling these self-aggregation and crystallization properties, superhydrophilic surfaces were obtained. An efficient durable water repellent coating of various metallic and polymeric surfaces was allowed. Moreover, these fatty acid esters promoting superhydrophilicity showed biological activity against Gram positive, Gram negative, and yeast-like micro-organisms. Such surfaces coated by self-assembled fatty acid esters in a stable coagel state present a novel solution to surface-contamination risks from pathogen proliferation.

  10. Comparison of the chromatography of octadecyl silane bonded silica and polybutadiene-coated zirconia phases based on a diverse set of cationic drugs.

    PubMed

    Dai, Jun; Yang, Xiqin; Carr, Peter W

    2003-07-11

    In this study, we compare the separation of basic drugs on several octadecyl silane bonded silica (ODS) phases and a polybutadiene-coated zirconia (PBD-ZrO2) phase. The retention characteristics were investigated in detail using a variety of cationic drugs as probe solutes. The ODS phases were selected to cover a relatively wide range in silanol activity and were studied with ammonium phosphate eluents at pH 3.0 and 6.0. Compared to any of the ODS phases, the PBD-ZrO2 phase showed very significant differences in selectivities towards these drugs. Due to the presence of both reversed-phase and ion-exchange interactions between the stationary phase and the basic analyte on ODS and PBD-ZrO2, mixed-mode retention takes place to some extent on both types of phases. However, very large differences in the relative contributions from ion-exchange and reversed-phase interactions on the two types of phases led to quite different selectivities. When phosphate is present in the eluent and adsorbs on the surface, the PBD-ZrO2 phase takes on a high negative charge over a wide pH range due to phosphate adsorption on its surface. On ODS phases, ion-exchange interactions result from the interactions between protonated basic compounds and ionized residual silanol groups. Since the pH of the eluent influences the charge state of the silanol groups, the ion-exchange interactions vary in strength depending on pH. At pH 6.0, the ion-exchange interactions are strong. However, at pH 3.0 the ion-exchange interactions on ODS are significantly smaller because the silanol groups are less dissociated at the lower pH. Thus, not only are the selectivities of the ODS and PBD-ZrO2 phases different but quite different trends in retention are observed on these two types of phases as the pH of the eluent is varied. More importantly, by using the large set of "real" basic analytes we show the extreme complexity of the chromatographic processes on the reversed stationary phases. Both the test condition

  11. Synthesis of a stationary phase based on silica modified with branched octadecyl groups by Michael addition and photoinduced thiol-yne click chemistry for the separation of basic compounds.

    PubMed

    Huang, Guang; Ou, Junjie; Wang, Hongwei; Ji, Yongsheng; Wan, Hao; Zhang, Zhang; Peng, Xiaojun; Zou, Hanfa

    2016-04-01

    A novel silica-based stationary phase with branched octadecyl groups was prepared by the sequential employment of the Michael addition reaction and photoinduced thiol-yne click chemistry with 3-aminopropyl-functionalized silica microspheres as the initial material. The resulting stationary phase denoted as SiO2 -N(C18)4 was characterized by elemental analysis, FTIR spectroscopy and Raman spectroscopy, demonstrating the existence of branched octadecyl groups in silica microspheres. The separations of benzene homologous compounds, acid compounds and amine analogues were conducted, demonstrating mixed-mode separation mechanism on SiO2 -N(C18)4 . Baseline separation of basic drugs mixture was acquired with the mobile phase of acetonitrile/H2 O (5%, v/v). SiO2 -N(C18)4 was further applied to separate Corydalis yanhusuo Wang water extracts, and more baseline separation peaks were obtained for SiO2 -N(C18)4 than those on Atlantis dC18 column. It can be expected that this new silica-based stationary phase will exhibit great potential in the analysis of basic compounds. PMID:26910263

  12. Brain, liver, and adipose tissue erucic and very long chain fatty acid levels in adrenoleukodystrophy patients treated with glyceryl trierucate and trioleate oils (Lorenzo's oil).

    PubMed

    Rasmussen, M; Moser, A B; Borel, J; Khangoora, S; Moser, H W

    1994-08-01

    Brain, liver, and adipose lipids were studied in the postmortem tissues of four adrenoleukodystrophy patients who had been treated with a mixture of glyceryl trioleate and trierucate oils ("Lorenzo's Oil") and compared to 7 untreated ALD patients and 3 controls. The dietary therapy appeared to reduce the levels of saturated very long chain fatty acids in the plasma, adipose tissue and liver; in the brain they were reduced in only one of the four patients. While substantial amounts of erucic acid were present in some of the tissues even 12 months after therapy had been discontinued, the levels in brain did not exceed those in controls at any time. The failure of erucic acid to enter the brain in significant quantity may be a factor in the disappointing results of dietary therapy for adrenoleukodystrophy.

  13. Determination of antihyperglycemic biguanides in serum and urine using an ion-pair solid-phase extraction technique followed by HPLC-UV on a pentafluorophenylpropyl column and on an octadecyl column.

    PubMed

    Tahara, Kayoko; Yonemoto, Ayumi; Yoshiyama, Yuji; Nakamura, Toshiya; Aizawa, Masaaki; Fujita, Yoshikuni; Nishikawa, Takashi

    2006-11-01

    An HPLC-UV method was established for the determination of metformin and buformin in biological fluids. Metformin was not retained on particles packed in conventional solid-phase extraction cartridges; in contrast, buformin was retained too firmly and not eluted with a solvent for recovery. However, both drugs were retained on particles that had been treated with an ion-pair reagent of heptanesulfonate or dodecylsulfate and recovered almost completely. The recovered fraction was subjected to HPLC on a pentafluorophenylpropyl column which was suitable for the determination of both biguanides in serum and in urine. Limits of quantitation were low enough for clinical use, and reproducibility was high with an RSD of 0.9-2.3%. HPLC on a conventional octadecyl column was suitable only for the determination of buformin in serum since interfering peaks appeared on the chromatograms of urine samples. The method was applied to analysis of some clinical specimens.

  14. Eugenolol and glyceryl-isoeugenol suppress LPS-induced iNOS expression by down-regulating NF-kappaB AND AP-1 through inhibition of MAPKS and AKT/IkappaBalpha signaling pathways in macrophages.

    PubMed

    Yeh, J L; Hsu, J H; Hong, Y S; Wu, J R; Liang, J C; Wu, B N; Chen, I J; Liou, S F

    2011-01-01

    Eugenol and isoeugenol, two components of clover oil, have been reported to possess several biomedical properties, such as anti-inflammatory, antimicrobial and antioxidant effects. This study aims to examine the anti-inflammatory effects of eugenol, isoeugenol and four of their derivatives on expression of inducible nitric oxide synthase (iNOS) activated by lipopolysaccharide (LPS) in mouse macrophages (RAW 264.7), and to investigate molecular mechanisms underlying these effects. We found that two derivatives, eugenolol and glyceryl-isoeugenol, had potent inhibitory effects on LPS-induced upregulation of nitrite levels, iNOS protein and iNOS mRNA. In addition, they both suppressed the release of tumor necrosis factor-alpha (TNF-alpha) and interleukin-1beta (IL-1beta) induced by LPS. Moreover, they both attenuated the DNA binding of NF-kB and AP-1, phosphorylation of inhibitory kB-alpha (IkB-alpha), and nuclear translocation of p65 protein induced by LPS. Finally, we demonstrated that glyceryl-isoeugenol suppressed the phosphorylation of ERK1/2, JNK and p38 MAPK, whereas eugenolol suppressed the phosphorylation of ERK1/2 and p38 MAPK. Taken together, these results suggest that that eugenolol and glyceryl-isoeugenol suppress LPS-induced iNOS expression by down-regulating NF-kB and AP-1 through inhibition of MAPKs and Akt/IkB-alpha signaling pathways. Thus, this study implies that eugenolol and glyceryl-isoeugenol may provide therapeutic benefits for inflammatory diseases.

  15. Ocular delivery of cyclosporine A based on glyceryl monooleate/poloxamer 407 liquid crystalline nanoparticles: preparation, characterization, in vitro corneal penetration and ocular irritation.

    PubMed

    Chen, Yan; Lu, Yi; Zhong, Yanqiang; Wang, Qingping; Wu, Wei; Gao, Shen

    2012-12-01

    The purpose of this study was to develop an ophthalmic drug delivery system for cyclosporine A (CsA) based on glyceryl monooleate (GMO)/poloxamer 407 liquid crystalline nanoparticles with reduced ocular irritancy and improved corneal penetration. CsA-loaded liquid crystalline nanoparticles were prepared via fragmentation of a bulk GMO/poloxamer 407 cubic phase gel by high-pressure homogenization and characterized. Corneal permeation and retention was evaluated using modified Franz diffusing cells. Intra-corneal transportation was investigated with fluorescein isothiocyanate (FITC)-labeled liquid crystalline nanoparticles. Ocular irritation was then evaluated using the Draize method. The mean particle size of liquid crystalline nanoparticles was 193.5 nm and the entrapment efficiency was 95.11 ± 0.67%. A bicontinuous cubic phase of cubic P-type was determined using cryo-transmission electron microscopy (cryo-TEM) observation and small angle X-ray diffraction (SAXD) analysis. A 1.52-fold increase in J(s) and a 2.2-fold increase in corneal retention was achieved by liquid crystalline nanoparticles compared with oil solution. In vitro corneal permeation investigated with FITC-labeled liquid crystalline nanoparticles revealed that CsA penetrated across the cornea under the transportation of liquid crystalline nanoparticles. Liquid crystalline nanoparticles exhibited excellent ocular tolerance in the ocular irritation test. This low-irritant vehicle based on liquid crystalline nanoparticles might be a promising system for effective ocular CsA delivery.

  16. Glyceryl monooleate/poloxamer 407 cubic nanoparticles as oral drug delivery systems: I. In vitro evaluation and enhanced oral bioavailability of the poorly water-soluble drug simvastatin.

    PubMed

    Lai, Jie; Chen, Jianming; Lu, Yi; Sun, Jing; Hu, Fuqiang; Yin, Zongning; Wu, Wei

    2009-01-01

    Glyceryl monooleate (GMO)/poloxamer 407 cubic nanoparticles were investigated as potential oral drug delivery systems to enhance the bioavailability of the water-insoluble model drug simvastatin. The simvastatin-loaded cubic nanoparticles were prepared through fragmentation of the GMO/poloxamer 407 bulk cubic-phase gel using high-pressure homogenization. The internal structure of the cubic nanoparticles was identified by cryo-transmission electron microscopy. The mean diameter of the cubic nanoparticles varied within the range of 100-150 nm, and both GMO/poloxamer 407 ratio and theoretical drug loading had no significant effect on particle size and distribution. Almost complete entrapment with efficiency over 98% was achieved due to the high affinity of simvastatin to the hydrophobic regions of the cubic phase. Release of simvastatin from the cubic nanoparticles was limited both in 0.1 M hydrochloride solution containing 0.2% sodium lauryl sulfate and fasted-state simulated intestinal fluid with a total release of <3.0% at 10 h. Pharmacokinetic profiles in beagle dogs showed sustained plasma levels of simvastatin for cubic nanoparticles over 12 h. The relative oral bioavailability of simvastatin cubic nanoparticles calculated on the basis of area under the curve was 241% compared to simvastatin crystal powder. The enhancement of simvastatin bioavailability was possibly attributable to facilitated absorption by lipids in the formulation rather than improved release.

  17. Glyceryl trinitrate metabolism in the quail embryo by the glutathione S-transferases leads to a perturbation in redox status and embryotoxicity.

    PubMed

    Bardai, Ghalib K; Hales, Barbara F; Sunahara, Geoffrey I

    2013-07-01

    Exposure of stage 9 quail (Coturnix coturnix japonica) embryos to glyceryl trinitrate (GTN) induces malformations that were associated in previous studies with an increase in protein nitration. Increased nitration suggests metabolism of GTN by the embryo. The goals of this study were to characterize the enzymes and co-factors required for GTN metabolism by quail embryos, and to determine the effects of in ovo treatment with N-acetyl cysteine (NAC), a precursor of glutathione (GSH), on GTN embryotoxicity. GTN treatment of quail embryos resulted in an increase in nitrite, a decrease in total GSH, and an increase in the ratio of NADP(+)/NADPH, indicating that redox balance may be compromised in exposed embryos. Glutathione S-transferases (GSTs; EC 2.5.1.18) purified from the whole embryo (K(m) 0.84 mM; V(max) 36 μM/min) and the embryonic eye (K(m) 0.20 mM; V(max) 30 μM/min) had GTN-metabolizing activity (1436 and 34 nmol/min/mg, respectively); the addition of ethacrynic acid, an inhibitor of GST activity, decreased GTN metabolism. Peptide sequencing of the GST isozymes indicated that alpha- or mu-type GSTs in the embryo and embryonic eye had GTN metabolizing activity. NAC co-treatment partially protected against the effects of GTN exposure. Thus, GTN denitration by quail embryo GSTs may represent a key initial step in the developmental toxicity of GTN.

  18. The Effect of Remote Ischemic Conditioning and Glyceryl Trinitrate on Perioperative Myocardial Injury in Cardiac Bypass Surgery Patients: Rationale and Design of the ERIC-GTN Study.

    PubMed

    Hamarneh, Ashraf; Sivaraman, Vivek; Bulluck, Heerajnarain; Shanahan, Hilary; Kyle, Bonnie; Ramlall, Manish; Chung, Robin; Jarvis, Claire; Xenou, Maria; Ariti, Cono; Cordery, Roger; Yellon, Derek M; Hausenloy, Derek J

    2015-11-01

    Remote ischemic conditioning (RIC) using transient limb ischemia/reperfusion has been reported to reduce perioperative myocardial injury in patients undergoing coronary artery bypass grafting and/or valve surgery. The role of intravenous glyceryl trinitrate (GTN) therapy administered during cardiac surgery as a cardioprotective agent and whether it interferes with RIC cardioprotection is not clear and is investigated in the ERIC-GTN trial ( http://www.clinicaltrials.gov: NCT01864252). The ERIC-GTN trial is a single-site, double-blind, randomized, placebo-controlled study. Consenting adult patients (age > 18 years) undergoing elective coronary artery bypass grafting ± valve surgery with blood cardioplegia will be eligible for inclusion. Two hundred sixty patients will be randomized to 1 of 4 treatment groups following anesthetic induction: (1) RIC alone, a RIC protocol comprising three 5-minute cycles of simultaneous upper-arm and thigh cuff inflation/deflation followed by an intravenous (IV) placebo infusion; (2) GTN alone, a simulated sham RIC protocol followed by an IV GTN infusion; (3) RIC + GTN, a RIC protocol followed by an IV GTN infusion; and (4) neither RIC nor GTN, a sham RIC protocol followed by IV placebo infusion. The primary endpoint will be perioperative myocardial injury as quantified by the 72-hour area-under-the-curve serum high-sensitivity troponin T. The ERIC-GTN trial will determine whether intraoperative GTN therapy is cardioprotective during cardiac surgery and whether it affects RIC cardioprotection.

  19. Solid phase extraction of ultra traces mercury (II) using octadecyl silica membrane disks modified by 1,3-bis(2-ethoxyphenyl)triazene (EPT) ligand and determination by cold vapor atomic absorption spectrometry.

    PubMed

    Rofouei, Mohammad Kazem; Sabouri, Alireza; Ahmadalinezhad, Asieh; Ferdowsi, Hadis

    2011-09-15

    A facile and highly efficient method was developed for the preconcentration of the ultra trace amounts of mercury (II) ions. Octadecyl silica membrane disk was modified by the recently synthesized triazene ligand, 1,3-bis(2-ethoxyphenyl)triazene (EPT), and cold vapor atomic absorption spectrometry was used to determine the resultant preconcentrated Hg(II) ions. Solution studies with EPT and a series of metal ions were done in advance, and the results showed a strong affinity of EPT to the mercury ions. To perform solid phase extraction, various parameters such as pH of the sample, flow rates and the amount of the ligand were optimized. A linear calibration curve was obtained in the range of 0.02-1.90 μg L(-1) with r(2) = 0.9990 (n = 8), and the limit of detection (LOD) based on three times the standard deviation of the blank was 10.6 ng L(-1). The relative standard deviation (RSD) for the determination of 0.1 μg L(-1) Hg(II) found to be 2.9% while a RSD value of 1.1% was obtained for the determination of 1.0 μg L(-1) Hg(II) (n = 8). The preconcentration and improvement factors were 380 and 74, respectively. The newly developed method was successfully applied to the determination of mercury ions in real water samples.

  20. Solid phase extraction of ultra traces mercury (II) using octadecyl silica membrane disks modified by 1,3-bis(2-ethoxyphenyl)triazene (EPT) ligand and determination by cold vapor atomic absorption spectrometry.

    PubMed

    Rofouei, Mohammad Kazem; Sabouri, Alireza; Ahmadalinezhad, Asieh; Ferdowsi, Hadis

    2011-09-15

    A facile and highly efficient method was developed for the preconcentration of the ultra trace amounts of mercury (II) ions. Octadecyl silica membrane disk was modified by the recently synthesized triazene ligand, 1,3-bis(2-ethoxyphenyl)triazene (EPT), and cold vapor atomic absorption spectrometry was used to determine the resultant preconcentrated Hg(II) ions. Solution studies with EPT and a series of metal ions were done in advance, and the results showed a strong affinity of EPT to the mercury ions. To perform solid phase extraction, various parameters such as pH of the sample, flow rates and the amount of the ligand were optimized. A linear calibration curve was obtained in the range of 0.02-1.90 μg L(-1) with r(2) = 0.9990 (n = 8), and the limit of detection (LOD) based on three times the standard deviation of the blank was 10.6 ng L(-1). The relative standard deviation (RSD) for the determination of 0.1 μg L(-1) Hg(II) found to be 2.9% while a RSD value of 1.1% was obtained for the determination of 1.0 μg L(-1) Hg(II) (n = 8). The preconcentration and improvement factors were 380 and 74, respectively. The newly developed method was successfully applied to the determination of mercury ions in real water samples. PMID:21782328

  1. The ether lipid 1-octadecyl-2-methyl-rac-glycero-3-phosphocholine induces expression of fos and jun proto-oncogenes and activates AP-1 transcription factor in human leukaemic cells.

    PubMed Central

    Mollinedo, F; Gajate, C; Modolell, M

    1994-01-01

    The ether lipid analogue 1-octadecyl-2-methyl-rac-glycero-3-phosphocholine (ET-18-OCH3) has been recently shown to induce apoptosis in the human leukaemic HL-60 and U937 myeloid cell lines [Mollinedo, Martinez-Dalmau and Modolell (1993) Biochem. Biophys. Res. Commun. 192, 603-609]. We have found that ET-18-OCH3 is also able to promote apoptosis in the human leukaemic Jurkat T lymphoid cell line. This lymphoid cell line as well as the two myeloid HL-60 and U937 cell lines incorporated significant amounts of exogenously added radiolabelled ET-18-OCH3. Addition of ET-18-OCH3 to these human leukaemic cells induced an increase in the steady-state mRNA levels of fos and jun proto-oncogenes, components of the transcription factor AP-1. These increases in fos and jun mRNA levels were associated with the activation of the AP-1 transcription factor after addition of ET-18-OCH3 to human leukaemic cells, as assessed by an enhanced binding activity of transcription factor AP-1 to its cognate DNA sequence as well as by stimulation of transcription from an AP-1 enhancer element. These data demonstrate that the ether lipid ET-18-OCH3 can affect gene expression by inducing expression of fos and jun proto-oncogenes and by modulating the activity of transcription factor AP-1. Images Figure 2 Figure 3 Figure 4 PMID:8092982

  2. Controlling retention, selectivity and magnitude of EOF by segmented monolithic columns consisting of octadecyl and naphthyl monolithic segments--applications to RP-CEC of both neutral and charged solutes.

    PubMed

    Karenga, Samuel; El Rassi, Ziad

    2011-04-01

    Monolithic capillaries made of two adjoining segments each filled with a different monolith were introduced for the control and manipulation of the electroosmotic flow (EOF), retention and selectivity in reversed phase-capillary electrochromatography (RP-CEC). These columns were called segmented monolithic columns (SMCs) where one segment was filled with a naphthyl methacrylate monolith (NMM) to provide hydrophobic and π-interactions, while the other segment was filled with an octadecyl acrylate monolith (ODM) to provide solely hydrophobic interaction. The ODM segment not only provided hydrophobic interactions but also functioned as the EOF accelerator segment. The average EOF of the SMC increased linearly with increasing the fractional length of the ODM segment. The neutral SMC provided a convenient way for tuning EOF, selectivity and retention in the absence of annoying electrostatic interactions and irreversible solute adsorption. The SMCs allowed the separation of a wide range of neutral solutes including polycyclic aromatic hydrocarbons (PAHs) that are difficult to separate using conventional alkyl-bonded stationary phases. In all cases, the k' of a given solute was a linear function of the fractional length of the ODM or NMM segment in the SMCs, thus facilitating the tailoring of a given SMC to solve a given separation problem. At some ODM fractional length, the fabricated SMC allowed the separation of charged solutes such as peptides and proteins that could not otherwise be achieved on a monolithic column made from NMM as an isotropic stationary phase due to the lower EOF exhibited by this monolith.

  3. Glyceryl Trinitrate for Prevention of Post-ERCP Pancreatitis and Improve the Rate of Cannulation: A Meta-Analysis of Prospective, Randomized, Controlled Trials

    PubMed Central

    Pan, Yue; Liu, Shan; Li, Youming

    2013-01-01

    Background Acute pancreatitis is the most common complication of diagnostic and therapeutic endoscopic retrograde cholangiopancreatography (ERCP). Several clinical trials used glyceryl trinitrate (GTN) to prevent the incidence of post-ERCP pancreatitis (PEP). However, the results were still controversial. Objective To conduct a meta-analysis of published, full-length, randomized controlled trials evaluating the effect of prophylactic GTN on the prevention of PEP, improve the rate of cannulation and the prevention of hyperamylasemia. Methods Literature searches were conducted using PubMed, EMBASE, The Cochrane Library and Web of Knowledge databases, using keywords "post-ERCP" and "pancreatitis" and limited in randomized controlled trials. Results Twelve RCTs involving 2649 patients were included. Eleven RCTs compared GTN with placebo for PEP prevention. Meta-analysis showed the overall incidence of PEP was significantly reduced by GTN treatment (RR 0.67; 95% CI, 0.52-0.87). Nevertheless, GTN administration did not decrease the incidence of moderate to severe PEP (RR 0.70; 95% CI, 0.42-1.15). Subgroup analyses revealed that GTN administered by sublingual was more effective than transdermal and topical in reducing the incidence of PEP. Besides, the prophylactic effect of GTN was far more obvious in the group of high PEP incidence than in the group of low PEP incidence. Additionally, the incidence of hyperamylasemia was significantly reduced by GTN treatment (RR 0.69; 95% CI, 0.54-0.90). No differences of the successful cannulation rate of bile ducts (RR 1.03; 95% CI, 0.99-1.06) attributable to GTN were observed. Conclusion Prophylactic use of GTN reduced the overall incidence of PEP and hyperamylasemia. However, GTN was not helpful for the severity of PEP and the rate of cannulation. PMID:24098392

  4. Selective anti-platelet aggregation synergism between a prostacyclin-mimetic, RS93427 and the nitrodilators sodium nitroprusside and glyceryl trinitrate.

    PubMed

    Willis, A L; Smith, D L; Loveday, M; Fulks, J; Lee, C H; Hedley, L; VanAntwerp, D

    1989-12-01

    1. Citrated platelet-rich plasma from human donors was used to examine turbidometrically the platelet aggregation response to collagen (2.5 micrograms ml-1) and ADP (1.6 microgram ml-1). 2. With collagen as an aggregating agent, the limited (35% maximal inhibition) inhibitory effects of glyceryl trinitrate (GTN, 0.78-50 micrograms ml-1) were markedly potentiated by threshold (3.3-10 ng ml-1) concentrations of RS93427, an orally active prostacyclin-mimetic. Almost complete inhibition of aggregation could then be produced. 3. A threshold concentration of RS93427 (3.3 ng ml-1) similarly potentiated the ability of sodium nitroprusside (NaNp, 0.78-10 micrograms ml-1) to inhibit collagen-induced platelet aggregation. There was an 8 fold reduction in the IC25 concentration of NaNp. 4. Threshold concentrations of the nitrodilators were also able to potentiate the anti-aggregatory effects of RS93427 (0.03-30 ng ml-1) on collagen-induced platelet aggregation. With threshold concentrations of either GTN (6.3-25 micrograms ml-1) or NaNp (0.3-1.3 microgram ml-1), the mean IC50 concentration of RS93427 was reduced 4 or 6 fold, respectively, while the IC25 concentration was reduced 6 or 10 fold, respectively. 5. No similar synergistic interactions were seen between RS93427 and the nitrodilators when ADP was used as an aggregating agent. 6. In spontaneously hypertensive rats, the dose-response for the hypotensive response to bolus doses of RS93427 was not altered by concomitant steady state infusion of a threshold dose (1 micrograms kg-1 min-1) of GTN. 7. Possible therapeutic implications of these findings are discussed.

  5. Oral nitric-oxide donor glyceryl-trinitrate induces sensitization in spinal cord pain processing in migraineurs: a double-blind, placebo-controlled, cross-over study.

    PubMed

    Perrotta, Armando; Serrao, Mariano; Tassorelli, Cristina; Arce-Leal, Natalia; Guaschino, Elena; Sances, Grazia; Rossi, Paolo; Bartolo, Michelangelo; Pierelli, Francesco; Sandrini, Giorgio; Nappi, Giuseppe

    2011-05-01

    Nitric-oxide donor glyceryl-trinitrate (GTN) modulates cerebral and spinal regions that are involved in migraine and pain processing. We hypothesized that in migraineurs, the susceptibility to develop a migraine attack after GTN administration should parallel with an high sensitivity to GTN-induced change in the pain processing at spinal level. We used the temporal summation threshold (TST) of the lower limb nociceptive withdrawal reflex (NWR) and the related pain sensation to study in parallel the time-course of the effect of the GTN administration on the pain processing at spinal level in migraine and healthy subjects. Twenty-eight (21 F; 7M; mean age 34.2 ± 8.2) migraine and 15 (11 F; 4M; mean age 35.9 ± 8.9) healthy subjects were recruited in a double-blind, placebo-controlled, cross-over trial. Neurophysiological examinations were carried out before (baseline) and 30', 60', 120', 180' and 240' after GTN (0.9 mg sublingual) or placebo administration during two different sessions. In migraineurs, GTN administration was associated to a significant facilitation in temporal summation of pain (reduced TST and increased painful sensation) 60', 120' and 180' after drug intake when compared to baseline, to placebo condition and to controls after GTN intake. Furthermore, in migraineurs who developed migraine after GTN, a significant facilitation in temporal summation of pain was detected 60', 120' and 180' after drug intake when compared to patients without clinical response. In migraineurs the susceptibility to develop migraine attack after GTN administration seems to be a specific trait of a subgroup of patients linked to a supersensitivity of the pain system to GTN.

  6. Protective effects of riboflavin and selenium on brain microsomal Ca2+-ATPase and oxidative damage caused by glyceryl trinitrate in a rat headache model.

    PubMed

    Nazıroğlu, Mustafa; Çelik, Ömer; Uğuz, Abdulhadi Cihangir; Bütün, Ayşe

    2015-03-01

    Migraine headaches are considered to be associated with increased mitochondrial energy metabolism. Mitochondrial oxidative stress is also important in migraine headache pathophysiology although riboflavin and selenium (Se) induced a modulator role on mitochondrial oxidative stress in the brain. The current study aimed to determine the effects of Se with/without riboflavin on the microsomal membrane Ca(2+)-ATPase (MMCA), lipid peroxidation, antioxidant, and electroencephalography (EEG) values in glyceryl trinitrate (GTN)-induced brain injury rats. Thirty-two rats were randomly divided into four groups. The first group was used as the control, and the second group was the GTN group. Se and Se plus oral riboflavin were administered to rats constituting the third and fourth groups for 10 days prior to GTN administration. The second, third, and fourth groups received GTN to induce headache. Ten hours after the administration of GTN, the EEG records and brain cortex samples were obtained for all groups. Brain cortex microsomes were obtained from the brain samples. The brain and microsomal lipid peroxidation levels were higher in the GTN group compared to the control group, whereas they were decreased by selenium and selenium + riboflavin treatments. Vitamin A, vitamin C, vitamin E, and reduced glutathione (GSH) concentrations of the brain and MMCA, GSH and glutathione peroxidase values of microsomes were decreased by the GTN administration, although the values and β-carotene concentrations were increased by Se and Se + riboflavin treatments. There was no significant change in EEG records of the four groups. In conclusion, Se with/without riboflavin administration protected against GTN-induced brain oxidative toxicity by inhibiting free radicals and the modulation of MMCA activity and supporting the antioxidant redox system.

  7. Riboflavin and vitamin E increase brain calcium and antioxidants, and microsomal calcium-ATP-ase values in rat headache models induced by glyceryl trinitrate.

    PubMed

    Bütün, Ayşe; Nazıroğlu, Mustafa; Demirci, Serpil; Çelik, Ömer; Uğuz, Abdulhadi Cihangir

    2015-04-01

    The essential use of riboflavin is the prevention of migraine headaches, although its effect on migraines is considered to be associated with the increased mitochondrial energy metabolism. Oxidative stress is also important in migraine pathophysiology. Vitamin E is a strong antioxidant in nature and its analgesic effect is not completely clear in migraines. The current study aimed to investigate the effects of glyceryl trinitrate (GTN)-sourced exogen nitric oxide (NO), in particular, and also riboflavin and/or vitamin E on involved in the headache model induced via GTN-sourced exogen NO on oxidative stress, total brain calcium levels, and microsomal membrane Ca(2+)-ATPase levels. GTN infusion is a reliable method to provoke migraine-like headaches in experimental animals and humans. GTN resulted in a significant increase in brain cortex and microsomal lipid peroxidation levels although brain calcium, vitamin A, vitamin C, and vitamin E, and brain microsomal-reduced glutathione (GSH), glutathione peroxidase (GSH-Px), and plasma-membrane Ca(2+)-ATPase values decreased through GTN. The lipid peroxidation, GSH, vitamin A, β-carotene, vitamin C, and vitamin E, and calcium concentrations, GSH-Px, and the Ca(2+)-ATPase activities were increased both by riboflavin and vitamin E treatments. Brain calcium and vitamin A concentrations increased through riboflavin only. In conclusion, riboflavin and vitamin E had a protective effect on the GTN-induced brain injury by inhibiting free radical production, regulation of calcium-dependent processes, and supporting the antioxidant redox system. However, the effects of vitamin E on the values seem more important than in riboflavin.

  8. Decreased sensitivity to 1-O-octadecyl-2-O-methyl-glycerophosphocholine in MCF-7 cells adapted for serum-free growth correlates with constitutive association of Raf-1 with cellular membranes.

    PubMed

    Samadder, P; Arthur, G

    1999-10-01

    We have previously shown that inhibition of MCF-7 cell proliferation by 1-O-octadecyl-2-O-methyl-glycerophosphocholine (ET-18-OCH3) is linked to a drug-induced decrease in membrane Raf-1 levels and the subsequent inhibition of mitogen-activated protein (MAP) kinase activation in response to growth factor stimulation. We now report that adaptation of MCF-7 cells for growth in a serum-free formulation results in decreased sensitivity to growth inhibition by ET-18-OCH3. The decrease in ET-18-OCH3 sensitivity occurred progressively during the adaptation process and correlated with the presence of increasing amounts of inactive Raf-1 that stably associated with MCF-7 cell membranes. ET-18-OCH3 sensitivity could be restored by growing the adapted cells in serum-containing medium, which resulted in the loss of membrane-associated Raf-1. In human normal mammary epithelial cells, which are insensitive to ET-18-OCH3, Raf-1 was also associated with membranes in quiescent cells. In both cell types, incubation with ET-18-OCH3 had no effect on the membrane-Raf-1 levels, suggesting that ET-18-OCH3-induced reduction of Raf-1 levels in growth factor-stimulated MCF-7 cells is due to inhibition of Raf translocation. The activation and termination of the MAP kinase pathway in response to growth factors in the adapted MCF-7 cells and HNME cells occurred without changes to membrane Raf-1 levels. Because membrane translocation is not required to activate Raf in these cells, inhibition of Raf translocation by ET-18-OCH3 subsequent to cell stimulation has no effect on the activation of the membrane-bound Raf and, consequently, the activation of the MAP kinase pathway. The ability of the cells to activate the MAP kinase pathway in the presence of the drugs enables them to resist the growth-inhibitory effects of the drug, leading to the observed ET-18-OCH3 insensitivity of the cells.

  9. Effect of Treatment Delay, Stroke Type, and Thrombolysis on the Effect of Glyceryl Trinitrate, a Nitric Oxide Donor, on Outcome after Acute Stroke: A Systematic Review and Meta-Analysis of Individual Patient from Randomised Trials

    PubMed Central

    Bath, Philip M.; Woodhouse, Lisa; Krishnan, Kailash; Anderson, Craig; Berge, Eivind; Ford, Gary A.; Robinson, Thompson G.; Saver, Jeffrey L.; Sprigg, Nikola; Wardlaw, Joanna M.; in Acute Stroke Collaboration (BASC), Blood pressure

    2016-01-01

    Background. Nitric oxide (NO) donors are a candidate treatment for acute stroke and two trials have suggested that they might improve outcome if administered within 4–6 hours of stroke onset. We assessed the safety and efficacy of NO donors using individual patient data (IPD) from completed trials. Methods. Randomised controlled trials of NO donors in patients with acute or subacute stroke were identified and IPD sought from the trialists. The effect of NO donor versus control on functional outcome was assessed using the modified Rankin scale (mRS) and death, by time to randomisation. Secondary outcomes included measures of disability, mood, and quality of life. Results. Five trials (4,197 participants) were identified, all involving glyceryl trinitrate (GTN). Compared with control, GTN lowered blood pressure by 7.4/3.3 mmHg. At day 90, GTN did not alter any clinical measures. However, in 312 patients randomised within 6 hours of stroke onset, GTN was associated with beneficial shifts in the mRS (odds ratio (OR) 0.52, 95% confidence interval (CI) 0.34–0.78) and reduced death (OR 0.32, 95% CI 0.14–0.78). Conclusions. NO donors do not alter outcome in patients with recent stroke. However, when administered within 6 hours, NO donors might improve outcomes in both ischaemic and haemorrhagic stroke. PMID:27190674

  10. Final report on the safety assessment of Ricinus Communis (Castor) Seed Oil, Hydrogenated Castor Oil, Glyceryl Ricinoleate, Glyceryl Ricinoleate SE, Ricinoleic Acid, Potassium Ricinoleate, Sodium Ricinoleate, Zinc Ricinoleate, Cetyl Ricinoleate, Ethyl Ricinoleate, Glycol Ricinoleate, Isopropyl Ricinoleate, Methyl Ricinoleate, and Octyldodecyl Ricinoleate.

    PubMed

    2007-01-01

    The oil derived from the seed of the Ricinus communis plant and its primary constituent, Ricinoleic Acid, along with certain of its salts and esters function primarily as skin-conditioning agents, emulsion stabilizers, and surfactants in cosmetics, although other functions are described. Ricinus Communis (Castor) Seed Oil is the naming convention for castor oil used in cosmetics. It is produced by cold pressing the seeds and subsequent clarification of the oil by heat. Castor oil does not contain ricin because ricin does not partition into the oil. Castor oil and Glyceryl Ricinoleate absorb ultraviolet (UV) light, with a maximum absorbance at 270 nm. Castor oil and Hydrogenated Castor Oil reportedly were used in 769 and 202 cosmetic products, respectively, in 2002; fewer uses were reported for the other ingredients in this group. The highest reported use concentration (81%) for castor oil is associated with lipstick. Castor oil is classified by Food and Drug Administration (FDA) as generally recognized as safe and effective for use as a stimulant laxative. The Joint Food and Agriculture Organization (FAO)/World Health Organization (WHO) Expert Committee on Food Additives established an acceptable daily castor oil intake (for man) of 0 to 0.7 mg/kg body weight. Castor oil is hydrolyzed in the small intestine by pancreatic enzymes, leading to the release of glycerol and Ricinoleic Acid, although 3,6-epoxyoctanedioic acid, 3,6-epoxydecanedioic acid, and 3,6-epoxydodecanedioic acid also appear to be metabolites. Castor oil and Ricinoleic Acid can enhance the transdermal penetration of other chemicals. Although chemically similar to prostaglandin E(1), Ricinoleic Acid did not have the same physiological properties. These ingredients are not acute toxicants, and a National Toxicology Program (NTP) subchronic oral toxicity study using castor oil at concentrations up to 10% in the diet of rats was not toxic. Other subchronic studies of castor oil produced similar findings

  11. Final report on the safety assessment of Ricinus Communis (Castor) Seed Oil, Hydrogenated Castor Oil, Glyceryl Ricinoleate, Glyceryl Ricinoleate SE, Ricinoleic Acid, Potassium Ricinoleate, Sodium Ricinoleate, Zinc Ricinoleate, Cetyl Ricinoleate, Ethyl Ricinoleate, Glycol Ricinoleate, Isopropyl Ricinoleate, Methyl Ricinoleate, and Octyldodecyl Ricinoleate.

    PubMed

    2007-01-01

    The oil derived from the seed of the Ricinus communis plant and its primary constituent, Ricinoleic Acid, along with certain of its salts and esters function primarily as skin-conditioning agents, emulsion stabilizers, and surfactants in cosmetics, although other functions are described. Ricinus Communis (Castor) Seed Oil is the naming convention for castor oil used in cosmetics. It is produced by cold pressing the seeds and subsequent clarification of the oil by heat. Castor oil does not contain ricin because ricin does not partition into the oil. Castor oil and Glyceryl Ricinoleate absorb ultraviolet (UV) light, with a maximum absorbance at 270 nm. Castor oil and Hydrogenated Castor Oil reportedly were used in 769 and 202 cosmetic products, respectively, in 2002; fewer uses were reported for the other ingredients in this group. The highest reported use concentration (81%) for castor oil is associated with lipstick. Castor oil is classified by Food and Drug Administration (FDA) as generally recognized as safe and effective for use as a stimulant laxative. The Joint Food and Agriculture Organization (FAO)/World Health Organization (WHO) Expert Committee on Food Additives established an acceptable daily castor oil intake (for man) of 0 to 0.7 mg/kg body weight. Castor oil is hydrolyzed in the small intestine by pancreatic enzymes, leading to the release of glycerol and Ricinoleic Acid, although 3,6-epoxyoctanedioic acid, 3,6-epoxydecanedioic acid, and 3,6-epoxydodecanedioic acid also appear to be metabolites. Castor oil and Ricinoleic Acid can enhance the transdermal penetration of other chemicals. Although chemically similar to prostaglandin E(1), Ricinoleic Acid did not have the same physiological properties. These ingredients are not acute toxicants, and a National Toxicology Program (NTP) subchronic oral toxicity study using castor oil at concentrations up to 10% in the diet of rats was not toxic. Other subchronic studies of castor oil produced similar findings

  12. Quantification of ultra-trace amounts of copper by using off-line solid phase extraction-flame atomic absorption spectrometric determination through the octadecyl silica-bonded phase membrane (OSPM) C18 disks impregnated with 2,2'-[ethane-1,2-diylbis(thio)]dianiline.

    PubMed

    Mohammadhosseini, Majid; Soliemani, Esmaeil

    2014-07-01

    This study reports a very selective, easy, and precise method for rapid separation of trace amounts of copper in aqueous samples using octadecyl silica-bonded phase membrane disks modified by 2,2'-[ethane-1,2-diylbis(thio)]dianiline (EDTD) combined with flame atomic absorption spectrometric determination. In addition, the synthesis and spectral characterization of EDTD have been described in detail. All the affecting experimental variables such as pH, amount of modifier, eluent type, sample and eluent flow rate, interfering ions, and disk capacity were also investigated. The target analyte (trace copper) was quantitatively retained at pH = 4 and eluted with 6.0 mL of 0.5 M HNO3 at flow rates of 40 and 10 mL min−1 for analyte passage and elution steps, respectively, through the disks modified with 17.0 mg of EDTD. The proposed method also allows an enrichment factor of about 500 and has a detection limit of 0.005 ng mL−1. The method has been successfully applied for isolation and determination of copper in different water samples, peppers, and standard alloys.

  13. 21 CFR 184.1324 - Glyceryl monostearate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... glycerolysis of certain fats or oils that are derived from edible sources or by esterification, with glycerin, of stearic acid that is derived from edible sources. (b) The ingredient must be of a purity...

  14. 21 CFR 172.811 - Glyceryl tristearate.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... reacting stearic acid with glycerol in the presence of a suitable catalyst. (b) The food additive meets the following specifications: Acid number: Not to exceed 1.0. Iodine number: Not to exceed 1.0....

  15. 21 CFR 172.811 - Glyceryl tristearate.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... glycerol content: Not to exceed 0.5 percent. Unsaponifiable matter: Not to exceed 0.5 percent. Melting point (Class II): 69 °C-73 °C. (c) The additive is used or intended for use as follows when standards...

  16. 21 CFR 172.811 - Glyceryl tristearate.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... glycerol content: Not to exceed 0.5 percent. Unsaponifiable matter: Not to exceed 0.5 percent. Melting point (Class II): 69 °C-73 °C. (c) The additive is used or intended for use as follows when standards...

  17. 21 CFR 172.811 - Glyceryl tristearate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... glycerol content: Not to exceed 0.5 percent. Unsaponifiable matter: Not to exceed 0.5 percent. Melting point (Class II): 69 °C-73 °C. (c) The additive is used or intended for use as follows when standards...

  18. 21 CFR 172.811 - Glyceryl tristearate.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... glycerol content: Not to exceed 0.5 percent. Unsaponifiable matter: Not to exceed 0.5 percent. Melting point (Class II): 69 °C-73 °C. (c) The additive is used or intended for use as follows when standards...

  19. 21 CFR 184.1323 - Glyceryl monooleate.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... ingredient is used in food with no limitation other than current good manufacturing practice. The affirmation of this ingredient as generally recognized as safe (GRAS) as a direct human food ingredient is based... vehicle as defined in § 170.3(o)(27) of this chapter. (2) The ingredient is used in the following foods...

  20. Effect of drug solubility and different excipients on floating behaviour and release from glyceryl monooleate matrices.

    PubMed

    Kumar M, Kiran; Shah, Manish H; Ketkar, Anant; Mahadik, K R; Paradkar, Anant

    2004-03-19

    Glycerol monooleate (GMO) matrix was found to be a gastro-retentive carrier system suitable for both polar and as well as non-polar drugs. Chlorpheniramine maleate (CPM) and diazepam (DZP) were used as model drugs. Effect of PEG 4000, PEG 10000, and stearic acid on floatability and release profile was studied. Water uptake increased with increase in the loading of polar drug (CPM) and decreased with non-polar drug (DZP). Similar effect was found to occur in case of drug release. PEGs increased the release up to certain concentration and decreased thereafter. Drug release decreased linearly with concentration of stearic acid. The type and extent of mesophases formed were significantly affected by the nature of drug, excipients and their concentration. Thus the selection of suitable excipients depending on polarity of drug, could help to modulate the floatability and release profile from GMO matrices.

  1. Treatment of Xerosis with a Topical Formulation Containing Glyceryl Glucoside, Natural Moisturizing Factors, and Ceramide

    PubMed Central

    Kausch, Martina; Rippke, Frank; Schoelermann, Andrea M.; Filbry, Alexander W.

    2012-01-01

    Objective: To assess the effects of Light Formulation, an oil-in-water emulsion, and Rich Formulation, a water-in-oil emulsion, for the treatment of xerosis. Design: Two double-blind, vehicle-controlled trials (both formulations); a double-blind, randomized regression study (Rich Formulation); and a single-blind tolerability study (Light Formulation). The two formulations were applied twice daily for two weeks, for five days in the regression study, and twice daily for two weeks in the tolerability study. Setting: Studies were conducted during winter in Hamburg, Germany. Participants: A total of 169 subjects were enrolled and 154 completed the studies. The majority were between 50 and 80 years of age, women, all with very dry skin. One withdrew because of an incompatibility reaction that reoccurred with the subject's own body lotion after sun exposure. Measurements: Skin hydration and skin barrier function with both formulations over two weeks, long-term moisturization effect after discontinuation of Rich Formulation, and symptom improvement and skin tolerability with Light Formulation. Results: Vehicle-controlled studies of Light and Rich Formulations demonstrated significantly improved hydration at Weeks 1 and 2 versus the untreated site and vehicles, and significantly reduced transepidermal water loss versus untreated site and basic vehicle. Both products significantly decreased visible dryness and tactile roughness. In the regression study, Rich Formulation maintained significant moisturization six days after treatment discontinuation. Light Formulation reduced symptoms of itching, burning, tightness, tingling, and feeling of dryness. Conclusion: These formulations represent a new approach for the treatment of xerosis by addressing multiple key deficiencies in skin hydration. PMID:22916312

  2. Glycerophosphocholine Metabolism in Higher Plant Cells. Evidence of a New Glyceryl-Phosphodiester Phosphodiesterase

    PubMed Central

    van der Rest, Benoît; Boisson, Anne-Marie; Gout, Elisabeth; Bligny, Richard; Douce, Roland

    2002-01-01

    Glycerophosphocholine (GroPCho) is a diester that accumulates in different physiological processes leading to phospholipid remodeling. However, very little is known about its metabolism in higher plant cells. 31P-Nuclear magnetic resonance spectroscopy and biochemical analyses performed on carrot (Daucus carota) cells fed with GroPCho revealed the existence of an extracellular GroPCho phosphodiesterase. This enzymatic activity splits GroPCho into sn-glycerol-3-phosphate and free choline. In vivo, sn-glycerol-3-phosphate is further hydrolyzed into glycerol and inorganic phosphate by acid phosphatase. We visualized the incorporation and the compartmentation of choline and observed that the major choline pool was phosphorylated and accumulated in the cytosol, whereas a minor fraction was incorporated in the vacuole as free choline. Isolation of plasma membranes, culture medium, and cell wall proteins enabled us to localize this phosphodiesterase activity on the cell wall. We also report the existence of an intracellular glycerophosphodiesterase. This second activity is localized in the vacuole and hydrolyzes GroPCho in a similar fashion to the cell wall phosphodiesterase. Both extra- and intracellular phosphodiesterases are widespread among different plant species and are often enhanced during phosphate deprivation. Finally, competition experiments on the extracellular phosphodiesterase suggested a specificity for glycerophosphodiesters (apparent Km of 50 μm), which distinguishes it from other phosphodiesterases previously described in the literature. PMID:12226504

  3. In-vivo evaluation of clindamycin release from glyceryl monooleate-alginate microspheres by NIR spectroscopy.

    PubMed

    Mohamed, Amir Ibrahim; Ahmed, Osama A A; Amin, Suzan; Elkadi, Omar Anwar; Kassem, Mohamed A

    2015-10-15

    The purpose of this study was to use near-infrared (NIR) transmission spectroscopic technique to determine clindamycin plasma concentration after oral administration of clindamycin loaded GMO-alginate microspheres using rabbits as animal models. Lyophilized clindamycin-plasma standard samples at a concentration range of 0.001-10 μg/ml were prepared and analyzed by NIR and HPLC as a reference method. NIR calibration model was developed with partial least square (PLS) regression analysis. Then, a single dose in-vivo evaluation was carried out and clindamycin-plasma concentration was estimated by NIR. Over 24 h time period, the pharmacokinetic parameters of clindamycin were calculated for the clindamycin loaded GMO-alginate microspheres (F3) and alginate microspheres (F2), and compared with the plain drug (F1). PLS calibration model with 7-principal components (PC), and 8000-9200 cm(-1) spectral range shows a good correlation between HPLC and NIR values with root mean square error of cross validation (RMSECV), root mean square error of prediction (RMSEP), and calibration coefficient (R(2)) values of 0.245, 1.164, and 0.9753, respectively, which suggests that NIR transmission technique can be used for drug-plasma analysis without any extraction procedure. F3 microspheres exhibited controlled and prolonged absorption Tmax of 4.0 vs. 1.0 and 0.5 h; Cmax of 2.37±0.3 vs. 3.81±0.8 and 5.43±0.7 μg/ml for F2 and F1, respectively. These results suggest that the combination of GMO and alginate (1:4 w/w) could be successfully employed for once daily clindamycin microspheres formulation which confirmed by low Cmax and high Tmax values.

  4. Effect of ethylcellulose and propylene glycol on the controlled-release performance of glyceryl monooleate-mertronidazole periodontal gel.

    PubMed

    Sallam, Al-Sayed; Hamudi, Firas Falih; Khalil, Enam Ayoub

    2015-03-01

    Controlled-release metronidazole, mucoadhesive gel proposed as a drug-delivery system for periodontal application was developed and characterized. The system was based on a mixture of glycerylmonooleate (GMO) and ethylcellulose (EC). The mechanism of release depends: firstly, on the ability of GMO to form a viscous liquid crystalline mesophases and secondly on the solubilized EC to form a hydrophobic network when the mixture comes into contact with water resulting in sustaining the release of the drug. Ethylcellulose dissolved in GMO had a profound influence on the rate of drug release, reduced the initial drug release and prolonged the sustained release of metronidazole. Propylene glycol (PG) was added to increase the solubility of the drug and water was added with PG to control the viscosity. A controlled release formulation containing w/w, 20% metronidazole, 10% PG, 5% water and 65% GMO that contains 7% EC was found to be mucoadhesive, easily injectable at room temperature, and to follow Fickian diffusion release mechanism. When the drug loading was increased the drug release was accelerated, and the mechanism followed anomalous controlled-release mechanism. Stability studies indicated that the formulation should be stored at 4 °C in a dark place.

  5. Liquid Crystalline Nanoparticles as an Ophthalmic Delivery System for Tetrandrine: Development, Characterization, and In Vitro and In Vivo Evaluation

    NASA Astrophysics Data System (ADS)

    Liu, Rui; Wang, Shuangshuang; Fang, Shiming; Wang, Jialu; Chen, Jingjing; Huang, Xingguo; He, Xin; Liu, Changxiao

    2016-05-01

    The purpose of this study was to develop novel liquid crystalline nanoparticles (LCNPs) that display improved pre-ocular residence time and ocular bioavailability and that can be used as an ophthalmic delivery system for tetrandrine (TET). The delivery system consisted of three primary components, including glyceryl monoolein, poloxamer 407, and water, and two secondary components, including Gelucire 44/14 and amphipathic octadecyl-quaternized carboxymethyl chitosan. The amount of TET, the amount of glyceryl monoolein, and the ratio of poloxamer 407 to glyceryl monoolein were selected as the factors that were used to optimize the dependent variables, which included encapsulation efficiency and drug loading. A three-factor, five-level central composite design was constructed to optimize the formulation. TET-loaded LCNPs (TET-LCNPs) were characterized to determine their particle size, zeta potential, entrapment efficiency, drug loading capacity, particle morphology, inner crystalline structure, and in vitro drug release profile. Corneal permeation in excised rabbit corneas was evaluated. Pre-ocular retention was determined using a noninvasive fluorescence imaging system. Finally, pharmacokinetic study in the aqueous humor was performed by microdialysis technique. The optimal formulation had a mean particle size of 170.0 ± 13.34 nm, a homogeneous distribution with polydispersity index of 0.166 ± 0.02, a positive surface charge with a zeta potential of 29.3 ± 1.25 mV, a high entrapment efficiency of 95.46 ± 4.13 %, and a drug loading rate of 1.63 ± 0.07 %. Transmission electron microscopy showed spherical particles that had smooth surfaces. Small-angle X-ray scattering profiles revealed an inverted hexagonal phase. The in vitro release assays showed a sustained drug release profile. A corneal permeation study showed that the apparent permeability coefficient of the optimal formulation was 2.03-fold higher than that of the TET solution. Pre-ocular retention

  6. Liquid Crystalline Nanoparticles as an Ophthalmic Delivery System for Tetrandrine: Development, Characterization, and In Vitro and In Vivo Evaluation.

    PubMed

    Liu, Rui; Wang, Shuangshuang; Fang, Shiming; Wang, Jialu; Chen, Jingjing; Huang, Xingguo; He, Xin; Liu, Changxiao

    2016-12-01

    The purpose of this study was to develop novel liquid crystalline nanoparticles (LCNPs) that display improved pre-ocular residence time and ocular bioavailability and that can be used as an ophthalmic delivery system for tetrandrine (TET). The delivery system consisted of three primary components, including glyceryl monoolein, poloxamer 407, and water, and two secondary components, including Gelucire 44/14 and amphipathic octadecyl-quaternized carboxymethyl chitosan. The amount of TET, the amount of glyceryl monoolein, and the ratio of poloxamer 407 to glyceryl monoolein were selected as the factors that were used to optimize the dependent variables, which included encapsulation efficiency and drug loading. A three-factor, five-level central composite design was constructed to optimize the formulation. TET-loaded LCNPs (TET-LCNPs) were characterized to determine their particle size, zeta potential, entrapment efficiency, drug loading capacity, particle morphology, inner crystalline structure, and in vitro drug release profile. Corneal permeation in excised rabbit corneas was evaluated. Pre-ocular retention was determined using a noninvasive fluorescence imaging system. Finally, pharmacokinetic study in the aqueous humor was performed by microdialysis technique. The optimal formulation had a mean particle size of 170.0 ± 13.34 nm, a homogeneous distribution with polydispersity index of 0.166 ± 0.02, a positive surface charge with a zeta potential of 29.3 ± 1.25 mV, a high entrapment efficiency of 95.46 ± 4.13 %, and a drug loading rate of 1.63 ± 0.07 %. Transmission electron microscopy showed spherical particles that had smooth surfaces. Small-angle X-ray scattering profiles revealed an inverted hexagonal phase. The in vitro release assays showed a sustained drug release profile. A corneal permeation study showed that the apparent permeability coefficient of the optimal formulation was 2.03-fold higher than that of the TET solution. Pre

  7. Stable isotope-assisted LC-MS/MS monitoring of glyceryl trinitrate bioactivation in a cell culture model of nitrate tolerance.

    PubMed

    Axton, Elizabeth R; Hardardt, Elizabeth A; Stevens, Jan F

    2016-04-15

    The nitric oxide (NO) metabolites nitrite (NO2(-)) and nitrate (NO3(-)) can be quantified as an endpoint of endothelial function. We developed a LC-MS/MS method of measuring nitrite and nitrate isotopologues, which has a lower limit of quantification (LLOQ) of 1 nM. This method allows for isotopic labeling to differentiate newly formed nitrite and nitrate from nanomolar to micromolar background levels of nitrite and nitrate in biological matrices. This method utilizes 2,3-diaminonaphthalene (DAN) derivatization, which reacts with nitrite under acidic conditions to produce 2,3-naphthotriazole (NAT). NAT was chromatographically separated on a Shimadzu LC System with an Agilent Extend-C18 5 μm 2.1 × 150 mm column and detected using a multiple reaction monitoring (MRM) method on an ABSciex 3200 QTRAP mass spectrometer operated in positive mode. Mass spectrometry allows for the quantification of (14)N-NAT (m/z 170.1) and (15)N-NAT (m/z 171.1). Both nitrite and nitrate demonstrated a linear detector response (1 nM - 10 μM, 1 nM - 100 nM, respectively), and were unaffected by common interferences (Dulbecco's Modified Eagle Medium (DMEM), fetal bovine serum (FBS), phenol red, and NADPH). This method requires minimal sample preparation, making it ideal for most biological applications. We applied this method to develop a cell culture model to study the development of nitrate tolerance in human endothelial cells (EA.hy926). PMID:26796748

  8. Choline alphoscerate (alpha-glyceryl-phosphoryl-choline) an old choline- containing phospholipid with a still interesting profile as cognition enhancing agent.

    PubMed

    Traini, Enea; Bramanti, Vincenzo; Amenta, Francesco

    2013-12-01

    Cholinergic precursors have represented the first approach to counter cognitive impairment occurring in adultonset dementia disorders. These compounds were early leaved because their clinical efficacy was not clearly demonstrated. This is probably not true for some choline-containing phospholipids including choline alphoscerate. Choline alphoscerate increases the release of acetylcholine in rat hippocampus, facilitates learning and memory in experimental animals, improves brain transduction mechanisms and decreases age-dependent structural changes occurring in rat brain areas involved in learning and memory. The compound exerts neuroprotective effects in models of altered cholinergic neurotransmission and of brain vascular injury. In clinical studies choline alphoscerate improved memory and attention impairment, as well as affective and somatic symptoms in dementia disorders. An ongoing trial indicates that association between the acetylcholinesterase inhibitor donepezil and choline alphoscerate is accompanied by an improvement in several cognitive tests superior to that induced by donepezil alone. It is suggested that this association may represent a therapeutic option to prolong beneficial effects of cholinergic therapies in Alzheimer's disease patients with concomitant ischemic cerebrovascular disorders. In summary, choline alphoscerate has significant effects on cognitive function with a good safety profile and tolerability. Although limited both in terms of size of the samples investigated and of the length of treatment, preclinical and clinical results presented suggest that cognitive enhancing capabilities of choline alphoscerate merit of being further investigated in appropriate trials.

  9. Particulate and bulk bicontinuous cubic phases obtained from mixtures of glyceryl monooleate and copolymers bearing blocks of lipid-mimetic anchors in water.

    PubMed

    Rangelov, Stanislav; Almgren, Mats

    2005-03-10

    Copolymers based on poly(ethylene glycol) bearing one or more lipid-mimetic anchors were mixed with glycerylmonooleate (GMO)-a lipid with nonlamellar propensity-to form bulk and particulate bicontinuous cubic phases in water. The particulate phase was obtained via a liquid precursor method. Three forms of copolymer/GMO mixtures were investigated-precursor dispersions in glycerol and bulk and particulate phases in water-by visual observations, dynamic light scattering (DLS), and cryogenic transmission electron microscopy (cryo-TEM). The bulk phases were found to very slowly develop a macroscopic appearance that can be associated with the bicontinuous cubic phase. They were prepared in a slight excess of water, which became opalescent in some of the preparations. Cryo-TEM investigation of the excess showed that vesicles and particles with a dense interior coexisted. The precursors were prepared as solutions in glycerol. The viscous liquid material was investigated by DLS. Diffusion coefficients and the corresponding hydrodynamic radii, ranging from about 10 to 30 nm, were calculated. The particles are presumably of a structure similar to that of conventional emulsion droplets with GMO in the interior and copolymer molecules in the outer regions. The particulate phase in water was obtained upon hydration of the liquid precursors. The dispersions were investigated by DLS and cryo-TEM. DLS revealed the formation of nanosized particles. The size was found to increase with increasing copolymer content for copolymers with only one lipid-mimetic anchor, whereas the opposite trend was observed for the formulations with copolymers bearing more than one lipid-mimetic anchor. The shape and interior of the particles were studied by cryo-TEM. It was found that most particles were globular. For some of the compositions, particles with a dense internal structure dominated. The texture of the internal structures was assigned to dispersed bicontinuous cubic or L3 phases. In other compositions, the interior seemingly consists of arrays of interlamellar attachments.

  10. 5-HIAA

    MedlinePlus

    HIAA; 5-hydroxyindole acetic acid; Serotonin metabolite ... interfere with the test. Medicines that can increase 5-HIAA measurements include acetaminophen (Tylenol), acetanilide, phenacetin, glyceryl ...

  11. [Analysis of constituents in urushi wax, a natural food additive].

    PubMed

    Jin, Zhe-Long; Tada, Atsuko; Sugimoto, Naoki; Sato, Kyoko; Masuda, Aino; Yamagata, Kazuo; Yamazaki, Takeshi; Tanamoto, Kenichi

    2006-08-01

    Urushi wax is a natural gum base used as a food additive. In order to evaluate the quality of urushi wax as a food additive and to obtain information useful for setting official standards, we investigated the constituents and their concentrations in urushi wax, using the same sample as scheduled for toxicity testing. After methanolysis of urushi wax, the composition of fatty acids was analyzed by GC/MS. The results indicated that the main fatty acids were palmitic acid, oleic acid and stearic acid. LC/MS analysis of urushi wax provided molecular-related ions of the main constituents. The main constituents were identified as triglycerides, namely glyceryl tripalmitate (30.7%), glyceryl dipalmitate monooleate (21.2%), glyceryl dioleate monopalmitate (2.1%), glyceryl monooleate monopalmitate monostearate (2.6%), glyceryl dipalmitate monostearate (5.6%), glyceryl distearate monopalmitate (1.4%). Glyceryl dipalmitate monooleate isomers differing in the binding sites of each constituent fatty acid could be separately determined by LC/MS/MS. PMID:16984037

  12. Lipstick dermatitis due to C18 aliphatic compounds.

    PubMed

    Hayakawa, R; Matsunaga, K; Suzuki, M; Arima, Y; Ohkido, Y

    1987-04-01

    An 18-year-old girl developed cheilitis. She had a past history of lip cream dermatitis, but the cause was not found. Patch tests with 2 lipsticks were strongly positive. Tests with the ingredients were positive to 2 aliphatic compounds, glyceryl diisostearate and diisostearyl malate. Impurities in the materials were suspected as the cause. Analysis by gas chromatography detected 3 chemicals in glyceryl diisostearate and 1 in diisostearyl malate as impurities. Patch testing with the impurities and glyceryl monoisostearate 0.01% pet in glyceryl diisostearate and isostearyl alcohol 0.25% pet in diisostearyl malate were strongly positive. The characteristics common to the 2 chemicals were liquidity at room temperature, branched C18 aliphatic compound and primary alcohol. Chemicals lacking any of the above 3 features did not react.

  13. 21 CFR 172.515 - Synthetic flavoring substances and adjuvants.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ...-Amylcinnamaldehyde dimethyl acetal. α-Amylcinnamyl acetate. α-Amylcinnamyl alcohol. α-Amylcinnamyl formate. α... phenylacetate. Anisyl propionate. Beechwood creosote. Benzaldehyde dimethyl acetal. Benzaldehyde glyceryl acetal...-undecenoate. Butyl valerate. Butyraldehyde. Cadinene. Camphene; 2,2-dimethyl-3-methylenenorbornane....

  14. 21 CFR 172.515 - Synthetic flavoring substances and adjuvants.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...-Amylcinnamaldehyde dimethyl acetal. α-Amylcinnamyl acetate. α-Amylcinnamyl alcohol. α-Amylcinnamyl formate. α... phenylacetate. Anisyl propionate. Beechwood creosote. Benzaldehyde dimethyl acetal. Benzaldehyde glyceryl acetal...-undecenoate. Butyl valerate. Butyraldehyde. Cadinene. Camphene; 2,2-dimethyl-3-methylenenorbornane....

  15. 21 CFR 172.515 - Synthetic flavoring substances and adjuvants.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ...-Amylcinnamaldehyde dimethyl acetal. α-Amylcinnamyl acetate. α-Amylcinnamyl alcohol. α-Amylcinnamyl formate. α... phenylacetate. Anisyl propionate. Beechwood creosote. Benzaldehyde dimethyl acetal. Benzaldehyde glyceryl acetal...-undecenoate. Butyl valerate. Butyraldehyde. Cadinene. Camphene; 2,2-dimethyl-3-methylenenorbornane....

  16. 21 CFR 172.515 - Synthetic flavoring substances and adjuvants.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...-Amylcinnamaldehyde dimethyl acetal. α-Amylcinnamyl acetate. α-Amylcinnamyl alcohol. α-Amylcinnamyl formate. α... phenylacetate. Anisyl propionate. Beechwood creosote. Benzaldehyde dimethyl acetal. Benzaldehyde glyceryl acetal...-undecenoate. Butyl valerate. Butyraldehyde. Cadinene. Camphene; 2,2-dimethyl-3-methylenenorbornane....

  17. Photocontact allergy to benzocaine.

    PubMed

    Kaidbey, K H; Allen, H

    1981-02-01

    A photodermatitis developed in two patients after the use of commercial sunscreens and a topical anesthetic lotion containing benzocaine. Photopatch testing indicated the presence of photocontact allergy to benzocaine. One patient had a positive photopatch test to a commercial glyceryl para-aminobenzoic acid (PABA) preparation that was heavily contaminated with benzocaine, but not to a benzocaine-free sample of glyceryl PABA. Benzocaine failed to produce phototoxic reactions in normal volunteers. Efforts to induce photocontact allergy in guinea pigs were unsuccessful.

  18. Improvement of clinical and MRI findings in a boy with adrenoleukodystrophy by dietary erucic acid therapy.

    PubMed

    Maeda, K; Suzuki, Y; Yajima, S; Asano, J; Yamaguchi, S; Matsumoto, N; Borel, J; Moser, H W; Orii, T

    1992-11-01

    A 5-year-old boy with adrenoleukodystrophy, with clinical symptoms of visual, mental and motor disturbances which progressed rapidly, was treated with Lorenzo's oil consisting 1 volume of glyceryl trierucate and 4 volumes of glyceryl trioleate. Five months after initiation of this therapy, ability to swallow was enhanced and T2-weighted magnetic resonance imaging of the brain revealed regression of high intensity area of the parieto-occipital white matter.

  19. Influence of nitrovasodilators on bovine pulmonary histamine release.

    PubMed

    Valentovic, M A; Ball, J G; Morenas, M; Szarek, J L; Gruetter, C A

    1992-06-01

    The organic nitrates and related nitrovasodilators are relaxants of vascular and airway smooth muscle. Very little information is currently available regarding the influence of nitrates and related nitrovasodilators on pulmonary autacoid release. This study examined the influence of glyceryl trinitrate, isosorbide dinitrate and sodium nitroprusside on histamine release from bovine lung mince. Spontaneous histamine release from bovine lung mince was not altered by 0.1 nM to 1 microM glyceryl trinitrate, isosorbide dinitrate or sodium nitroprusside. Glyceryl trinitrate, isosorbide dinitrate and sodium nitroprusside produced a concentration-dependent decrease in A23187 (10 microM) stimulated histamine release. Glyceryl trinitrate also inhibited histamine liberation following the addition of compound 48/80. Further studies indicated that the inhibitory action of glyceryl trinitrate was reversed by coincubation with the guanylate cyclase inhibitor, methylene blue (10 microM). These findings indicate that glyceryl trinitrate, sodium nitroprusside and isosorbide dinitrate inhibit non-immunologically stimulated pulmonary histamine release and suggest that alterations in guanylate cyclase activity may influence pulmonary histamine release.

  20. [Preparation and properties of organobentonites].

    PubMed

    Zheng, Yu-Ying; Zhang, Han-Hui; Cai, Wei-Long; Fu, Ming-Lian; Wang, Liang-En

    2005-01-01

    The chemistry organobentonites were synthesized by means of the ionexchange reaction between single-octadecyl trimethyl ammonium chloride(SOAC), di-octadecyl dimethyl ammonium chloride (DOAC) , tri-octadecyl methylammonium chloride (TOAC) quaternary ammonium salts and sodium base bentonies, respectively. The authors used FTIR, X-ray diffraction diagram and DSC thermograms to characterate the structure of the modified bentonites, and discussed the effect of different quaternary ammonium salt on the properties of organobentonites. The results showed that ion of the surfactants had entered into the chip layer of the bentonites, and changed the hydrophilic environment of the chip layer into hydrophobic environment and increased the distance among the chip layer, all of these had laid a base for the preparation of the nanometer composite material of high polymer/bentonite. PMID:15852820

  1. Interactions of non-charged tadalafil stereoisomers with cyclodextrins: capillary electrophoresis and nuclear magnetic resonance studies.

    PubMed

    Fejős, Ida; Kazsoki, Adrienn; Sohajda, Tamás; Márványos, Ede; Volk, Balázs; Szente, Lajos; Béni, Szabolcs

    2014-10-10

    The single isomer drug R,R-tadalafil (Cialis) contains two chiral centers thus four stereoisomers (R,R-, S,S-, S,R- and R,S-tadalafil) exist, however, only the most potent inhibitor, the R,R-tadalafil is in clinical use. In our study, over 20 charged cyclodextrin (CD) derivatives were studied for enantiospecific host-guest type interactions in CD-modified capillary electrophoresis. Tadalafil stereoisomers are non-charged; therefore, their electrophoretic separation poses a challenge. Several candidates of both positively and negatively charged hosts were found to be effective for the enantioseparation. Eight out of the beta derivatives and three of alpha derivatives (including sulfated, sulfoalkylated, carboxyalkylated and amino derivatives) resolved all four stereoisomers partially or completely. Cavity size-dependent absolute enantiomer migration order (EMO) reversals were observed in the case of sulfopropyl-alpha (EMO: R,S; S,R; R,R; S,S) and sulfopropyl-beta (S,S; R,R; S,R; R,S) derivatives, while substituent-dependent partial EMO reversals were detected for sulfobutyl-ether-alpha (R,S; S,R; S,S; R,R) and sulfated-alpha-CD (R,R; S,S; R,S; S,R) selectors. Complexation-induced (1)H NMR chemical shift changes reflected that the benzodioxole moiety plays a major role in cavity size-dependent EMO reversal. Sulfobutyl-ether-alpha-CD was the only selector that provided the desired EMO in which the clinically applied eutomer R,R-tadalafil migrates last. Finally, an electrophoretic method applying a background electrolyte (BGE) containing 75 mM Tris-acetic acid buffer (pH 4.75) and 7 mM sulfobutyl-ether-alpha-CD was developed for the baseline resolution of all isomers at 25 °C and +25 kV applied voltage.

  2. Physicochemical characteristics of the sorption of 4-aminoquinoline derivatives from water-acetonitrile solutions on nonpolar sorbents

    NASA Astrophysics Data System (ADS)

    Paramonova, A. S.; Kurbatova, S. B.; Zemtsova, M. N.

    2014-02-01

    Regularities of the retention of certain 4-aminoquinoline derivatives in the conditions of the reversed phase type of high performance liquid chromatography (HPLC) on octadecyl silica (ODS) and hypercrosslinked polystyrene (HCLPS) are studied. The correlation between the structure of aminoquinolines and their chromatographic retention is demonstrated.

  3. DOPC liposomes doped with octadecylferulate

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Octadecyl ferulate, found in limit quantities in plants, is a natural phenolic derivative with the potential as a cosmeceautical, nutriceutical, and/or pharmaceutical ingredient because of its lipophilic and antioxidant properties. The current work demonstrates our ability to chemically synthesize a...

  4. Sorption of benzotriazoles under the conditions of RP HPLC

    NASA Astrophysics Data System (ADS)

    Dzhabieva, S. A.; Kurbatova, S. V.; Belousova, Z. P.

    2016-02-01

    The results of a chromatographic study of sorption of several benzotriazole derivatives on octadecyl silica gel were reported. The physicochemical and electronic parameters of benzotriazoles were calculated. The effect of the structure of analyte molecules and eluent composition on chromatographic retention of these substances was analyzed.

  5. Effects of nanoclay type on the physical and antimicrobial properties of PVOH-based nanocomposite films

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Polyvinyl alcohols-based nanocomposite films were fabricated with four types of montmorillonite (MMT) nanoclay, including 18-amino stearic acid (I.24TL), methyl, bis hydroxyethyl, octadecyl ammonium (I.34TCN), di-methyl, di-hydrogenated tallow ammonium/siloxane (I.44PSS) organically modified MMT, an...

  6. 21 CFR 178.3860 - Release agents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... agent, applied on the internal parts of reactors employed in the production of polyvinyl chloride and... per million. N,N′-Dioleoylethylenediamine For use only in polyvinyl chloride films in amounts such... of octadecyl isocyanate and vinyl alcohol/vinyl acetate copolymer; minimum average molecular...

  7. GdDOTAGA(C18)2: an efficient amphiphilic Gd(iii) chelate for the preparation of self-assembled high relaxivity MRI nanoprobes.

    PubMed

    Filippi, M; Remotti, D; Botta, M; Terreno, E; Tei, L

    2015-12-21

    A new amphiphilic GdDOTA-like complex functionalized with two octadecyl chains was synthesised and incorporated into the bilayer of liposomes and dendrimersomes. (1)H NMR relaxometric studies and in vivo MRI experiments on mice bearing a syngeneic melanoma tumour have shown a great improvement in performance.

  8. Effect of the physicochemical parameters of benzimidazole molecules on their retention by a nonpolar sorbent from an aqueous acetonitrile solution

    NASA Astrophysics Data System (ADS)

    Shafigulin, R. V.; Safonova, I. A.; Bulanova, A. V.

    2015-09-01

    The effect of the structure of benzimidazoles on their chromatographic retention on octadecyl silica gel from an aqueous acetonitrile eluent was studied. One- and many-parameter correlation equations were obtained by linear regression analysis, and their prognostic potential in determining the retention factors of benzimidazoles under study was analyzed.

  9. 21 CFR 178.3860 - Release agents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... agent, applied on the internal parts of reactors employed in the production of polyvinyl chloride and... per million. N,N′-Dioleoylethylenediamine For use only in polyvinyl chloride films in amounts such... of octadecyl isocyanate and vinyl alcohol/vinyl acetate copolymer; minimum average molecular...

  10. Formulation and evaluation of controlled release antibiotic biodegradable implants for post operative site delivery.

    PubMed

    Mathur, Vijay; Mudnaik, Rajesh; Barde, Laxmikant; Roy, Arghya; Shivhare, Umesh; Bhusari, Kishore

    2010-03-01

    Biodegradable implants of ciprofloxacin hydrochloride for post operative site delivery were prepared using glyceryl monostearate and different concentrations of polyethylene glycol (PEG 6000), glycerol and Tween 80 as erosion enhancers by compression and molding technique. Formulations were subjected to in vitro drug release by the USP dissolution method, while promising formulations were subjected to in vitro drug release by the agar gel method and also to stability studies. It was observed that glyceryl monostearate formed hydrophobic matrix and delayed the drug delivery. Antibiotic release profile was controlled by using different combinations of erosion enhancers. The formulation prepared by the compression method showed more delayed release compared to formulations prepared by the molding method.

  11. NO donors. Part 18: Bioactive metabolites of GTN and PETN--synthesis and vasorelaxant properties.

    PubMed

    Lange, Kathrin; Koenig, Andreas; Roegler, Carolin; Seeling, Andreas; Lehmann, Jochen

    2009-06-01

    The vasodilators glyceryl trinitrate (GTN) and pentaerythrityl tetranitrate (PETN) are supposed to be degraded in vivo to the lower nitrates PETriN, PEDN, PEMN, 1,2-GDN, 1,3-GDN, 1-GMN, and 2-GMN. We synthesized these bioactive metabolites as reference compounds for pharmacokinetic studies. The use of HPLC-methods for monitoring the stepwise reduction of PETN to lower nitrates and the syntheses of the glyceryl dinitrates proved advantageous. Furthermore, we measured the vasorelaxant properties of all metabolites by performing organ bath experiments with porcine pulmonary arteries. In general, the vasodilator potency increases with the number of nitrate moieties in the compound.

  12. In vitro drug release mechanism and drug loading studies of cubic phase gels.

    PubMed

    Lara, Marilisa G; Bentley, M Vitória L B; Collett, John H

    2005-04-11

    Glyceryl monooleate/water cubic phase systems were investigated as drug delivery systems, using salicylic acid as a model drug. The liquid crystalline phases formed by the glyceryl monooleate (GMO)/water systems were characterized by polarizing microscopy. In vitro drug release studies were performed and the influences of initial water content, swelling and drug loading on the drug release properties were evaluated. Water uptake followed second-order swelling kinetics. In vitro release profiles showed Fickian diffusion control and were independent on the initial water content and drug loading, suggesting GMO cubic phase gels suitability for use as drug delivery system.

  13. Investigations into the chemistry and insecticidal activity of euonymus europaeus seed oil and methanol extract

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Euonymus europaeus seeds and seed oil were investigated for their volatiles using GC-MS-FID, Headspace-SPME/GC-MS-FID, and derivative GC-MS-FID for their volatiles and HPLC-DAD-CAD/MS for their non-volatile compounds. The seeds contain about 30% of fatty oil, mainly glyceryl trioleate, small amounts...

  14. 21 CFR 172.515 - Synthetic flavoring substances and adjuvants.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...; pentyl alcohol. Amyl butyrate. α-Amylcinnamaldehyde. α-Amylcinnamaldehyde dimethyl acetal. α-Amylcinnamyl... creosote. Benzaldehyde dimethyl acetal. Benzaldehyde glyceryl acetal; 2-phenyl-m-dioxan-5-ol. Benzaldehyde.... Camphene; 2,2-dimethyl-3-methylenenorbornane. d-Camphor. Carvacrol; 2-p-cymenol. Carvacryl ethyl ether;...

  15. 21 CFR 175.210 - Acrylate ester copolymer coating.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ..., and methacrylic acid applied in emulsion form to molded virgin fiber and heat-cured to an insoluble... application of the emulsion may include substances named in this paragraph, in an amount not to exceed that... emulsion defoamer. Disodium hydrogen phosphate Do. Formaldehyde Glyceryl monostearate Methyl...

  16. Antihistamine Effect of a Pure Bioactive Compound Isolated from Slug (Diplosolenodes occidentalis) Material

    PubMed Central

    Jacob, AS; Simon, OR; Wheatle, D; Ruddock, P; McCook, K

    2014-01-01

    ABSTRACT Objective: Folklore claims of the therapeutic effect of garden slug (Diplosolenodes occidentalis) extract used to relieve bronchoconstriction in asthmatic individuals were never validated scientifically. The aim of this study was to isolate the pure bioactive compound from slug extract causing this effect. Methods: The crude ground material was prepared in ethanol and after filtration, separation by flash column chromatography method was done. The structure was elucidated by data from hydrogen and carbon nuclear magnetic resonance (NMR) profiles. The bioactive compound was assessed for dose dependent response effects on guinea pig tracheal smooth muscle pre-contracted with histamine. Receptor specificity studies were done by using HTMT dimaleate (H1 agonist). The type of antagonism was also identified. Results: The pure component isolated from garden slug material was identified by spectral studies as glyceryl trilinolenate. It caused dose-dependent relaxation in guinea pig tracheal smooth muscle strips pre-contracted with histamine, it acted via H1 type receptors and showed non-competitive antagonism. Conclusion: Glyceryl trilinolenate produced dose-dependent relaxation in tracheal smooth muscle strips in the presence of the agonist histamine. Glyceryl trilinolenate displayed non-competitive antagonism at H1 receptors in the trachea. This agent was able to alleviate bronchoconstriction in individuals presenting with atopic asthma in rural agricultural areas in Jamaica (verbal communications). It is possible that glyceryl trilinolenate can be used therapeutically to produce tracheal smooth muscle relaxation in individuals presenting with atopic asthma. PMID:25781274

  17. [Glycerol monothioglycolate eczema in a hairdresser. Persistence of the allergen in the hair several weeks after the application of a permanent].

    PubMed

    Reygagne, A; Garnier, R; Efthymiou, M L; Gervais, P

    1991-01-01

    Glyceryl thioglycolate has been used for a pair of years in acid permanent wave solutions. It appears to be much more sensitizing than ammonium thioglycolate which is usually the main component of this kind of cosmetics. A case of allergic contact dermatitis due to glyceryl thioglycolate is reported. The patient was a 43-year old woman with an eczematous dermatitis of both hands. She was a hairdresser and eczematous eruptions were strictly work-related. She had no direct contact with most cosmetics and only used tools (scissors, clips, pins, rollers, combs...) and hair spray. Patch testing was however done with the standard patch-test screening tray and all the products used in the shop. The only positive reaction was due to a permanent wave solution containing only glyceryl thioglycolate and glycerol. Positive patch-test reactions were also obtained with hair treated with the permanent wave solution and cut immediately or several weeks after the application of the preparation. This observation shows that glyceryl thioglycolate may be responsible for allergic contact dermatitis in hairdressers; it emphasizes the long remanence of the allergen in the hair that makes its eviction specially difficult. PMID:1834830

  18. [Isolation and identification of the secondary metabolites from Hydroclathrus clathratus].

    PubMed

    Xiaoling, Li; Shihai, Xu; Kai, Yang; Shuhao, Guo; Xiangchao, Zeng

    2004-04-01

    Four compounds have been isolated from the algae Hydroclathrus clathratus collected from the South China Sea. Their structures were established as 1-glyceryl hexadecanoate (1), eicosanamide, N-[2'-hydroxy-1'-(hydroxymethyl) pentadecyl] (2), uracil (3), mannitol (4) by MS, 1HNMR and 13CNMR. Compound 1, 2 and 3 were isolated from this algae for the first time.

  19. The pharmacology and therapeutic relevance of endocannabinoid derived cyclo-oxygenase (COX)-2 products.

    PubMed

    Woodward, D F; Carling, R W C; Cornell, C L; Fliri, H G; Martos, J L; Pettit, S N; Liang, Y; Wang, J W

    2008-10-01

    The discovery of anandamide and 2-arachidonyl glycerol (2-AG) as naturally occurring mammalian endocannabinoids has had important and wide-reaching therapeutic implications. This, to a large extent, ensues from the complexity of endocannabinoid biology. One facet of endocannabinoid biology now receiving increased attention is the cyclo-oxygenase-2 (COX-2) derived oxidation products. Anandamide and 2-AG are oxidized to a range of PG-ethanolamides and PG-glyceryl esters that closely approaches that of the prostaglandins (PGs) formed from arachidonic acid. The pharmacology of these electrochemically neutral PG-ethanolamides (prostamides) and PG-glyceryl esters appears to be unique. No meaningful interaction with natural or recombinant prostanoid receptors is apparent. Nevertheless, in certain cells and tissues, prostamides and PG-glyceryl esters exert potent effects. The recent discovery of selective antagonists for the putative prostamide receptor has been a major advance in further establishing prostamide pharmacology as an entity distinct from prostanoid receptors. Since discovery of the prototype prostamide antagonist (AGN 204396), rapid progress has been made. The latest prostamide antagonists (AGN 211334-6) are 100 times more potent than the prototype and are, therefore, sufficiently active to be used in living animal studies. These compounds will allow a full evaluation of the role of prostamides in health and disease. To date, the only therapeutic application for prostamides is in glaucoma. The prostamide analog, bimatoprost, being the most effective ocular hypotensive drug currently available. Interestingly, PGE(2)-glyceryl ester and its chemically stable analog PGE(2)-serinolamide also lower intraocular pressure in dogs. Nevertheless, the therapeutic future of PGE(2)-glyceryl ester is more likely to reside in inflammation. PMID:18700152

  20. Modification of the surfaces of Wyoming montmorillonite by the cationic surfactants alkyl trimethyl, dialkyl dimethyl, and trialkyl methyl ammonium bromides.

    PubMed

    Xi, Yunfei; Frost, Ray L; He, Hongping

    2007-01-01

    Surfaces of a Wyoming SWy-2 sodium montmorillonite were modified using microwave radiation through intercalation with the cationic surfactants octadecyl-trimethyl ammonium bromide, dimethyldioctadecylammonium bromide, and methyl-tri-octadecyl ammonium bromide by an ion exchange mechanism. Changes in the surfaces and structure were characterized using X-ray diffraction (XRD), thermal analysis (TG) and infrared (IR) spectroscopy. Different configurations of surfactants within montmorillonite interlayer are proposed based on d(001) basal spacings. A range of surfactant molecular environments within the surface-modified montmorillonite are proposed based upon their thermal decomposition. IR spectroscopy using a smart endurance single bounce diamond attenuated total reflection (ATR) cell has been used to study the changes in the spectra of CH asymmetric and symmetric stretching modes of the surfactants to provide more information of the surfactant molecular configurations.

  1. Synthesis of Discrete Alkyl-Silica Hybrid Nanowires and Their Assembly into Nanostructured Superhydrophobic Membranes.

    PubMed

    Yi, Deliang; Xu, Chenglong; Tang, Ruidie; Zhang, Xuehua; Caruso, Frank; Wang, Yajun

    2016-07-11

    We report the synthesis of highly flexible and mechanically robust hybrid silica nanowires (NWs) which can be used as novel building blocks to construct superhydrophobic functional materials with three-dimensional macroporous networks. The hybrid silica NWs, with an average diameter of 80 nm and tunable length of up to 12 μm, are prepared by anisotropic deposition of the hydrolyzed tetraethylorthosilicate in water/n-pentanol emulsions. A mechanistic investigation reveals that the trimethoxy(octadecyl)silane introduced to the water-oil interface in the synthesis plays key roles in stabilizing the water droplets to sub-100 nm and also growing a layer of octadecyl groups on the NW surface. This work opens a solution-based route for the one-pot preparation of monodisperse, hydrophobic silica NWs and represents an important step toward the bottom-up construction of 3D superhydrophobic materials and macroporous membranes. PMID:27278242

  2. Precipitation polymerization of hydrophobically modified polyelectrolyte poly(AA-co-ODA) in supercritical carbon dioxide and solution rheology properties

    NASA Astrophysics Data System (ADS)

    Zhang, Huaiping; Li, Wei; Cao, Qing; Chen, Mingcai

    2014-05-01

    Hydrophobically modified (HM) polyelectrolytes were prepared by using precipitation polymerization of acrylic acid (AA) and octadecyl acrylate (ODA) in various molar ratios in supercritical carbon dioxide. The product was obtained in the form of a white powder and the micrographs show aggregates of primary particles < 1 μm in size. The effects of polymer concentration, ODA content in polymer, surfactant, shear time, shear rate on the apparent viscosity were investigated. The reason leaded to a significant viscosity enhancement was discussed. Steady-state and oscillatory tests of solution were also investigated. Solution exhibited shear thinning behavior and thixotropy. Polymers contain octadecyl acrylate (3.4 mol%) at 0.2 g/dL behaved as high entanglement structures or association gels, since the modulus G' were being higher than G″ throughout the frequency range. The comparison of apparent and complex viscosities confirmed the association gel properties.

  3. Synthesis of Discrete Alkyl-Silica Hybrid Nanowires and Their Assembly into Nanostructured Superhydrophobic Membranes.

    PubMed

    Yi, Deliang; Xu, Chenglong; Tang, Ruidie; Zhang, Xuehua; Caruso, Frank; Wang, Yajun

    2016-07-11

    We report the synthesis of highly flexible and mechanically robust hybrid silica nanowires (NWs) which can be used as novel building blocks to construct superhydrophobic functional materials with three-dimensional macroporous networks. The hybrid silica NWs, with an average diameter of 80 nm and tunable length of up to 12 μm, are prepared by anisotropic deposition of the hydrolyzed tetraethylorthosilicate in water/n-pentanol emulsions. A mechanistic investigation reveals that the trimethoxy(octadecyl)silane introduced to the water-oil interface in the synthesis plays key roles in stabilizing the water droplets to sub-100 nm and also growing a layer of octadecyl groups on the NW surface. This work opens a solution-based route for the one-pot preparation of monodisperse, hydrophobic silica NWs and represents an important step toward the bottom-up construction of 3D superhydrophobic materials and macroporous membranes.

  4. Studies of the active substances in herbs used for hair treatment. III. Isolation of hair-regrowth substances from Polygara senega var. latifolia TORR. et GRAY.

    PubMed

    Ishida, H; Inaoka, Y; Okada, M; Fukushima, M; Fukazawa, H; Tsuji, K

    1999-11-01

    Four active principles, 1, 2, 3 and 4, were isolated from Polygara senega var. latifolia TORR. et GRAY by a combination of partition and column chromatography on silica gel and octadecyl silica gel (ODS), monitored by a hair-regrowth activity assay. Compounds 1, 2, 3 and 4 were identified as senegose A, senegin II, senegin III, and senegasaponin b by comparison of their spectral data with those of authentic samples. PMID:10598039

  5. Determination of phospholipids in milk using a new phosphodiester stationary phase by liquid chromatography-matrix assisted desorption ionization mass spectrometry.

    PubMed

    Walczak, Justyna; Pomastowski, Paweł; Bocian, Szymon; Buszewski, Bogusław

    2016-02-01

    A methodology employing high performance liquid chromatography coupled with matrix-assisted laser desorption and ionization time-of-flight mass spectrometry has been utilized to determine the quality of phospholipid classes. Home-made phosphoester chemically bonded stationary phase containing diol, phosphate and octadecyl groups (Diol-P-C18) has been employed in the separation of polar lipids from milk. Each phospholipid fraction was collected manually and identified by MALDI-TOF MS.

  6. Komrower Lecture. Adrenoleukodystrophy: natural history, treatment and outcome.

    PubMed

    Moser, H W

    1995-01-01

    Our laboratory has identified nearly 2000 patients with X-linked adrenoleukodystrophy (ALD) and conducted therapeutic trials in groups of patients who represent the major phenotypes. We report recent results of dietary therapy with a mixture of glyceryl trioleate and glyceryl trierucate oil, also referred to as Lorenzo's Oil, in the asymptomatic and childhood cerebral phenotypes. Fifty-three patients started this therapy at a mean age of 7.5 years at a time when they were free of neurological symptoms. Although analysis of data is hampered by the lack of a concurrent control group, follow-up studies after 39 months of therapy suggest that subsequent neurological involvement was less frequent and less severe than anticipated from historical controls. Retrospective analysis of the effect of the oil in patients with the severe childhood cerebral phenotype indicates that there was a slight but statistically significant slowing of clinical progression and delay of death.

  7. "Lorenzo's oil" therapy for X-linked adrenoleukodystrophy: rationale and current assessment of efficacy.

    PubMed

    Moser, Hugo W; Moser, Ann B; Hollandsworth, Kim; Brereton, N Hong; Raymond, Gerald V

    2007-09-01

    X-linked adrenoleukodystrophy (X-ALD) is a genetic disorder that damages the nervous system and is associated with the accumulation of saturated very long chain fatty acids (SVLCFA). Oral administration of "Lorenzo's oil" (LO), a 4:1 mixture of glyceryl trioleate and glyceryl trierucate, normalizes the SVLCFA levels in plasma, but its clinical efficacy and the clinical indications for its use have been controversial for more than 15 years. We review the biochemical effects of LO administration and the rationale for its use and present a current appraisal of its capacity to reduce the risk for the childhood cerebral phenotype when administered to asymptomatic boys and to slow progression of adrenomyeloneuropathy in patients without cerebral involvement. We also present current efforts to provide definitive evaluation of its clinical efficacy and discuss its possible role in the new therapeutic opportunities that will arise if newborn screening for X-ALD is validated and implemented.

  8. Recurrent myocardial infarction secondary to Prinzmetal’s variant angina

    PubMed Central

    Murdoch, Dale; Dhillon, Priyanka; Niranjan, Selvanayagam

    2015-01-01

    Prinzmetal’s variant angina describes chest pain secondary to reversible coronary artery vasospasm in the context of both diseased and non-diseased coronary arteries. Symptoms typically occur when the patient is at rest and are associated with transient ST-segment elevation. Acute episodes respond to glyceryl trinitrate, but myocardial infarction and other potentially fatal complications can occur, and long-term management can be challenging. Although it is not well understood, the underlying mechanism appears to involve a combination of endothelial damage and vasoactive mediators. In this case, a 35-year-old woman with myocardial infarction secondary to coronary artery vasospasm experienced recurrent chest pain. Coronary angiography revealed severe focal stenosis in the mid left anterior descending artery, which completely resolved after administration of intracoronary glyceryl trinitrate. The patient was discharged on nitrates and calcium channel blockers. The patient re-presented with another myocardial infarction, requiring up-titration of medical therapy. PMID:26034323

  9. [Studies on the constituents of trichosanthes root. III. Constituents of roots of Trichosanthes bracteata Voigt].

    PubMed

    Kitajima, J; Mukai, A; Masuda, Y; Tanaka, Y

    1989-04-01

    From the fresh roots of Trichosanthes bracteata Voigt., the following substances were identified: methyl palmitate, palmitic acid, suberic acid, alpha-spinasterol, stigmast-7-en-3 beta-ol, alpha-spinasterol 3-O-beta-D-glucopyranoside, stigmast-7-en-3 beta-ol 3-O-beta-D-glucopyranoside, glyceryl 1-palmitate, glyceryl 1-stearate, bryonolic acid, cucurbitacin B, isocucurbitacin B, 3-epi-isocucurbitacin B, 23,24-dihydrocucurbitacin B, 23,24-dihydroisocucurbitacin B, 23,24-dihydro-3-epi-isocucurbitacin B, cucurbitacin D, isocucurbitacin D and D-glucose. This root contains more than 6 times cucurbitacin of the root of T. kirilowii Maxim. var. japonicum Kitam. PMID:2760813

  10. 21 CFR 184.1901 - Triacetin.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Triacetin. 184.1901 Section 184.1901 Food and....1901 Triacetin. (a) Triacetin (C8 H14O6, CAS Reg. No. 102-76-1), also known as 1,2,3,-propanetriol triacetate or glyceryl triacetate, is the triester of glycerin and acetic acid. Triacetin can be prepared...

  11. Identification de filtres solaires dérivés de l'acide para-aminobenzoique par spectroscopie RMN et par CPG/SM.

    PubMed

    Masse, M O; Delporte, C; Bervelt, E

    2001-10-01

    Gas chromatography coupled with mass spectrometry and protonic nuclear magnetic resonance used directly or on fractions obtained by preparative thin layer chromatography, allow identification of the main molecule in commercial samples of PABA (Cas RN 150-13-0), PEG-25 PABA (Cas RN 116242-27-4), glyceryl PABA (Cas RN136-44-7), ethyl dihydroxypropyl PABA (Cas RN 58882-17-0) or octyl dimethyl PABA (Cas RN 21245-02-3).

  12. Anaesthetic management of coronary artery bypass grafting in a patient with central core disease and susceptibility to malignant hyperthermia on statin therapy.

    PubMed

    Johi, R R; Mills, R; Halsall, P J; Hopkins, P M

    2003-11-01

    Central core disease and malignant hyperthermia (MH) are both associated with mutations in the RYR1 gene. We report the anaesthetic management of one such patient presenting for coronary artery bypass grafting. Her medication included aspirin 75 mg, atorvastatin 20 mg, isosorbide mononitrate 60 mg, atenolol 25 mg and glyceryl trinitrite sublingual spray as required. The use of aprotinin, statins and moderate hypothermia in patients with central core disease and known susceptibility to MH has not been documented.

  13. Electrochemical characterization of bilayer lipid membrane-semiconductor junctions

    SciTech Connect

    Zhao, Xiao Kang; Baral, S.; Fendler, J.H. )

    1990-03-08

    Three different systems of glyceryl monooleate (GMO), bilayer lipid membrane (BLM) supported semiconductor particles have been prepared and characterized. A single composition of particulate semiconductor deposited only on one side of the BLM constituted system A, two different compositions of particulate semiconductors sequentially deposited on the same side of the BLM represented system B, and two different compositions of particulate semiconductors deposited on the opposite sides of the BLM made up system C.

  14. Effects of dietary carbohydrate on hepatic de novo lipogenesis in European seabass (Dicentrarchus labrax L.).

    PubMed

    Viegas, Ivan; Jarak, Ivana; Rito, João; Carvalho, Rui A; Metón, Isidoro; Pardal, Miguel A; Baanante, Isabel V; Jones, John G

    2016-07-01

    Farmed seabass have higher adiposity than their wild counterparts and this is often attributed to carbohydrate (CHO) feeding. Whether this reflects a reduction in fat oxidation, increased de novo lipogenesis (DNL), or both, is not known. To study the effects of high CHO diets on hepatic TG biosynthesis, hepatic TG deuterium ((2)H) enrichment was determined following 6 days in (2)H-enriched tank water for fish fed with a no-CHO control diet (CTRL), and diets with digestible starch (DS) and raw starch (RS). Hepatic fractional synthetic rates (FSRs, percent per day(-1)) were calculated for hepatic TG-glyceryl and FA moieties through (2)H NMR analysis. Glyceryl FSRs exceeded FA FSRs in all cases, indicating active cycling. DS fish did not show increased lipogenic potential compared to CTRL. RS fish had lower glyceryl FSRs compared with the other diets and negligible levels of FA FSRs despite similar hepatic TG levels to CTRL. DS-fed fish showed higher activity for enzymes that can provide NADPH for lipogenesis, relative to CTRL in the case of glucose-6-phosphate dehydrogenase (G6PDH) and relative to RS for both G6PDH and 6-phosphogluconate dehydrogenase. This approach indicated that elevated hepatic adiposity from DS feeding was not attributable to increased DNL. PMID:27247346

  15. Formulation and characterization of nanostructured lipid carrier of ubiquinone (Coenzyme Q10).

    PubMed

    Nanjwade, Basavaraj K; Kadam, Vikrant T; Manvi, F V

    2013-03-01

    Nanostructured lipid carriers (NLC) developed from mixtures of solid lipid and spatially incompatible liquid lipid by solvent diffusion method. This new type of lipid nanoparticles offers the advantage of improved drug loading capacity and release properties. In this study, Glyceryl distearate and Glyceryl behenate were chosen as solid lipid and Glyceryl triacetate used as liquid lipid. Ubidecarenone used as model drug was incorporated into the NLC. The influences of different type of solid lipid and liquid lipid concentration on physiochemical properties of the NLC were characterized. As a result, the drug encapsulation efficiencies were improved by adding the liquid lipid into the solid lipid of nanoparticles. NLC had higher encapsulation efficiency and drug release. In addition, in vivo study showed that the antioxidant activity of the Ubidecarenone (Co. Q10 NLC) was more effective than the Ubidecarenone (Coenzyme Q10) solution form on DPPH scavenging, anti-lipid peroxidation, lowers the effect of amnesia induced by scopolamine and increased bioavailability observed in Cmax, Tmax, and AUC. These results indicated that nanostructured lipid formulation of Ubiquinone (Coenzyme Q10) has more antioxidant activity than that of solution form and it can be used to reduce the oxidative stress and to increase the antioxidant enzyme activity in many neurodegenerative disorders such as Alzheimer's disease, Parkinson's disease etc. PMID:23621001

  16. In vitro study on sustained release capsule formulation of acetazolamide.

    PubMed

    Pandey, V P; Kannan, K; Manavalan, R; Desai, N

    2003-10-01

    In the present study formulation of sustained release capsule of acetazolamide 250 mg was tried using nonpareil seeds. Nonpareil seeds were coated with drug, polyvinylpyrrolidone, glyceryl monostearate, microcrystalline wax, and glyceryl distearate either individually or in combination to achieve sustained release capsule 250 mg. In successful formulation 20% drug coated pellets and 80% wax coated pellets were taken. Wax coated pellets for successful formulation contained coating of microcrystalline wax and glyceryl distearate on drug coated pellets of the same concentration of 1.6% w/w. Successful formulated sustained release capsule 250 mg of acetazolamide was compared in in vitro study with theoretical sustained release formulation suggested by wagner and one marketed sustained release capsule 250 mg. Formulated capsule showed result superior to or on par with marketed capsule. For successful formulation pellets were filled in '1' size hard gelatin capsule and stability study was carried out in hot air over at room temperature and 45 degrees C for 5 weeks. The formulation was found stable in respect of drug content and release rate.

  17. The development of Cutina lipogels and gel microemulsion for topical administration of fluconazole.

    PubMed

    El Laithy, H M; El-Shaboury, K M F

    2002-01-01

    The influence of the vehicle on the release and permeation of fluconazole, a topical antifungal drug dissolved in Jojoba oil was evaluated. Series of Cutina lipogels (Cutina CPA [cetyl palmitate], CBS [mixture of glyceryl stearate, cetearyl alcohol, cetyl palmitate, and cocoglycerides], MD [glyceryl stearate], and GMS [glyceryl monostearate]) in different concentrations as well as gel microemulsion were prepared. In-vitro drug release in Sorensen's citrate buffer (pH 5.5) and permeation through the excised skin of hairless mice, using a modified Franz diffusion cell, were performed. The rheological behavior and the apparent viscosity values for different gel bases were measured before and after storage under freezing conditions at -4 degrees C and were taken as measures for stability of network structure. Candida albicans was used as a model fungus to evaluate the antifungal activity of the best formula achieved. The results of in vitro drug release and its percutaneous absorption showed that the highest values from gel microemulsion were assured. The rheological behavior of the prepared systems showed pseudoplastic (shear-thinning) flow indicating structural breakdown of the existing intermolecular interactions between polymeric chains. Moreover, the stability study revealed no significant difference between viscosity before and after storage for different formulae except for CPA Cutina lipogel (using analysis of variance [ANOVA] test at level of significance.05). The antifungal activity of fluconazole showed the widest zone of inhibition with gel microemulsion. The gel microemulsion is an excellent vehicle for fluconazole topical drug delivery.

  18. Absorption enhancement of rectally infused cefoxitin by medium chain monoglycerides in conscious rats.

    PubMed

    Watanabe, Y; van Hoogdalem, E J; de Boer, A G; Breimer, D D

    1988-10-01

    The enhancing effect of the medium chain monoglycerides glyceryl-1-monoctanoate (GMO), glyceryl-1-monodecanoate (GMD), and glyceryl-1-monododecanoate (GMDD) on rectal absorption of the cephalosporin antibiotic cefoxitin [(6R,7S)-3-hydroxymethyl)-7-methoxy-8-oxo-7-[2-(2-thienyl)acetamido]-5- thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid carbamate (ester)] was investigated in unanesthetized rats. Rectal infusion of 3 mg of cefoxitin sodium without monoglyceride resulted in a mean bioavailability of 31 +/- 18% and a mean residence time (MRT) of 134 +/- 44 min. Coadministration with 53% (w/w) GMO significantly enhanced cefoxitin absorption, resulting in a mean bioavailability of 84 +/- 11% and a mean MRT of 75 +/- 8 min. In a lower concentration, GMD (13% w/w) also significantly promoted cefoxitin bioavailability to 68 +/- 14% and reduced MRT to 70 +/- 11 min. With GMDD only, a trend of increasing bioavailability with increasing monoglyceride concentration was observed, which may be explained by its limited aqueous solubility. Concerning the action of GMO and GMD, the longer monoglyceride is, in terms of effective concentration, more potent in enhancing the extent and rate of cefoxitin absorption. However, a further increase in chain length results in a loss of effect, indicating that the effect of monoglycerides on drug absorption may be determined by their intrinsic absorption enhancing action and solubility.

  19. Effect of alkyl chain length on the rotational diffusion of nonpolar and ionic solutes in 1-alkyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imides.

    PubMed

    Gangamallaiah, V; Dutt, G B

    2013-10-10

    Rotational diffusion of a nonpolar solute 9-phenylanthracene (9-PA) and a cationic solute rhodamine 110 (R110) has been examined in a series of 1-alkyl-3-methylimidazolium (alkyl = octyl, decyl, dodecyl, tetradecyl, hexadecyl, and octadecyl) bis(trifluoromethylsulfonyl)imides to understand the influence of alkyl chain length on solute rotation. In this study, reorientation times (τr) have been measured as a function of viscosity (η) by varying the temperature (T) of the solvents. These results have been analyzed using the Stokes-Einstein-Debye (SED) hydrodynamic theory along with the ones obtained for the same solutes in 1-alkyl-3-methylimidazolium (alkyl = methyl, ethyl, propyl, butyl, and hexyl) bis(trifluoromethylsulfonyl)imides (Gangamallaiah and Dutt, J. Phys. Chem. B 2012, 116, 12819-12825). It has been noticed that the data for 9-PA and R110 follows the relation τr = A(η/T)(n) with A being the ratio of hydrodynamic volume of the solute to the Boltzmann constant and n = 1 as envisaged by the SED theory. However, upon increasing the alkyl chain length from methyl to octadecyl significant deviations from the SED theory have been observed especially from the octyl derivative onward. From methyl to octadecyl derivatives, the value of A decreases by a factor of 3 for both the solutes and n by a factor of 1.4 and 1.6 for 9-PA and R110, respectively. These observations have been rationalized by taking into consideration the organized structure of the ionic liquids, whose influence appears to be pronounced when the number of carbon atoms in the alkyl chain attached to the imidazolium cation exceeds eight.

  20. Thermoreversible Gels Composed of Colloidal Silica Rods with Short-Range Attractions.

    PubMed

    Murphy, Ryan P; Hong, Kunlun; Wagner, Norman J

    2016-08-23

    Dynamic arrest transitions of colloidal suspensions containing nonspherical particles are of interest for the design and processing of various particle technologies. To better understand the effects of particle shape anisotropy and attraction strength on gel and glass formation, we present a colloidal model system of octadecyl-coated silica rods, termed as adhesive hard rods (AHR), which enables control of rod aspect ratio and temperature-dependent interactions. The aspect ratios of silica rods were controlled by varying the initial TEOS concentration following the work of Kuijk et al. (J. Am. Chem. Soc., 2011, 133, 2346-2349) and temperature-dependent attractions were introduced by coating the calcined silica rods with an octadecyl-brush and suspending in tetradecane. The rod length and aspect ratio were found to increase with TEOS concentration as expected, while other properties such as the rod diameter, coating coverage, density, and surface roughness were nearly independent of the aspect ratio. Ultrasmall angle X-ray scattering measurements revealed temperature-dependent attractions between octadecyl-coated silica rods in tetradecane, as characterized by a low-q upturn in the scattered intensity upon thermal quenching. Lastly, the rheology of a concentrated AHR suspension in tetradecane demonstrated thermoreversible gelation behavior, displaying a nearly 5 orders of magnitude change in the dynamic moduli as the temperature was cycled between 15 and 40 °C. The adhesive hard rod model system serves as a tunable platform to explore the combined influence of particle shape anisotropy and attraction strength on the dynamic arrest transitions in colloidal suspensions with thermoreversible, short-range attractions. PMID:27466883

  1. Studies of the active substances in herbs used for hair treatment. II. Isolation of hair regrowth substances, acetosyringone and polyporusterone A and B, from Polyporus umbellatus Fries.

    PubMed

    Ishida, H; Inaoka, Y; Shibatani, J; Fukushima, M; Tsuji, K

    1999-11-01

    Fractionation of the 50% ethanol extract of Polyporus umbellatus Fries by column chromatography on Amberlite XAD-2, silica gel, Sephadex LH-20 and octadecyl silica gel (ODS) (C18)) monitored by a hair-regrowth activity assay, afforded three active principles, 1, 2 and 3. The structures of 1, 2 and 3 were determined as acetosyringone, polyporusterone A, and polyporusterone B by comparison of their spectral data with that of authentic samples, respectively. The effects of several compounds related to acetosyringone, 3,4-dihydroxybenzaldehyde or polyporusterone A on hair regrowth were also investigated. PMID:10598026

  2. Retention of Proteins and Metalloproteins in Open Tubular Capillary Electrochromatography with Etched Chemically Modified Columns

    PubMed Central

    Pesek, Joseph J.; Matyska, Maria T.; Salgotra, Vasudha

    2010-01-01

    Etched chemically modified capillaries with two different bonded groups (pentyl and octadecyl) are compared for their migration behavior of several common proteins and metalloproteins as well as metalloproteinases. Migration times, efficiency and peak shape are evaluated over the pH range of 2.1 to 8.1 to determine any effects of the bonded group on the electrochromatographic behavior of these compounds. One goal was to determine if the relative hydrophobicity of the stationary phase has a significant effect on proteins in the open tubular format of capillary electrochromatography as it does in HPLC. Reproducibility of the migration times is also investigated. PMID:18850653

  3. Theory analysis of mass spectra of long-chain isocyanates.

    PubMed

    Liu, Dongliang; Hao, Ce; Zhang, Hua; Qiao, Weihong; Li, Zongshi; Yu, Guanghui; Yan, Kelu; Guo, Yuliang; Cheng, Lvbo

    2008-07-01

    Electron impact mass spectra of four long-chain isocyanates, lauryl isocyanate, tetradecyl isocyanate, hexadecyl isocyanate and octadecyl isocyanate, were obtained with a GCT high-resolution time-of-flight mass spectrometer. The four isocyanates studied gave a common base peak of m/z 99, which suggested the formation of a stable six-membered ring structure to decentralize the positive charge. Quantum-mechanical energy calculation justified that the six-membered ring base peak had the lowest energy. The positive charge assigned during the fragmentation of the radical cation, and the relative intensity of the fragment ion peaks, were explained by quantum-mechanical calculations as well.

  4. A Novel Class of Metal-Directed Supramolecular DNA-Delivery Systems

    SciTech Connect

    Cruz-Campa, I.; Arzola, A.; Santiago, L.; Parsons, J.G.; Varela-Ramirez, A.; Aguilera, R.J.; Noveron, J.C.

    2009-06-03

    The bis-complexes [Cu(L{sub dt}){sub 2}](OTf){sub 2} ( 1) and [Cu(L{sub ot}){sub 2}](OTf){sub 2} ( 2), where L{sub dt} = 1-dodecyl-1,4,7-triazacyclononane, L{sup ot} = 1-octadecyl-1,4,7-triazacyclononane and OTf = trifluoromethanesulfonate, formed a novel class of metallo-liposomes in water that transfect pEGFP-N1 plasmids into HEK 293-T cells at 38% and 4% efficiency, respectively.

  5. [Simultaneous separation of organic acid and organic salts by electrostatic ion chromatography].

    PubMed

    Shen, G J; Yang, R F; Yu, A M

    2001-09-01

    The electrostatic ion chromatographic column was prepared by coating conjugated acid salt micelles on the surface of octadecyl silica stationary phase. Pure water was used as mobile phase, and the conductance detector was connected on-line to electrostatic ion chromatograph. The conditions under which organic acid and organic salts were detected were studied. The mechanism for the above separation is discussed. Sodium benzoate and citric acid in Lichee drink were separated and determined. This method is rapid, simple with little interference and good reproducibility without any pollution since the mobile phase is water. This is an environmental friendly analytical method. PMID:12545440

  6. Functional double-shelled silicon nanocrystals for two-photon fluorescence cell imaging: spectral evolution and tuning

    NASA Astrophysics Data System (ADS)

    Chandra, Sourov; Ghosh, Batu; Beaune, Grégory; Nagarajan, Usharani; Yasui, Takao; Nakamura, Jin; Tsuruoka, Tohru; Baba, Yoshinobu; Shirahata, Naoto; Winnik, Françoise M.

    2016-04-01

    Functional near-IR (NIR) emitting nanoparticles (NPs) adapted for two-photon excitation fluorescence cell imaging were obtained starting from octadecyl-terminated silicon nanocrystals (ncSi-OD) of narrow photoluminescence (PL) spectra having no long emission tails, continuously tunable over the 700-1000 nm window, PL quantum yields exceeding 30%, and PL lifetimes of 300 μs or longer. These NPs, consisting of a Pluronic F127 shell and a core made up of assembled ncSi-OD kept apart by an octadecyl (OD) layer, were readily internalized into the cytosol, but not the nucleus, of NIH3T3 cells and were non-toxic. Asymmetrical field-flow fractionation (AF4) analysis was carried out to determine the size of the NPs in water. HiLyte Fluor 750 amine was linked via an amide link to NPs prepared with Pluronic-F127-COOH, as a first demonstration of functional NIR-emitting water dispersible ncSi-based nanoparticles.Functional near-IR (NIR) emitting nanoparticles (NPs) adapted for two-photon excitation fluorescence cell imaging were obtained starting from octadecyl-terminated silicon nanocrystals (ncSi-OD) of narrow photoluminescence (PL) spectra having no long emission tails, continuously tunable over the 700-1000 nm window, PL quantum yields exceeding 30%, and PL lifetimes of 300 μs or longer. These NPs, consisting of a Pluronic F127 shell and a core made up of assembled ncSi-OD kept apart by an octadecyl (OD) layer, were readily internalized into the cytosol, but not the nucleus, of NIH3T3 cells and were non-toxic. Asymmetrical field-flow fractionation (AF4) analysis was carried out to determine the size of the NPs in water. HiLyte Fluor 750 amine was linked via an amide link to NPs prepared with Pluronic-F127-COOH, as a first demonstration of functional NIR-emitting water dispersible ncSi-based nanoparticles. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01437b

  7. Constituents of Carapa guianensis Aubl. (Meliaceae).

    PubMed

    Qi, Shu-Hua; Wu, Da-Gang; Zhang, Si; Luo, Xiao-Dong

    2004-06-01

    Nine compounds were isolated from the EtOH extraction of the twig of Carapa guianensis Aubl. On the basis of spectroscopic methods, their structures were elucidated as 1,3-di-benzene carbon amine-2-octadecylic acid-glyceride (1), hexacosanoic acid-2,3-dihydroxy-glyceride (2), ursolic acid (3), naringenin (4), scopoletin (5), 3,4-dihydroxymethylbenzoate (6), 2,6-dihydroxymethylbenzoate (7), tetratriacontanoic acid (8), triacontanoic acid (9) respectively. Among them 1 was new, 2 was firstly isolated from nature, and 3-9 were obtained from this plant for the first time.

  8. Short-chain flavor ester synthesis in organic media by an E. coli whole-cell biocatalyst expressing a newly characterized heterologous lipase.

    PubMed

    Brault, Guillaume; Shareck, François; Hurtubise, Yves; Lépine, François; Doucet, Nicolas

    2014-01-01

    Short-chain aliphatic esters are small volatile molecules that produce fruity and pleasant aromas and flavors. Most of these esters are artificially produced or extracted from natural sources at high cost. It is, however, possible to 'naturally' produce these molecules using biocatalysts such as lipases and esterases. A gene coding for a newly uncovered lipase was isolated from a previous metagenomic study and cloned into E. coli BL21 (DE3) for overexpression using the pET16b plasmid. Using this recombinant strain as a whole-cell biocatalyst, short chain esters were efficiently synthesized by transesterification and esterification reactions in organic media. The recombinant lipase (LipIAF5-2) showed good affinity toward glyceryl trioctanoate and the highest conversion yields were obtained for the transesterification of glyceryl triacetate with methanol. Using a simple cetyl-trimethylammonium bromide pretreatment increased the synthetic activity by a six-fold factor and the whole-cell biocatalyst showed the highest activity at 40°C with a relatively high water content of 10% (w/w). The whole-cell biocatalyst showed excellent tolerance to alcohol and short-chain fatty acid denaturation. Substrate affinity was equally effective with all primary alcohols tested as acyl acceptors, with a slight preference for methanol. The best transesterification conversion of 50 mmol glyceryl triacetate into isoamyl acetate (banana fragrance) provided near 100% yield after 24 hours using 10% biocatalyst loading (w/w) in a fluidized bed reactor, allowing recycling of the biocatalyst up to five times. These results show promising potential for an industrial approach aimed at the biosynthesis of short-chain esters, namely for natural flavor and fragrance production in micro-aqueous media. PMID:24670408

  9. Endocannabinoids and their oxygenation by cyclo-oxygenases, lipoxygenases and other oxygenases.

    PubMed

    Urquhart, P; Nicolaou, A; Woodward, D F

    2015-04-01

    The naturally occurring mammalian endocannabinoids possess biological attributes that extend beyond interaction with cannabinoid receptors. These extended biological properties are the result of oxidative metabolism of the principal mammalian endocannabinoids arachidonoyl ethanolamide (anandamide; A-EA) and 2-arachidonoylglycerol (2-AG). Both endocannabinoids are oxidized by cyclo-oxygenase-2 (COX-2), but not by COX-1, to a series of prostaglandin derivatives (PGs) with quite different biological properties from those of the parent substrates. PG ethanolamides (prostamides, PG-EAs) and PG glyceryl esters (PG-Gs) are not only pharmacologically distinct from their parent endocannabinoids, they are distinct from the corresponding acidic PGs, and are differentiated from each other. Ethanolamides and glyceryl esters of the major prostanoids PGD2, PGE2, PGF2α, and PGI2 are formed by the various PG synthases, and thromboxane ethanolamides and glyceryl esters are not similarly produced. COX-2 is also of interest by virtue of its corollary central role in modulating endocannabinoid tone, providing a new therapeutic approach for treating pain and anxiety. Other major oxidative conversion pathways are provided for both A-EA and 2-AG by several lipoxygenases (LOXs), resulting in the formation of numerous hydroxyl metabolites. These do not necessarily represent inactivation pathways for endocannabinoids but may mimic or modulate the endocannabinoids or even display alternative pharmacology. Similarly, A-EA and 2-AG may be oxidized by P450 enzymes. Again a very diverse number of metabolites are formed, with either cannabinoid-like biological properties or an introduction of disparate pharmacology. The biological activity of epoxy and hydroxyl derivatives of the endocannabinoids remains to be fully elucidated. This review attempts to consolidate and compare the findings obtained to date in an increasingly important research area. This article is part of a Special Issue entitled

  10. Short-chain flavor ester synthesis in organic media by an E. coli whole-cell biocatalyst expressing a newly characterized heterologous lipase.

    PubMed

    Brault, Guillaume; Shareck, François; Hurtubise, Yves; Lépine, François; Doucet, Nicolas

    2014-01-01

    Short-chain aliphatic esters are small volatile molecules that produce fruity and pleasant aromas and flavors. Most of these esters are artificially produced or extracted from natural sources at high cost. It is, however, possible to 'naturally' produce these molecules using biocatalysts such as lipases and esterases. A gene coding for a newly uncovered lipase was isolated from a previous metagenomic study and cloned into E. coli BL21 (DE3) for overexpression using the pET16b plasmid. Using this recombinant strain as a whole-cell biocatalyst, short chain esters were efficiently synthesized by transesterification and esterification reactions in organic media. The recombinant lipase (LipIAF5-2) showed good affinity toward glyceryl trioctanoate and the highest conversion yields were obtained for the transesterification of glyceryl triacetate with methanol. Using a simple cetyl-trimethylammonium bromide pretreatment increased the synthetic activity by a six-fold factor and the whole-cell biocatalyst showed the highest activity at 40°C with a relatively high water content of 10% (w/w). The whole-cell biocatalyst showed excellent tolerance to alcohol and short-chain fatty acid denaturation. Substrate affinity was equally effective with all primary alcohols tested as acyl acceptors, with a slight preference for methanol. The best transesterification conversion of 50 mmol glyceryl triacetate into isoamyl acetate (banana fragrance) provided near 100% yield after 24 hours using 10% biocatalyst loading (w/w) in a fluidized bed reactor, allowing recycling of the biocatalyst up to five times. These results show promising potential for an industrial approach aimed at the biosynthesis of short-chain esters, namely for natural flavor and fragrance production in micro-aqueous media.

  11. Short-Chain Flavor Ester Synthesis in Organic Media by an E. coli Whole-Cell Biocatalyst Expressing a Newly Characterized Heterologous Lipase

    PubMed Central

    Brault, Guillaume; Shareck, François; Hurtubise, Yves; Lépine, François; Doucet, Nicolas

    2014-01-01

    Short-chain aliphatic esters are small volatile molecules that produce fruity and pleasant aromas and flavors. Most of these esters are artificially produced or extracted from natural sources at high cost. It is, however, possible to ‘naturally’ produce these molecules using biocatalysts such as lipases and esterases. A gene coding for a newly uncovered lipase was isolated from a previous metagenomic study and cloned into E. coli BL21 (DE3) for overexpression using the pET16b plasmid. Using this recombinant strain as a whole-cell biocatalyst, short chain esters were efficiently synthesized by transesterification and esterification reactions in organic media. The recombinant lipase (LipIAF5-2) showed good affinity toward glyceryl trioctanoate and the highest conversion yields were obtained for the transesterification of glyceryl triacetate with methanol. Using a simple cetyl-trimethylammonium bromide pretreatment increased the synthetic activity by a six-fold factor and the whole-cell biocatalyst showed the highest activity at 40°C with a relatively high water content of 10% (w/w). The whole-cell biocatalyst showed excellent tolerance to alcohol and short-chain fatty acid denaturation. Substrate affinity was equally effective with all primary alcohols tested as acyl acceptors, with a slight preference for methanol. The best transesterification conversion of 50 mmol glyceryl triacetate into isoamyl acetate (banana fragrance) provided near 100% yield after 24 hours using 10% biocatalyst loading (w/w) in a fluidized bed reactor, allowing recycling of the biocatalyst up to five times. These results show promising potential for an industrial approach aimed at the biosynthesis of short-chain esters, namely for natural flavor and fragrance production in micro-aqueous media. PMID:24670408

  12. Functional double-shelled silicon nanocrystals for two-photon fluorescence cell imaging: spectral evolution and tuning.

    PubMed

    Chandra, Sourov; Ghosh, Batu; Beaune, Grégory; Nagarajan, Usharani; Yasui, Takao; Nakamura, Jin; Tsuruoka, Tohru; Baba, Yoshinobu; Shirahata, Naoto; Winnik, Françoise M

    2016-04-28

    Functional near-IR (NIR) emitting nanoparticles (NPs) adapted for two-photon excitation fluorescence cell imaging were obtained starting from octadecyl-terminated silicon nanocrystals (ncSi-OD) of narrow photoluminescence (PL) spectra having no long emission tails, continuously tunable over the 700-1000 nm window, PL quantum yields exceeding 30%, and PL lifetimes of 300 μs or longer. These NPs, consisting of a Pluronic F127 shell and a core made up of assembled ncSi-OD kept apart by an octadecyl (OD) layer, were readily internalized into the cytosol, but not the nucleus, of NIH3T3 cells and were non-toxic. Asymmetrical field-flow fractionation (AF4) analysis was carried out to determine the size of the NPs in water. HiLyte Fluor 750 amine was linked via an amide link to NPs prepared with Pluronic-F127-COOH, as a first demonstration of functional NIR-emitting water dispersible ncSi-based nanoparticles. PMID:27076260

  13. Bonded-phase extraction column isolation of organic compounds in groundwater at a hazardous waste site

    USGS Publications Warehouse

    Rostad, C.E.; Pereira, W.E.; Ratcliff, S.M.

    1984-01-01

    A procedure for isolation of hazardous organic compounds from water for gas chromatography/mass spectrometry analysis Is presented and applied to creosote- and pentachlorophenol-contaminated groundwater resulting from wood-treatment processes. This simple procedure involved passing a 50-100-mL sample through a bonded-phase extraction column, eluting the trapped organic compounds from the column with 2-4 mL of solvent, and evaporating the sample to 100 ??L with a stream of dry nitrogen, after which the sample was ready for gas chromatography/mass spectrometry analysis. Representative compounds indicative of creosote contamination were used for recovery and precision studies from the cyclohexyl-bonded phase. Recovery of these compounds from n-octyl-, n-octadecyl-, cyclohexyl-, and phenyl-bonded phases was compared. The bonded phase that exhibited the best recovery and least bias toward acidic or basic cmpounds was the n-octadecyl phase. Detailed compound Identification Is given for compounds Isolated from creosote- and pentachlorophenol-contaminated groundwater using the cyclohexyl-bonded phase.

  14. Aging and nonlinear rheology of thermoreversible colloidal gels

    NASA Astrophysics Data System (ADS)

    Wagner, Norman; Gordon, Melissa; Kloxin, Christopher

    Colloidal dispersions are found in a wide variety of consumer products such as paint, food and pharmaceuticals. We investigate gel formation and aging in a thermoreverible gel consisting of octadecyl-coated silica nanoparticles suspended in n-tetradecane. In this system, the octadecyl brush can undergo a phase change allowing the attractions between particles to be tuned by temperature (1,2). By probing the system with steady shear and large amplitude oscillatory shear, we have studied the effect of thermal history and shear history on gel formation and gel mechanical properties during aging. Gels were formed by approaching a common temperature from above and below to determine a reference state from which creep tests were conducted. Creep ringing was observed as expected for the viscoelastic gel. The rheological aging is interpreted in terms of the gel microstructure formed with differing thermal and shear histories to determine how processing affects structure. Recently proposed scaling laws for the rheology and structure under flow are explored within the context of gel aging (3). Through rheological and microstructural measurements, we will further the understanding of gel formation and aging in this model system which may be applied to processing conditions in an industrial setting.

  15. Porous silica particles grafted with an amphiphilic side-chain polymer as a stationary phase in reversed-phase high-performance liquid chromatography.

    PubMed

    Shahruzzaman, Md; Takafuji, Makoto; Ihara, Hirotaka

    2015-07-01

    The amphiphilic polymer-grafted silica was newly prepared as a stationary phase in high-performance liquid chromatography. Poly(4-vinylpyridine) with a trimethoxysilyl group at one end was grafted onto porous silica particles and the pyridyl side chains were quaternized with 1-bromooctadecane. The obtained poly(octadecylpyridinium)-grafted silica was characterized by elemental analysis, diffuse reflectance infrared Fourier transform spectroscopy and Brunauer-Emmett-Teller analysis. The degree of quaternization of the pyridyl groups on the obtained stationary phase was estimated to be 70%. The selective retention behaviors of polycyclic aromatic hydrocarbons including some positional isomers were investigated using poly(octadecylpyridinium)-grafted silica as an amphiphilic polymer stationary phase in high-performance liquid chromatography and results were compared with commercially available polymeric octadecylated silica and phenyl-bonded silica columns. The results indicate that the selectivity toward polycyclic aromatic hydrocarbons exhibited by the amphiphilic polymer stationary phase is higher than the corresponding selectivity exhibited by a conventional phenyl-bonded silica column. However, compared with the polymeric octadecylated silica phase, the new stationary phase presents similar retention behavior for polycyclic aromatic hydrocarbons but different retention behavior particularly for positional isomers of disubstituted benzenes as the aggregation structure of amphiphilic polymers on the surface of silica substrate has been altered during mobile phase variation.

  16. Hydrolysis of triacetin catalyzed by immobilized lipases: effect of the immobilization protocol and experimental conditions on diacetin yield.

    PubMed

    Hernandez, Karel; Garcia-Verdugo, Eduardo; Porcar, Raul; Fernandez-Lafuente, Roberto

    2011-05-01

    The effect of the immobilization protocol and some experimental conditions (pH value and presence of acetonitrile) on the regioselective hydrolysis of triacetin to diacetin catalyzed by lipases has been studied. Lipase B from Candida antarctica (CALB) and lipase from Rhizomucor miehei (RML) were immobilized on Sepabeads (commercial available macroporous acrylic supports) activated with glutaraldehyde (covalent immobilization) or octadecyl groups (adsorption via interfacial activation). All the biocatalysts accumulated diacetin. Covalently immobilized RML was more active towards rac-methyl mandelate than the adsorbed RML. However, this covalent RML preparation presented the lowest activity towards triacetin. For this reason, this preparation was discarded as biocatalyst for this reaction. At pH 7, acyl migration occurred giving a mixture of 1,2 and 1,3 diacetin, but at pH 5.5, only 1,2 diacetin was produced. Yields were improved at acidic pH values and in the presence of 20% acetonitrile (to over 95%). RML immobilized on octadecyl Sepabeads was proposed as optimal preparation, mainly due to its higher specific activity. Each enzyme preparation presented very different properties. Moreover, changes in the reaction conditions affected the various immobilized enzymes in a different way.

  17. A continuous spectrophotometric assay that distinguishes between phospholipase A1 and A2 activities[S

    PubMed Central

    El Alaoui, Meddy; Soulère, Laurent; Noiriel, Alexandre; Popowycz, Florence; Khatib, Abdallah; Queneau, Yves; Abousalham, Abdelkarim

    2016-01-01

    A new spectrophotometric assay was developed to measure, continuously and specifically, phospholipase A1 (PLA1) or phospholipase A2 (PLA2) activities using synthetic glycerophosphatidylcholines (PCs) containing α-eleostearic acid, either at the sn-1 position [1-α-eleostearoyl-2-octadecyl-rac-glycero-3-phosphocholine (EOPC)] or at the sn-2 position [1-octadecyl-2-α-eleostearoyl-rac-glycero-3-phosphocholine (OEPC)]. The substrates were coated onto the wells of microtiter plates. A nonhydrolyzable ether bond, with a non-UV-absorbing alkyl chain, was introduced at the other sn position to prevent acyl chain migration during lipolysis. Upon enzyme action, α-eleostearic acid is liberated and then solubilized into the micellar phase. The PLA1 or PLA2 activity was measured by the increase in absorbance at 272 nm due to the transition of α-eleostearic acid from the adsorbed to the soluble state. EOPC and OEPC differentiate, with excellent accuracy, between PLA1 and PLA2 activity. Lecitase®, guinea pig pancreatic lipase-related protein 2 (known to be a PLA1 enzyme), bee venom PLA2, and porcine pancreatic PLA2 were all used to validate the assay. Compared with current assays used for continuously measuring PLA1 or PLA2 activities and/or their inhibitors, the development of this sensitive enzymatic method, using coated PC substrate analogs to natural lipids and based on the UV spectroscopic properties of α-eleostearic acid, is a significant improvement. PMID:27194811

  18. Inhibition of cell adhesion by a synthetic polymer adsorbed to glass shown under defined hydrodynamic stress.

    PubMed

    Owens, N F; Gingell, D; Rutter, P R

    1987-06-01

    A co-polymer with hydrophobic and hydrophilic segments was allowed to adsorb from aqueous solution onto glass previously made hydrophobic by derivatization with octadecyl dimethylchlorosilane. The polymer is thought to adsorb via its hydrophobic segments, leaving the hydrophilic segments free to extend into the water. After allowing cells to settle on the treated surface, the shear stress at the chamber wall required to remove red blood cells, Dictyostelium discoideum amoebae and Escherichia coli was determined in a calibrated laminar flow chamber. On octadecyl glass a shear stress of 2-3 Nm-2 evicts 50% of adherent red cells and E. coli. No D. discoideum amoebae could be removed at 5Nm-2. In striking contrast, the lowest experimentally obtainable shear stress of 0.03 Nm-2 removes 97.0-99.5% of cells of all three types from the polymer-treated surface, even after a cell residence time of 1 h without flow in the absence of free polymer. The minimum shear stress of 0.03Nm-2 corresponds to only approximately equal to 20 times the force of gravity on a red cell. The mechanism of action of the polymer and the implications of the results are discussed. PMID:3312253

  19. Sustained release of antibiotic from poly(2-hydroxyethyl methacrylate) to prevent blinding infections after cataract surgery

    PubMed Central

    Anderson, Erin M.; Noble, Misty L.; Garty, Shai; Ma, Hongyan; Bryers, James D.; Shen, Tueng T.; Ratner, Buddy D.

    2010-01-01

    Intraocular lens implantation after opacified natural lens removal is the primary treatment for cataracts in developed countries. Cataract surgery is generally considered safe, but entails significant risks in countries where sophisticated sterile operating theaters are not widely available. Post-operative infection (endophthalmitis) is a potential blinding complication. Infection often results from bacterial colonization of the new lens implant and subsequent antibiotic-tolerant biofilm formation. To combat this risk, we developed a polymeric hydrogel system that can deliver effective levels of antibiotic over an extended period of time within the globe of the eye. Norfloxacin™ antibiotic was loaded into cross-linked poly(2-hydroxyethyl methacrylate) (pHEMA) gels, which were subsequently surface-modified with octadecyl isocyanate to produce a hydrophobic rate-limiting barrier controlling norfloxacin release. Octadecyl surface modification was characterized using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). A 15-min modification leads to a uniform surface coating and near zero order release of norfloxacin from the matrix. Norfloxacin released from coated pHEMA kills Staphylococcus epidermidis in suspension and on a simulated medical implant surface. With these data, we demonstrate a new and effective system for sustained drug release from a hydrogel matrix with specific application for intraocular lens surgery. PMID:19631376

  20. Boundary lubrication of stainless steel and CoCrMo alloy based on phosphorous and boron compounds in oil-in-water emulsion

    NASA Astrophysics Data System (ADS)

    Yan, Jincan; Zeng, Xiangqiong; Ren, Tianhui; van der Heide, Emile

    2014-10-01

    Emulsion lubrication is widely used in metal forming operations and has potential applications in the biomedical field, yet the emulsion lubrication mechanism is not well understood. This work explores the possibilities of three different oil-in-water (O/W) emulsions containing dibutyl octadecylphosphoramidate (DBOP), 6-octadecyl-1,3,6,2-dioxazaborocan-2-ol calcium salt (ODOC) and 2-(4-dodecylphenoxy)-6-octadecyl-1,3,6,2-dioxazaborocane (DOB) to generate boundary films on stainless steel AISI 316 and CoCrMo alloy surfaces. Experimental results show lower friction values for the emulsions in combination with CoCrMo compared to AISI 316. The different performance of the additives is related to the composition of the adsorption and reaction film on the interacting surfaces, which was shown to be dependent on the active elements and molecular structure of the additives. The friction profile of the emulsions indicates that the emulsion appears to be broken during the rubbing process, then the additives adsorb onto the metal surface to form protecting boundary layers. The XPS analysis shows that for boundary lubrication conditions, the additive molecules in the emulsion first adsorb on the metal surface after the droplet is broken, and then decompose and react with the metal surface during the rubbing process to form stable lubricating films on the rubbed surfaces.

  1. Sustained release of antibiotic from poly(2-hydroxyethyl methacrylate) to prevent blinding infections after cataract surgery.

    PubMed

    Anderson, Erin M; Noble, Misty L; Garty, Shai; Ma, Hongyan; Bryers, James D; Shen, Tueng T; Ratner, Buddy D

    2009-10-01

    Intraocular lens implantation after opacified natural lens removal is the primary treatment for cataracts in developed countries. Cataract surgery is generally considered safe, but entails significant risks in countries where sophisticated sterile operating theaters are not widely available. Post-operative infection (endophthalmitis) is a potential blinding complication. Infection often results from bacterial colonization of the new lens implant and subsequent antibiotic-tolerant biofilm formation. To combat this risk, we developed a polymeric hydrogel system that can deliver effective levels of antibiotic over an extended period of time within the globe of the eye. Norfloxacin antibiotic was loaded into cross-linked poly(2-hydroxyethyl methacrylate) (pHEMA) gels, which were subsequently surface-modified with octadecyl isocyanate to produce a hydrophobic rate-limiting barrier controlling norfloxacin release. Octadecyl surface modification was characterized using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). A 15-min modification leads to a uniform surface coating and near zero order release of norfloxacin from the matrix. Norfloxacin released from coated pHEMA kills Staphylococcus epidermidis in suspension and on a simulated medical implant surface. With these data, we demonstrate a new and effective system for sustained drug release from a hydrogel matrix with specific application for intraocular lens surgery.

  2. High-resolution proton nuclear magnetic resonance characterization of seminolipid from bovine spermatozoa.

    PubMed

    Alvarez, J G; Storey, B T; Hemling, M L; Grob, R L

    1990-06-01

    The high-resolution one- and two-dimensional proton nuclear magnetic resonance (1H-NMR) characterization of seminolipid from bovine spermatozoa is presented. The 1H-NMR data was confirmed by gas-liquid chromatography-mass spectrometric analysis of the partially methylated alditol acetates of the sugar unit, mild alkaline methanolysis of the glyceryl ester, mobility on normal phase and diphasic thin-layer chromatography (HPTLC), and fast atom bombardment mass spectrometry (FAB-MS). The structure of the molecule corresponds to 1-O-hexadecyl-2-O-hexadecanoyl-3-O-beta-D-(3'-sulfo)-galactopyranosyl- sn-glycerol. PMID:2373957

  3. Studies on the endogenous phosphatides of mammalian pancreas and their hydrolysis by endogenous phospholipases - I. The lipids of dog pancreas and their in vitro hydrolysis, primed by trypsin, by phospholipase A2.

    PubMed

    Helmy, F M; Hack, M H

    1982-01-01

    1. The phosphoglyceride and sphingolipid content of dog pancreas has been determined and their in vitro response to the endogenous lipolytic enzymes, initiated by trypsin, at pH 7.4 was examined by TLC technology. 2. The glyceryl ether phosphatides were found to consist primarily of PE and PC, each with alkyl and alk-1-enyl components both of which were hydrolyzed to their respective 1-radyl lyso derivatives under the described incubation conditions. 3. A new TLC visualizing reaction for lipids, OSPAS, is described.

  4. Lipid nanoparticles for oral delivery of raloxifene: optimization, stability, in vivo evaluation and uptake mechanism.

    PubMed

    Ravi, Punna Rao; Aditya, N; Kathuria, Himanshu; Malekar, Srinivas; Vats, Rahul

    2014-05-01

    Raloxifene HCl (RLX) shows low oral bioavailability (<2%) in humans due to poor aqueous solubility and extensive (>90%) metabolism in gut. Lipid nanoparticles (SLN) with glyceryl tribehenate were designed to enhance drug's oral bioavailability. Box-Bhenken design was used to optimize manufacturing conditions. Optimized SLN had particle size of 167±3nm and high encapsulation efficiency (>92%). Oral bioavailability of RLX from SLN was improved by 3.24 folds compared to free RLX in female Wistar rats. Both clathrin and caveolae mediated endocytosis pathways were involved in the uptake of SLN. Lymphatic transport inhibitor, cycloheximide significantly reduced oral bioavailability of SLN. PMID:24378615

  5. High-resolution proton nuclear magnetic resonance characterization of seminolipid from bovine spermatozoa.

    PubMed

    Alvarez, J G; Storey, B T; Hemling, M L; Grob, R L

    1990-06-01

    The high-resolution one- and two-dimensional proton nuclear magnetic resonance (1H-NMR) characterization of seminolipid from bovine spermatozoa is presented. The 1H-NMR data was confirmed by gas-liquid chromatography-mass spectrometric analysis of the partially methylated alditol acetates of the sugar unit, mild alkaline methanolysis of the glyceryl ester, mobility on normal phase and diphasic thin-layer chromatography (HPTLC), and fast atom bombardment mass spectrometry (FAB-MS). The structure of the molecule corresponds to 1-O-hexadecyl-2-O-hexadecanoyl-3-O-beta-D-(3'-sulfo)-galactopyranosyl- sn-glycerol.

  6. Solvent-free mechanochemical glycosylation in ball mill.

    PubMed

    Tyagi, Mohit; Khurana, Darpan; Kartha, K P Ravindranathan

    2013-09-20

    Starting from acetobromosugars and an alcohol (alkyl/substituted alkyl/akenyl/alkynyl/glyceryl/cyclohexyl/steryl) various O-glycosides have been prepared mechanochemically under solvent-free conditions employing a planetary ball mill in the presence of metal carbonates (environmentally benign or otherwise) as promoters. The method was proven to be mild and efficient and applicable on preparative scale for the synthesis of various mono- and disaccharide glycosides. 4-Pentenyl glycoside so produced could, in four successive reactions in the same pot, be converted in high isolated yields into triazole-substituted pentyl glycoside that can find application in the area of medicinal chemistry.

  7. Adrenoleukodystrophy in a Chinese boy.

    PubMed

    Wong, V

    1992-07-01

    We report the first Chinese boy with adrenoleukodystrophy (ALD) who presented with hyperpigmentation, behavioral change and demyelination shown in magnetic resonance imaging of the brain. ALD was confirmed by the elevation of very long chain fatty acid in the serum and biochemical evidence of adrenal insufficiency. A trial of special diet with restriction of very long chain fatty acid and addition of glyceryl trierucate/glycerol trioleate oil (GTEO or Lorenzo's oil) failed to prevent clinical deterioration. The child had progressive visual loss and spastic tetraparesis despite dietary manipulation, adrenal steroid replacement and intravenous gammaglobulin treatment.

  8. Preventing neurodegeneration in the Drosophila mutant bubblegum.

    PubMed

    Min, K T; Benzer, S

    1999-06-18

    The Drosophila melanogaster recessive mutant bubblegum (bgm) exhibits adult neurodegeneration, with marked dilation of photoreceptor axons. The bubblegum mutant shows elevated levels of very long chain fatty acids (VLCFAs), as seen in the human disease adrenoleukodystrophy (ALD). In ALD, the excess can be lowered by dietary treatment with "Lorenzo's oil," a mixture of unsaturated fatty acids. Feeding the fly mutant one of the components, glyceryl trioleate oil, blocked the accumulation of excess VLCFAs as well as development of the pathology. Mutant flies thus provide a potential model system for studying mechanisms of neurodegenerative disease and screening drugs for treatment.

  9. Holographic interferometry of ultrasmall-pressure-induced curvature changes of bilayer lipid membranes

    SciTech Connect

    Picard, G.; Schneider-Henriquez, J.E.; Fendler, J.H. )

    1990-01-25

    Two-exposure interferometric holograms have been shown to sensitively report ultrasmall-pressure (10 natm)-induced curvature changes in glyceryl monooleate (GMO) bilayer lipid membranes (BLMs). The number of concentric fringes observed, and hence the lateral distance between the plane of the Teflon and the BLM, increased linearly with increasing transmembrane pressure and led to a value of 1.1 {plus minus} 0.05 dyn/cm for the surface tension of the BLM. BLMs with appreciable Plateau-Gibbs borders have been shown to undergo nonuniform deformation; the bilayer portion is distorted less than the surrounding Plateau-Gibbs border upon the application of a transmembrane pressure gradient.

  10. Nitroglycerin headache and nitroglycerin-induced primary headaches from 1846 and onwards: a historical overview and an update.

    PubMed

    Tfelt-Hansen, Peer C; Tfelt-Hansen, Jacob

    2009-03-01

    Nitroglycerin (NTG) (glyceryl trinitrate) was synthesized by the Italian chemist Ascanio Sobrero in Paris in 1846. A very unstable explosive, Alfred Nobel while working on explosives, combined it with Kiselguhr and patented it as dynamite in 1867. NTG was introduced in 1879 in medicine in the treatment of angina pectoris by the English doctor William Murrell. NTG-induced headache was quickly recognized as an important adverse event both in the industrial use of NTG, where it was used to produce dynamite, as well as in the use of NTG as drug. This review traces the evolution of our understanding of NTG headache.

  11. Development of endocannabinoid-based chemical probes for the study of cannabinoid receptors.

    PubMed

    Martín-Couce, Lidia; Martín-Fontecha, Mar; Capolicchio, Samanta; López-Rodríguez, María L; Ortega-Gutiérrez, Silvia

    2011-07-28

    We report the synthesis of new chemical probes (1a,b, 2a-c, 3a-c) based on the structure of the main endocannabinoids for their use in biological systems directly or via click chemistry. As proof of concept, 2-arachidonyl glyceryl ether based biotinylated 3b enables direct visualization of CB(1) receptor in cells. These results represent the starting point for the development of advanced small molecule chemical probes able to generate valuable information about the cannabinoid receptors.

  12. Potential use of nanostructured lipid carriers for topical delivery of flurbiprofen.

    PubMed

    González-Mira, E; Nikolić, S; García, M L; Egea, M A; Souto, E B; Calpena, A C

    2011-01-01

    The potential use of nanostructured lipid carriers (NLC) composed of a fatty acid [stearic acid (SA)] or a triglyceride (glyceryl behenate) as solid lipids, and a mixture of medium chain triglycerides and castor oil as liquid lipids, for skin administration of flurbiprofen (FB), has been explored. Two different optimized NLC formulations (FB-SANLC based on SA vs. FB-C888NLC based on glyceryl behenate), with respect to the morphometrical properties (particle size and polydispersity index) and the entrapment efficiency, were used in this study. The ex vivo permeation profiles of FB-C888NLC, FB-SANLC and conventional FB solution were evaluated using human skin. An improved FB permeation was observed when the drug was delivered by skin application of FB-C888NLC, attributed to the particle size and matrix crystallinity. The differential scanning calorimetry and X-ray diffraction studies suggested major polymorphic transitions in the lipid matrix of FB-C888NLC. A good correlation between polymorphic transitions and increased drug permeation was observed. However, both NLC dispersions showed a penetration-enhancing ratio (ER) higher than conventional FB solution. The in vitro and in vivo irritancy and local tolerability were assessed by running, respectively, the SKINTEX™ and Draize test. Both FB-C888NLC and FB-SANLC were classified as nonirritant.

  13. In vivo study of an instantly formed lipid-water cubic phase formulation for efficient topical delivery of aminolevulinic acid and methyl-aminolevulinate.

    PubMed

    Evenbratt, Hanne; Jonsson, Charlotte; Faergemann, Jan; Engström, Sven; Ericson, Marica B

    2013-08-16

    We demonstrate a rapidly formed cubic liquid crystalline phase, i.e. typically 1g cubic phase in less than 1 min confirmed by X-ray diffraction, consisting of an ether lipid, 1-glyceryl monooleyl ether (GME), an aprotic solvent (propylene glycol or pentane-1,5-diol) and water. The efficacy of the cubic formulation was tested in vivo by administrating formulations containing 3% (w/w) of the HCl salts of δ-aminolevulinic acid (ALA) or methylaminolevulinate (MAL) to hairless mice. The endogenous formation of protoporphyrin IX (PpIX) was monitored spectrophotometrically as a marker for cellular uptake of active compound. As reference, a commercial product containing 16% (w/w) MAL in an oil-in-water emulsion (Metvix(®)), and a cubic phase based on an ester lipid (glyceryl monooleate, GMO), previously shown to facilitate topical delivery of both ALA and MAL, were applied. It was found that in general the cubic phases gave rise to higher fluorescence levels than the mice exposed to the commercial product. The instantly formed cubic formulations based on GME demonstrated the same efficiency as the GMO based formulations. The results imply that instantly formed cubic formulations opens up new opportunities, particularly for transdermal drug delivery of substances subject to stability problems in, e.g. aqueous environments.

  14. Safety Evaluation of Polyethylene Glycol (PEG) Compounds for Cosmetic Use

    PubMed Central

    Shin, Chan Young; Kim, Kyu-Bong

    2015-01-01

    Polyethylene glycols (PEGs) are products of condensed ethylene oxide and water that can have various derivatives and functions. Since many PEG types are hydrophilic, they are favorably used as penetration enhancers, especially in topical dermatological preparations. PEGs, together with their typically nonionic derivatives, are broadly utilized in cosmetic products as surfactants, emulsifiers, cleansing agents, humectants, and skin conditioners. The compounds studied in this review include PEG/PPG-17/6 copolymer, PEG-20 glyceryl triisostearate, PEG-40 hydrogenated castor oil, and PEG-60 hydrogenated castor oil. Overall, much of the data available in this review are on PEGylated oils (PEG-40 and PEG-60 hydrogenated castor oils), which were recommended as safe for use in cosmetics up to 100% concentration. Currently, PEG-20 glyceryl triisostearate and PEGylated oils are considered safe for cosmetic use according to the results of relevant studies. Additionally, PEG/PPG-17/6 copolymer should be further studied to ensure its safety as a cosmetic ingredient. PMID:26191379

  15. Nanosized self-emulsifying lipid vesicles of diacylglycerol-PEG lipid conjugates: Biophysical characterization and inclusion of lipophilic dietary supplements

    SciTech Connect

    Koynova, Rumiana; Tihova, Mariana

    2010-04-12

    Hydrated diacylglycerol-PEG lipid conjugates, glyceryl dioleate-PEG12 (GDO-PEG12) and glyceryl dipalmitate-PEG23 (GDP-PEG23), spontaneously form uni- or oligolamellar liposomes in their liquid crystalline phase, in distinct difference from the PEGylated phospholipids which form micelles. GDP-PEG23 exhibits peculiar hysteretic phase behavior and can arrange into a long-living hexagonal phase at ambient and physiological temperatures. Liposomes of GDO-PEG12 and its mixture with soy lecithin exchange lipids with the membranes much more actively than common lecithin liposomes; such an active lipid exchange might facilitate the discharging of the liposome cargo upon uptake and internalization, and can thus be important in drug delivery applications. Diacylglycerol-PEG lipid liposome formulations can encapsulate up to 20-30 wt.% lipophilic dietary supplements such as fish oil, coenzyme Q10, and vitamins D and E. The encapsulation is feasible by way of dry mixing, avoiding the use of organic solvent.

  16. Production of bioadditives from glycerol esterification over zirconia supported heteropolyacids.

    PubMed

    Zhu, Shanhui; Zhu, Yulei; Gao, Xiaoqing; Mo, Tao; Zhu, Yifeng; Li, Yongwang

    2013-02-01

    The synthesis of bioadditives for biofuels from glycerol esterification with acetic acid was performed over zirconia supported heteropolyacids catalysts using H(4)SiW(12)O(40) (HSiW), H(3)PW(12)O(40) (HPW) and H(3)PMo(12)O(40) (HPMo) as active compounds. The as-prepared catalysts were characterized by N(2)-physisorption, XRD, Raman spectroscopy, NH(3)-TPD, FTIR of pyridine adsorption and H(2)O-TPD. Among the catalysts tested, HSiW/ZrO(2) achieved the best catalytic performance owing to the better combination of surface Brønsted acid sites and hydrothermal stability. A 93.6% combined selectivity of glyceryl diacetate and glyceryl triacetate with complete glycerol conversion was obtained at 120°C and 4h of reaction time in the presence of HSiW/ZrO(2). This catalyst also presented consistent activity for four consecutive reaction cycles, while HPW/ZrO(2) and HPMo/ZrO(2) exhibited distinct deactivation after reusability tests. In addition, HSiW/ZrO(2) can be resistant to the impurities present in bulk glycerol.

  17. Fatty Acid Ethyl Esters Are Less Toxic Than Their Parent Fatty Acids Generated during Acute Pancreatitis.

    PubMed

    Patel, Krutika; Durgampudi, Chandra; Noel, Pawan; Trivedi, Ram N; de Oliveira, Cristiane; Singh, Vijay P

    2016-04-01

    Although ethanol causes acute pancreatitis (AP) and lipolytic fatty acid (FA) generation worsens AP, the contribution of ethanol metabolites of FAs, ie, FA ethyl esters (FAEEs), to AP outcomes is unclear. Previously, pancreata of dying alcoholics and pancreatic necrosis in severe AP, respectively, showed high FAEEs and FAs, with oleic acid (OA) and its ethyl esters being the most abundant. We thus compared the toxicities of FAEEs and their parent FAs in severe AP. Pancreatic acini and peripheral blood mononuclear cells were exposed to FAs or FAEEs in vitro. The triglyceride of OA (i.e., glyceryl tri-oleate) or OAEE was injected into the pancreatic ducts of rats, and local and systemic severities were studied. Unsaturated FAs at equimolar concentrations to FAEEs induced a larger increase in cytosolic calcium, mitochondrial depolarization, and necro-apoptotic cell death. Glyceryl tri-oleate but not OAEE resulted in 70% mortality with increased serum OA, a severe inflammatory response, worse pancreatic necrosis, and multisystem organ failure. Our data show that FAs are more likely to worsen AP than FAEEs. Our observations correlate well with the high pancreatic FAEE concentrations in alcoholics without pancreatitis and high FA concentrations in pancreatic necrosis. Thus, conversion of FAs to FAEE may ameliorate AP in alcoholics.

  18. Modern Perspectives in the Treatment of Chronic Anal Fissures

    PubMed Central

    Bhardwaj, R; Parker, MC

    2007-01-01

    INTRODUCTION Anal fissures are commonly encountered in routine colorectal practice. Developments in the pharmacological understanding of the internal anal sphincter have resulted in more conservative approaches towards treatment. Simple measures are often effective for early fissures. Glyceryl trinitrate is well established as a first-line pharmacological therapy. The roles of diltiazem and botulinum, particularly as rescue therapy, are not well understood. Surgery has a defined role and should not be discounted completely. METHODS Data were obtained from Medline publications citing ‘anal fissure’. Manual cross-referencing of salient articles was conducted. We have sought to highlight various controversies in the management of anal fissures. FINDINGS Acute fissures may heal spontaneously, although simple conservative measures are sufficient. Idiopathic chronic anal fissures need careful evaluation to decide what therapy is suitable. Pharmacological agents such as glyceryl trinitrate (GTN), diltiazem and botulinum toxin have been subjected to most scrutiny. Though practices in the UK vary, GTN or diltiazem would be suitable as first-line therapy with botulinum toxin used as rescue treatment. Sphincterotomy is indicated for unhealed fissures; fissurectomy has been revisited and advancement flaps have a role in patients in whom sphincter division is not suitable. PMID:17688717

  19. Enhancing vitamin E bioaccessibility: factors impacting solubilization and hydrolysis of α-tocopherol acetate encapsulated in emulsion-based delivery systems.

    PubMed

    Yang, Ying; Decker, Eric Andrew; Xiao, Hang; McClements, David Julian

    2015-01-01

    Oil-soluble vitamins are often encapsulated within emulsion-based delivery systems to facilitate their incorporation into aqueous-based products. We have examined the influence of carrier oil type and simulated small intestinal fluid (SSIF) composition on the bioaccessibility of emulsified vitamin E using a gastrointestinal model. Oil-in-water emulsions containing vitamin E acetate were prepared using bile salts as emulsifier, and either long chain triacylglycerols (glyceryl trioleate, LCT) or medium chain triacylglycerols (glyceryl trioctanoate, MCT) as carrier oils. The addition of calcium (CaCl₂) to the SSIF increased the extent of lipid digestion in LCT-emulsions, but had little impact in MCT-emulsions. The bioaccessibility of vitamin E increased in the presence of calcium and phospholipids (DOPC) in LCT-emulsions, but decreased in MCT-emulsions. The highest bioaccessibility (≈66%) was achieved for LCT-emulsions when the SSIF contained both calcium and phospholipids. The conversion of α-tocopherol acetate to α-tocopherol after in vitro digestion was considerably higher for LCT-emulsions when calcium ions were present in the SSIF, but was not strongly affected by SSIF composition for MCT-emulsions. In general, this research provides important information about the factors influencing the bioaccessibility of emulsified vitamin E, which could be used to design more effective emulsion-based delivery systems for increasing the oral bioavailability of this important bioactive component.

  20. Lorenzo's oil inhibits ELOVL1 and lowers the level of sphingomyelin with a saturated very long-chain fatty acid.

    PubMed

    Sassa, Takayuki; Wakashima, Takeshi; Ohno, Yusuke; Kihara, Akio

    2014-03-01

    X-linked adrenoleukodystrophy (X-ALD) is a peroxisomal disorder caused by impaired degradation of very long-chain fatty acids (VLCFAs) due to mutations in the ABCD1 gene responsible for VLCFA transport into peroxisomes. Lorenzo's oil, a 4:1 mixture of glyceryl trioleate and glyceryl trierucate, has been used to reduce the saturated VLCFA level in the plasma of X-ALD patients; however, the mechanism by which this occurs remains elusive. We report the biochemical characterization of Lorenzo's oil activity toward elongation of very long-chain fatty acid (ELOVL) 1, the primary enzyme responsible for the synthesis of saturated and monounsaturated VLCFAs. Oleic and erucic acids inhibited ELOVL1, and, moreover, their 4:1 mixture (the FA composition of Lorenzo's oil) exhibited the most potent inhibitory activity. The kinetics analysis revealed that this was a mixed (not a competitive) inhibition. At the cellular level, treatment with the 4:1 mixture reduced the level of SM with a saturated VLCFA accompanied by an increased level of SM with a monounsaturated VLCFA, probably due to the incorporation of erucic acid into the FA elongation cycle. These results suggest that inhibition of ELOVL1 may be an underlying mechanism by which Lorenzo's oil exerts its action.

  1. Lorenzo's oil inhibits ELOVL1 and lowers the level of sphingomyelin with a saturated very long-chain fatty acid[S

    PubMed Central

    Sassa, Takayuki; Wakashima, Takeshi; Ohno, Yusuke; Kihara, Akio

    2014-01-01

    X-linked adrenoleukodystrophy (X-ALD) is a peroxisomal disorder caused by impaired degradation of very long-chain fatty acids (VLCFAs) due to mutations in the ABCD1 gene responsible for VLCFA transport into peroxisomes. Lorenzo's oil, a 4:1 mixture of glyceryl trioleate and glyceryl trierucate, has been used to reduce the saturated VLCFA level in the plasma of X-ALD patients; however, the mechanism by which this occurs remains elusive. We report the biochemical characterization of Lorenzo's oil activity toward elongation of very long-chain fatty acid (ELOVL) 1, the primary enzyme responsible for the synthesis of saturated and monounsaturated VLCFAs. Oleic and erucic acids inhibited ELOVL1, and, moreover, their 4:1 mixture (the FA composition of Lorenzo's oil) exhibited the most potent inhibitory activity. The kinetics analysis revealed that this was a mixed (not a competitive) inhibition. At the cellular level, treatment with the 4:1 mixture reduced the level of SM with a saturated VLCFA accompanied by an increased level of SM with a monounsaturated VLCFA, probably due to the incorporation of erucic acid into the FA elongation cycle. These results suggest that inhibition of ELOVL1 may be an underlying mechanism by which Lorenzo's oil exerts its action. PMID:24489110

  2. Dissimilarities between methylene blue and cyanide on relaxation and cyclic GMP formation in endothelium-intact intrapulmonary artery caused by nitrogen oxide-containing vasodilators and acetylcholine

    SciTech Connect

    Ignarro, L.J.; Harbison, R.G.; Wood, K.S.; Kadowitz, P.J.

    1986-01-01

    The objective of the present study was to ascertain whether cyanide shares the properties of methylene blue as a selective inhibitor of vascular smooth muscle relaxation elicited by agents that stimulate the formation of cyclic GMP. Experiments were performed with endothelium-intact rings prepared from bovine intrapulmonary artery. Methylene blue, a good inhibitor of soluble guanylate cyclase, antagonized both arterial relaxation and cyclic GMP accumulation in response to sodium nitroprusside, glyceryl trinitrate, S-nitroso-N-acetylpenicillamine and acetylcholine. In contrast, cyanide inhibited only the responses to sodium nitroprusside. Increasing concentrations of methylene blue depressed resting arterial levels of cyclic GMP and caused slowly developing but marked contractions whereas cyanide was without effect. Contractile responses to phenylephrine, potassium and U46619 were potentiated by methylene blue but not by cyanide. Preincubation of dilute solutions of cyanide containing sodium nitroprusside in oxygenated Krebs' buffer at 37 degrees C for 15 min before addition to bath chambers depressed relaxation and cyclic GMP accumulation caused by sodium nitroprusside markedly. Similar treatment of glyceryl trinitrate, however, failed to alter its effects in arterial rings. A chemical inactivation of sodium nitroprusside by cyanide appears to account for the specific inhibitory action of cyanide on arterial responses to sodium nitroprusside. This study indicates clearly that cyanide does not share the properties of methylene blue as an inhibitor of arterial relaxation elicited by vasodilators that stimulate cyclic GMP formation.

  3. Effect of Antiadherents on the Physical and Drug Release Properties of Acrylic Polymeric Films.

    PubMed

    Ammar, Hussein O; Ghorab, Mamdouh M; Felton, Linda A; Gad, Shadeed; Fouly, Aya A

    2016-06-01

    Antiadherents are used to decrease tackiness of a polymer coating during both processing and subsequent storage. Despite being a common excipient in coating formulae, antiadherents may affect mechanical properties of the coating film as well as drug release from film-coated tablets, but how could addition of antiadherents affect these properties and to what extent and is there a relation between the physical characteristics of the tablet coat and the drug release mechanisms? The aim of this study was to evaluate physical characteristics of films containing different amounts of the antiadherents talc, glyceryl monostearate, and PlasACRYL(TM) T20. Eudragit RL30D and Eudragit RS30D as sustained release polymers and Eudragit FS30D as a delayed release material were used. Polymer films were characterized by tensile testing, differential scanning calorimetry (DSC), microscopic examination, and water content as calculated from loss on drying. The effect of antiadherents on in vitro drug release for the model acetylsalicylic acid tablets coated with Eudragit FS30D was also determined. Increasing talc concentration was found to decrease the ability of the polymer films to resist mechanical stress. In contrast, glyceryl monostearate (GMS) and PlasACRYL produced more elastic films. Talc at concentrations higher than 25% caused negative effects, which make 25% concentration recommended to be used with acrylic polymers. All antiadherents delayed the drug release at all coating levels; hence, different tailoring of drug release may be achieved by adjusting antiadherent concentration with coating level. PMID:26314244

  4. Tackiness of acrylic and cellulosic polymer films used in the coating of solid dosage forms.

    PubMed

    Wesseling, M; Kuppler, F; Bodmeier, R

    1999-01-01

    The objective was to determine the tackiness of acrylic and cellulosic polymer films in order to make predictions on the tackiness (agglomeration) of coated dosage forms during coating and curing. Force-displacement curves of the detachment process of two polymeric films were used as a measure of tackiness. Various polymers (cellulosic (Aquacoat and acrylics (Eudragit RS 30D, L 30D, NE 30D)), plasticizers (triacetin, triethyl citrate, tributyl citrate, acetyltributyl citrate) and anti-tacking agents (talc and glyceryl monostearate) were investigated. The order of tackiness for films prepared from the different aqueous polymer dispersions was in order of Eudragit NE 30D > RS 30D > RL 30D > Aquacoat. The tackiness increased with increasing plasticizer concentration due to the softening of the polymer. A correlation between the minimum film formation temperature and the tackiness was observed, however, no correlation between the tackiness and the lipophilicity of the plasticizer was seen. Talc and glyceryl monostearate (GMS) reduced the tackiness of the films significantly, with GMS being effective at much lower concentrations. Curing of Eudragit RS 30D-coated theophylline beads at temperatures higher than 40 degrees C in an irreversible agglomeration of the beads and damage of the coating upon separation of the beads. This resulted in a faster release than with uncured beads. Blending the beads with talc just prior to the curing step eliminated the agglomeration and therefore film damage, even at a curing temperature of 60 degrees C. PMID:10234529

  5. Oral L-arginine improves endothelium-dependent dilation in hypercholesterolemic young adults.

    PubMed Central

    Clarkson, P; Adams, M R; Powe, A J; Donald, A E; McCredie, R; Robinson, J; McCarthy, S N; Keech, A; Celermajer, D S; Deanfield, J E

    1996-01-01

    In hypercholesterolemic rabbits, oral L-arginine (the substrate for endothelium derived nitric oxide) attenuates endothelial dysfunction and atheroma formation, but the effect in hypercholesterolemic humans is unknown. Using high resolution external ultrasound, we studied arterial physiology in 27 hypercholesterolemic subjects aged 29+/-5 (19-40) years, with known endothelial dysfunction and LDL-cholesterol levels of 238+/-43 mg/dl. Each subject was studied before and after 4 wk of L-arginine (7 grams x 3/day) or placebo powder, with 4 wk washout, in a randomized double-blind crossover study. Brachial artery diameter was measured at rest, during increased flow (causing endothelium-dependent dilation, EDD) and after sublingual glyceryl trinitrate (causing endothelium-independent dilation). After oral L-arginine, plasma L-arginine levels rose from 115+/-103 to 231+/-125 micromol/liter (P<0.001), and EDD improved from 1.7+/-1.3 to 5.6+/-3.0% (P<0.001). In contrast there was no significant change in response to glyceryl trinitrate. After placebo there were no changes in endothelium-dependent or independent vascular responses. Lipid levels were unchanged after L-arginine and placebo. Dietary supplementation with L-arginine significantly improves EDD in hypercholesterolemic young adults, and this may impact favorably on the atherogenic process. PMID:8621785

  6. Tackiness of acrylic and cellulosic polymer films used in the coating of solid dosage forms.

    PubMed

    Wesseling, M; Kuppler, F; Bodmeier, R

    1999-01-01

    The objective was to determine the tackiness of acrylic and cellulosic polymer films in order to make predictions on the tackiness (agglomeration) of coated dosage forms during coating and curing. Force-displacement curves of the detachment process of two polymeric films were used as a measure of tackiness. Various polymers (cellulosic (Aquacoat and acrylics (Eudragit RS 30D, L 30D, NE 30D)), plasticizers (triacetin, triethyl citrate, tributyl citrate, acetyltributyl citrate) and anti-tacking agents (talc and glyceryl monostearate) were investigated. The order of tackiness for films prepared from the different aqueous polymer dispersions was in order of Eudragit NE 30D > RS 30D > RL 30D > Aquacoat. The tackiness increased with increasing plasticizer concentration due to the softening of the polymer. A correlation between the minimum film formation temperature and the tackiness was observed, however, no correlation between the tackiness and the lipophilicity of the plasticizer was seen. Talc and glyceryl monostearate (GMS) reduced the tackiness of the films significantly, with GMS being effective at much lower concentrations. Curing of Eudragit RS 30D-coated theophylline beads at temperatures higher than 40 degrees C in an irreversible agglomeration of the beads and damage of the coating upon separation of the beads. This resulted in a faster release than with uncured beads. Blending the beads with talc just prior to the curing step eliminated the agglomeration and therefore film damage, even at a curing temperature of 60 degrees C.

  7. Effect of Antiadherents on the Physical and Drug Release Properties of Acrylic Polymeric Films.

    PubMed

    Ammar, Hussein O; Ghorab, Mamdouh M; Felton, Linda A; Gad, Shadeed; Fouly, Aya A

    2016-06-01

    Antiadherents are used to decrease tackiness of a polymer coating during both processing and subsequent storage. Despite being a common excipient in coating formulae, antiadherents may affect mechanical properties of the coating film as well as drug release from film-coated tablets, but how could addition of antiadherents affect these properties and to what extent and is there a relation between the physical characteristics of the tablet coat and the drug release mechanisms? The aim of this study was to evaluate physical characteristics of films containing different amounts of the antiadherents talc, glyceryl monostearate, and PlasACRYL(TM) T20. Eudragit RL30D and Eudragit RS30D as sustained release polymers and Eudragit FS30D as a delayed release material were used. Polymer films were characterized by tensile testing, differential scanning calorimetry (DSC), microscopic examination, and water content as calculated from loss on drying. The effect of antiadherents on in vitro drug release for the model acetylsalicylic acid tablets coated with Eudragit FS30D was also determined. Increasing talc concentration was found to decrease the ability of the polymer films to resist mechanical stress. In contrast, glyceryl monostearate (GMS) and PlasACRYL produced more elastic films. Talc at concentrations higher than 25% caused negative effects, which make 25% concentration recommended to be used with acrylic polymers. All antiadherents delayed the drug release at all coating levels; hence, different tailoring of drug release may be achieved by adjusting antiadherent concentration with coating level.

  8. A simple strategy to monitor lipase activity using liquid crystal-based sensors.

    PubMed

    Hu, Qiong-Zheng; Jang, Chang-Hyun

    2012-09-15

    In this study, we developed a simple label-free technique for monitoring the enzymatic activity of lipase using liquid crystal (LC)-based sensors. The optical response of LCs changed from a bright to dark appearance when an aqueous solution of lipase was in contact with a nematic LC, 4-cyano-4'-pentylbiphenyl (5CB), that was doped with glyceryl trioleate, which is a glyceride that can be enzymatically hydrolyzed by lipase. Since the oleic acid released from the enzymatic reaction could spontaneously form a self-assembled monolayer at the aqueous/LC interface due to its amphiphilic property, the orientation of the LCs transited from a planar to homeotropic state, which induced a change in the optical response of the LCs. We did not observe a bright-to-dark shift in the optical appearance of LCs when pure 5CB was immersed into the lipase solution. Moreover, we further confirmed the specificity of the enzymatic reaction by transferring an aqueous buffer solution not containing an analyte, or with bovine serum albumin (BSA) or trypsin onto the interface of aqueous solutions and the glyceryl trioleate-doped 5CB, which did not produce any distinctive contrast in the optical appearance. These results suggest the feasibility of measuring the enzymatic activity of lipase using the LC-based sensing technique. Furthermore, our strategy could also be used for the preparation of a self-assembled monolayer of carboxylates at the aqueous/LC interface. PMID:22967518

  9. In vivo study of an instantly formed lipid-water cubic phase formulation for efficient topical delivery of aminolevulinic acid and methyl-aminolevulinate.

    PubMed

    Evenbratt, Hanne; Jonsson, Charlotte; Faergemann, Jan; Engström, Sven; Ericson, Marica B

    2013-08-16

    We demonstrate a rapidly formed cubic liquid crystalline phase, i.e. typically 1g cubic phase in less than 1 min confirmed by X-ray diffraction, consisting of an ether lipid, 1-glyceryl monooleyl ether (GME), an aprotic solvent (propylene glycol or pentane-1,5-diol) and water. The efficacy of the cubic formulation was tested in vivo by administrating formulations containing 3% (w/w) of the HCl salts of δ-aminolevulinic acid (ALA) or methylaminolevulinate (MAL) to hairless mice. The endogenous formation of protoporphyrin IX (PpIX) was monitored spectrophotometrically as a marker for cellular uptake of active compound. As reference, a commercial product containing 16% (w/w) MAL in an oil-in-water emulsion (Metvix(®)), and a cubic phase based on an ester lipid (glyceryl monooleate, GMO), previously shown to facilitate topical delivery of both ALA and MAL, were applied. It was found that in general the cubic phases gave rise to higher fluorescence levels than the mice exposed to the commercial product. The instantly formed cubic formulations based on GME demonstrated the same efficiency as the GMO based formulations. The results imply that instantly formed cubic formulations opens up new opportunities, particularly for transdermal drug delivery of substances subject to stability problems in, e.g. aqueous environments. PMID:23727140

  10. Brain activations in the premonitory phase of nitroglycerin-triggered migraine attacks.

    PubMed

    Maniyar, Farooq Husain; Sprenger, Till; Monteith, Teshamae; Schankin, Christoph; Goadsby, Peter James

    2014-01-01

    Our aim was identify brain areas involved in the premonitory phase of migraine using functional neuroimaging. To this end, we performed positron emission tomography scans with H2(15)O to measure cerebral blood flow as a marker of neuronal activity. We conducted positron emission tomography scans at baseline, in the premonitory phase without pain and during migraine headache in eight patients. We used glyceryl trinitrate (nitroglycerin) to trigger premonitory symptoms and migraine headache in patients with episodic migraine without aura who habitually experienced premonitory symptoms during spontaneous attacks. The main outcome was comparing the first premonitory scans in all patients to baseline scans in all patients. We found activations in the posterolateral hypothalamus, midbrain tegmental area, periaqueductal grey, dorsal pons and various cortical areas including occipital, temporal and prefrontal cortex. Brain activations, in particular of the hypothalamus, seen in the premonitory phase of glyceryl trinitrate-triggered migraine attacks can explain many of the premonitory symptoms and may provide some insight into why migraine is commonly activated by a change in homeostasis.

  11. Release of Methane from Bering Sea Sediments During the Last Glacial Period

    SciTech Connect

    Mea Cook; Lloyd Keigwin

    2007-11-30

    Several lines of evidence suggest that during times of elevated methane flux the sulfate-methane transition zone (SMTZ) was positioned near the sediment-water interface. We studied two cores (from 700 m and 1457 m water depth) from the Umnak Plateau region. Anomalously low d13C and high d18O in benthic and planktonic foraminifera in these cores are the consequence of diagenetic overgrowths of authigenic carbonates. There are multiple layers of authigenic-carbonate-rich sediment in these cores, and the stable isotope compositions of the carbonates are consistent with those formed during anaerobic oxidation of methane (AOM). The carbonate-rich layers are associated with biomarkers produced by methane-oxidizing archaea, archaeol and glyceryl dibiphytanyl glyceryl tetraether (GDGT). The d13C of the archaeol and certain GDGTs are isotopically depleted. These carbonate- and AOM-biomarker-rich layers were emplaced in the SMTZ during episodes when there was a high flux of methane or methane-rich fluids upward in the sediment column. The sediment methane in the Umnak Plateau region appears to have been very dynamic during the glacial period, and interacted with the ocean-atmosphere system at millennial time scales. The upper-most carbonate-rich layers are in radiocarbon-dated sediment deposited during interstitials 2 and 3, 28-20 ka, and may be associated with the climate warming during this time.

  12. Flavonolignans and other constituents from Lepidium meyenii with activities in anti-inflammation and human cancer cell lines.

    PubMed

    Bai, Naisheng; He, Kan; Roller, Marc; Lai, Ching-Shu; Bai, Lu; Pan, Min-Hsiung

    2015-03-11

    From the roots of Lepidium meyenii Walpers (Brassicaceae) have been isolated and identified 2 flavonolignans, tricin 4'-O-[threo-β-guaiacyl-(7″-O-methyl)-glyceryl] ether (1) and tricin 4'-O-(erythro-β-guaiacyl-glyceryl) ether (2), along with 11 other known compounds, tricin (3), pinoresinol (4), 4-hydroxycinnamic acid (5), guanosine (6), glucotropaeolin (7), desulfoglucotropaeolin (8), 3-hydroxybenzylisothiocyanate (9), malic acid benzoate (10), 5-(hydroxymethyl)-2-furfural (11), d-phenylalanine (12), and vanillic acid 4-O-β-d-glucoside (13). Structures were elucidated on the basis of NMR and MS data. Some isolates and previously isolated lepidiline B (14) were tested for cytotoxicity in a small panel of human cancer cell lines (Hep G2, COLO 205, and HL-60) and for anti-inflammatory activities in LPS-treated RAW 264.7 macrophage. Among them, compounds 1 and 14 were modestly active for inhibiting nitrite production in macrophage. Compounds 1, 14, and 3 were demonstrated to be selectively active against HL-60 cells with IC50 values of 40.4, 52.0, and 52.1 μM, respectively. PMID:25667964

  13. Induction of primary, antiviral cytotoxic, and proliferative responses with antigens administered via dendritic cells.

    PubMed Central

    Nair, S; Babu, J S; Dunham, R G; Kanda, P; Burke, R L; Rouse, B T

    1993-01-01

    Cytotoxic T lymphocytes (CTL) play an essential role in recovery from viral infections, but induction of CTL responses with nonreplicating antigens is difficult to achieve. Exogenous antigens, such as viral proteins and peptides, normally induce CD4+ T-cell responses unless appropriately delivered to the major histocompatibility complex class I antigen presentation pathway. In vitro studies performed to address this issue revealed a similar scenario, and primary CTL induction with nonreplicating antigens has rarely been reported. This study demonstrated primary antiviral CTL induction in vitro with exogenous antigens delivered in vivo to dendritic cells. This study also evaluated the efficacy of glycoprotein B peptide (free or encapsulated in liposomes), peptide-tripalmitoyl-S-glyceryl cysteinyl conjugate (acylpeptide), and glycoprotein B protein encapsulated in pH-sensitive liposomes as antigen delivery vehicles. Our results show that higher levels of cytotoxicity against herpes simplex virus type 1 resulted from exposure of dendritic cells to peptide-tripalmitoyl-S-glyceryl cysteinyl in liposomes. Macrophages treated in a similar manner were not effective stimulators for primary CTL induction. Our data have relevance to the understanding of mechanisms of antigen processing and presentation and the design of antiviral vaccines. PMID:8510217

  14. Mycosporine-like Amino Acids and Other Phytochemicals Directly Detected by High-Resolution NMR on Klamath (Aphanizomenon flos-aquae) Blue-Green Algae.

    PubMed

    Righi, Valeria; Parenti, Francesca; Schenetti, Luisa; Mucci, Adele

    2016-09-01

    This study describes for the first time the use of high-resolution nuclear magnetic resonance (NMR) on Klamath (Aphanizomenon flos-aquae, AFA) blue-green algae directly on powder suspension. These algae are considered to be a "superfood", due to their complete nutritional profile that has proved to have important therapeutic effects. The main advantage of NMR spectroscopy is that it permits the detection of a number of metabolites all at once. The Klamath alga metabolome was revealed to be quite complex, and the most peculiar phytochemicals that can be detected directly on algae by NMR are mycosporine-like amino acids (porphyra-334, P334; shinorine, Shi) and low molecular weight glycosides (glyceryl β-d-galactopyranoside, GalpG; glyceryl 6-amino-6-deoxy-α-d-glucopyranoside, ADG), all compounds with a high nutraceutical value. The presence of cis-3,4-DhLys was revealed for the first time. This molecule could be involved in the anticancer properties ascribed to AFA.

  15. Mycosporine-like Amino Acids and Other Phytochemicals Directly Detected by High-Resolution NMR on Klamath (Aphanizomenon flos-aquae) Blue-Green Algae.

    PubMed

    Righi, Valeria; Parenti, Francesca; Schenetti, Luisa; Mucci, Adele

    2016-09-01

    This study describes for the first time the use of high-resolution nuclear magnetic resonance (NMR) on Klamath (Aphanizomenon flos-aquae, AFA) blue-green algae directly on powder suspension. These algae are considered to be a "superfood", due to their complete nutritional profile that has proved to have important therapeutic effects. The main advantage of NMR spectroscopy is that it permits the detection of a number of metabolites all at once. The Klamath alga metabolome was revealed to be quite complex, and the most peculiar phytochemicals that can be detected directly on algae by NMR are mycosporine-like amino acids (porphyra-334, P334; shinorine, Shi) and low molecular weight glycosides (glyceryl β-d-galactopyranoside, GalpG; glyceryl 6-amino-6-deoxy-α-d-glucopyranoside, ADG), all compounds with a high nutraceutical value. The presence of cis-3,4-DhLys was revealed for the first time. This molecule could be involved in the anticancer properties ascribed to AFA. PMID:27537083

  16. In vitro peptide release from liquid crystalline buccal delivery systems.

    PubMed

    Lee, J; Kellaway, I W

    2000-02-15

    Swelling and [D-Ala(2), D-Leu(5)]enkephalin (DADLE) release from the lamellar and cubic liquid crystalline phases of glyceryl monooleate (GMO) were studied using two in vitro methods, a total immersion method and a Franz cell method. The swelling of the lamellar phase and glyceryl monooleate (0% w/w water content) and DADLE release from the liquid crystalline phases were temperature dependent. The swelling ratio was greater at 20 degrees C than 37 degrees C while DADLE release increased at 37 degrees C compared to 20 degrees C for both the lamellar and cubic phases. The water uptake increased dramatically with decreasing initial water content of the liquid crystalline phases. However, DADLE release increased with increasing initial water content, which corresponded to increased viscosity. The swelling and DADLE release profiles obtained using a Franz cell method with a moist nylon membrane to mimic buccal drug release conditions were slower than the total immersion method. These results show that the swelling and DADLE release strongly depended on temperature, the initial water content of the liquid crystalline matrix and the methodology employed for determining the swelling and DADLE release.

  17. Multivariate assessment of lipophilicity scales-computational and reversed phase thin-layer chromatographic indices.

    PubMed

    Andrić, Filip; Bajusz, Dávid; Rácz, Anita; Šegan, Sandra; Héberger, Károly

    2016-08-01

    Needs for fast, yet reliable means of assessing the lipophilicities of diverse compounds resulted in the development of various in silico and chromatographic approaches that are faster, cheaper, and greener compared to the traditional shake-flask method. However, at present no accepted "standard" approach exists for their comparison and selection of the most appropriate one(s). This is of utmost importance when it comes to the development of new lipophilicity indices, or the assessment of the lipophilicity of newly synthesized compounds. In this study, 50 well-known, diverse compounds of significant pharmaceutical and environmental importance have been selected and examined. Octanol-water partition coefficients have been measured with the shake-flask method for most of them. Their retentions have been studied in typical reversed thin-layer chromatographic systems, involving the most frequently employed stationary phases (octadecyl- and cyano-modified silica), and acetonitrile and methanol as mobile phase constituents. Twelve computationally estimated logP-s and twenty chromatographic indices together with the shake-flask octanol-water partition coefficient have been investigated with classical chemometric approaches-such as principal component analysis (PCA), hierarchical cluster analysis (HCA), Pearson's and Spearman's correlation matrices, as well as novel non-parametric methods: sum of ranking differences (SRD) and generalized pairwise correlation method (GPCM). Novel SRD and GPCM methods have been introduced based on the Comparisons with One VAriable (lipophilicity metric) at a Time (COVAT). For the visualization of COVAT results, a heatmap format was introduced. Analysis of variance (ANOVA) was applied to reveal the dominant factors between computational logPs and various chromatographic measures. In consensus-based comparisons, the shake-flask method performed the best, closely followed by computational estimates, while the chromatographic estimates often

  18. Multivariate assessment of lipophilicity scales-computational and reversed phase thin-layer chromatographic indices.

    PubMed

    Andrić, Filip; Bajusz, Dávid; Rácz, Anita; Šegan, Sandra; Héberger, Károly

    2016-08-01

    Needs for fast, yet reliable means of assessing the lipophilicities of diverse compounds resulted in the development of various in silico and chromatographic approaches that are faster, cheaper, and greener compared to the traditional shake-flask method. However, at present no accepted "standard" approach exists for their comparison and selection of the most appropriate one(s). This is of utmost importance when it comes to the development of new lipophilicity indices, or the assessment of the lipophilicity of newly synthesized compounds. In this study, 50 well-known, diverse compounds of significant pharmaceutical and environmental importance have been selected and examined. Octanol-water partition coefficients have been measured with the shake-flask method for most of them. Their retentions have been studied in typical reversed thin-layer chromatographic systems, involving the most frequently employed stationary phases (octadecyl- and cyano-modified silica), and acetonitrile and methanol as mobile phase constituents. Twelve computationally estimated logP-s and twenty chromatographic indices together with the shake-flask octanol-water partition coefficient have been investigated with classical chemometric approaches-such as principal component analysis (PCA), hierarchical cluster analysis (HCA), Pearson's and Spearman's correlation matrices, as well as novel non-parametric methods: sum of ranking differences (SRD) and generalized pairwise correlation method (GPCM). Novel SRD and GPCM methods have been introduced based on the Comparisons with One VAriable (lipophilicity metric) at a Time (COVAT). For the visualization of COVAT results, a heatmap format was introduced. Analysis of variance (ANOVA) was applied to reveal the dominant factors between computational logPs and various chromatographic measures. In consensus-based comparisons, the shake-flask method performed the best, closely followed by computational estimates, while the chromatographic estimates often

  19. Porphyrins as Second Order Nonlinear Optical Materials

    NASA Astrophysics Data System (ADS)

    Chou, Homer

    Because of the unusually high thermal and chemical stability of porphyrins as well as their very large pi-conjugated systems, three classes of high beta-value push-pull porphyrins were synthesized and subsequently successfully engineered into Langmuir-Blodgett (LB) films for a systematic evaluation of porphyrins as chi^{(2)} materials. Class I explored the effects of the number of donor-acceptor groups on the porphyrin periphery (i.e., H_2(an_3P), H_2 (cis-a_2n_2P), H_2(a_3nP), H _2(a_4P) where a = 4-(N-octadecylamido)phenyl or 4-(N-octadecyl-amino)phenyl; n = 4-nitrophenyl; P = 5,10,15,20 substituted tetraarylporphyrinate (2-).). Class II examined the effect of varying the strength of cis-substituted donor-acceptor pairs on the porphyrin periphery (i.e., H_2(cis-a_2n _2P), H_2(cis-c _2p_2P), and H_2 (cis-h_2py_2P) where c = 4-(2-cholesteryloxy)-ethoxyphenyl; h = 4-hydroxyphenyl or 4-methoxyphenyl; and py = 4-pyridyl or 4-(N-octadecyl) pyridiniumyl). Class III looked at the respone of a heterosubstituted bis- push-pull cerium sandwich porphyrin complex, (Ce ^{IV}(TPyP)(TMeP)) ^{4+}I_4 (where Py = 4-(N-octadecyl)pyridiniumyl and Me = 4-methoxyphenyl). Characterization of the porphyrin LB films reveals rather surprising behavior. The isotherm data show that the mean molecular area of the porphyrins increase smoothly from 80-200A as the number of aliphatic chains increase around the porphyrin periphery from one to four. In addition, based on UV-visible linear dichroism, all of the porphyrin films possess C _{infty v} symmetry and adopt a tilt angle, theta, of about 33^circ with respect to the fused quartz substrate. The proposed fixed orientation model suggests that the interporphyrin pi -pi interactions dominate the porphyrin orientation while the number of aliphatic chains around the porphyrin periphery determines the porphyrin's packing density in the LB film. After these monolayers were transferred to fused quartz substrates, the chi^{(2)} response of these

  20. Composition and method for encapsulating photovoltaic devices

    SciTech Connect

    Pern, F.J.

    2000-07-25

    A composition and method are disclosed for encapsulating a photovoltaic device which minimizes discoloration of the encapsulant. The composition includes an ethylene-vinyl acetate encapsulant, a curing agent, an optional ultraviolet light stabilizer, and/or an optional antioxidant. The curing agent is preferably 1,1-di-(t-butylperoxy)-3,3,5-trimethylcyclohexane; the ultraviolet light stabilizer is bis-(N-octyloxy-tetramethyl) piperidinyl sebacate and the antioxidant is selected from the group consisting of tris (2,4-di-tert-butylphenyl) phosphite, tetrakis methylene (3,5-di-tert-butyl-4-hydroxyhydrocinnamate) methane, octadecyl 3,5-di-tert-butyl-4-hydroxyhydrocinnamate, and 2,2{prime}-ethylidene bis(4,6-di-t-butylphenyl) fluorophosponite. The composition is applied to a solar cell then cured. The cured product contains a minimal concentration of curing-generated chromophores and resists UV-induced degradation.

  1. Composition and method for encapsulating photovoltaic devices

    DOEpatents

    Pern, Fu-Jann

    2000-01-01

    A composition and method for encapsulating a photovoltaic device which minimizes discoloration of the encapsulant. The composition includes an ethylene-vinyl acetate encapsulant, a curing agent, an optional ultraviolet light stabilizer, and/or an optional antioxidant. The curing agent is preferably 1,1-di-(t-butylperoxy)-3,3,5-trimethylcyclohexane; the ultraviolet light stabilizer is bis-(N-octyloxy-tetramethyl) piperidinyl sebacate and the antioxidant is selected from the group consisting of tris (2,4-di-tert-butylphenyl) phosphite, tetrakis methylene (3,5-di-tert-butyl-4-hydroxyhydrocinnamate) methane, octadecyl 3,5-di-tert-butyl-4-hydroxyhydrocinnamate, and 2,2'-ethylidene bis(4,6-di-t-butylphenyl) fluorophosponite. The composition is applied to a solar cell then cured. The cured product contains a minimal concentration of curing-generated chromophores and resists UV-induced degradation.

  2. Determination of thiram in natural waters using flow-injection with cerium(IV)-quinine chemiluminescence system.

    PubMed

    Waseem, Amir; Yaqoob, Mohammad; Nabi, Abdul

    2010-01-01

    A simple and rapid flow-injection chemiluminescence method has been developed for the determination of dithiocarbamate fungicide thiram based on the chemiluminescence reaction of thiram with ceric sulfate and quinine in aqueous sulfuric acid. The present method allowed the determination of thiram in the concentration range of 7.5-2500 ng/mL and the detection limit (signal-to-noise ratio = 3) was 7.5 ng/mL with sample throughput of 120/h. The relative standard deviation was 2.5% for 10 replicate analyses of 500 ng/mL thiram. The effects of foreign species including various anions and cations present in water at environmentally relevant concentrations and some pesticides were also investigated. The proposed method was applied to determine thiram in spiked natural waters using octadecyl bonded phase silica (C(18)) cartridges for solid-phase extraction. The recoveries were in the range 99 +/- 1 to 104 +/- 1%.

  3. Degradation of thiram in water, soil and plants: a study by high-performance liquid chromatography.

    PubMed

    Gupta, Bina; Rani, Manviri; Kumar, Rahul

    2012-01-01

    A comprehensive study was conducted to evaluate the persistence of thiram in water and soil under controlled conditions and on two plants, namely tomato and radish, in field conditions. In order to follow the decay of the pesticide, an HPLC procedure was developed employing an octadecyl endcapped RP-C18 column using a mixture of acetonitrile and water as the mobile phase and an ultraviolet detector. Studies conducted in water at different temperature, pH and organic content revealed that the persistence of the pesticide decreases with the increase in all the three variables. In the three different types of soils studied, the effect of pH was more or less apparent on a similar line. On average a slower decay was observed in the case of plants than in water and soil.

  4. Porosity in Polysilsesquioxane Xerolgels

    SciTech Connect

    Baugher, B.M.; Loy, D.A.; Rahimian, K.

    1999-08-17

    Polymerization of organotrialkoxysilanes is a convenient method for introducing organic functionality into hybrid organic-inorganic materials. However, not much is known about the effects of the organic substituent on the porosity of the resulting xerogels. In this study, we prepared a series of polysilsesquioxane xerogels from organotrialkoxysilanes, RSi(OR{sup 1}){sub 3}, with different organic groups (R = H, Me, Et dodecyl, hexadecyl, octadecyl, vinyl, chloromethyl, (p-chloromethyl) phenyl, cyanoethyl). Polymerizations of the monomers were carried out under a variety of conditions, varying monomer concentration, type of catalyst, and alkoxide substituent. The effect of the organic substituent on the sol-gel process was often dramatic. In many cases, gels were formed only at very high monomer concentration and/or with only one type of catalyst. All of the gels were processed as xerogels and characterized by scanning electron microscopy and nitrogen sorption porosimetry to evaluate their pore structure.

  5. A recyclable enzymatic biodiesel production process in ionic liquids.

    PubMed

    De Diego, Teresa; Manjón, Arturo; Lozano, Pedro; Iborra, José L

    2011-05-01

    Immobilized Candida antarctica lipase B suspended in ionic liquids containing long alkyl-chain cations showed excellent synthetic activity and operational stability for biodiesel production. The interest of this process lies in the possibility of recycling the biocatalyst and the easy separation of the biodiesel from the reaction mixture. The ionic liquids used, 1-hexadecyl-3-methylimidazolium triflimide ([C(16)MIM][NTf(2)]) and 1-octadecyl-3-methylimidazolium triflimide ([C(18)MIM][NTf(2)]), produced homogeneous systems at the start of the reaction and, at the end of the same, formed a three-phase system, allowing the selective extraction of the products using straightforward separation techniques, and the recycling of both the ionic liquid and the enzyme. These are very important advantages which may be found useful in environmentally friendly production conditions.

  6. Determination of traces of pesticides in water by solid-phase extraction and liquid chromatography-ionspray mass spectrometry.

    PubMed

    Giraud, D; Ventura, A; Camel, V; Bermond, A; Arpino, P

    1997-08-01

    A multi-residue analytical method for six pesticides (atrazine, hydroxyatrazine, carbofuran, promecarb, linuron and monolinuron) in drinking water has been developed. The method combines liquid chromatography and mass spectrometry using an ionspray interface. The linearity domain, as well as the limits of detection and quantification, were determined for each compound. Although satisfactory performance could be achieved, present drinking water regulations (0.1 microgram l-1 for single pesticide) requires a pre-concentration step. This was performed using solid-phase extraction with octadecyl-bonded silica cartridges. The analytical procedure was tested on water samples spiked at the 0.04 and 0.08 microgram l-1 levels, and allowed the determination of the investigated pesticides (except hydroxyatrazine) at these trace concentrations.

  7. Three New Isoprenylated Flavonoids from the Root Bark of Morus alba.

    PubMed

    Jung, Jae-Woo; Park, Ji-Hae; Lee, Yeong-Geun; Seo, Kyeong-Hwa; Oh, Eun-Ji; Lee, Dae-Young; Lim, Dong-Wook; Han, Daeseok; Baek, Nam-In

    2016-01-01

    Phytochemical investigation of the root bark of Morus alba has led to the isolation and identification of three new isoprenylated flavonoids, namely sanggenon U (1), sanggenon V (2), and sanggenon W (3), along with four known isoprenylated flavonoids: euchrenone a₇ (4), sanggenon J (5), kuwanon E (6), and kuwanon S (7). All compounds were isolated by repeated silica gel (SiO₂), octadecyl SiO₂ (ODS), and Sephadex LH-20 open column chromatography. The structure of the compounds were determined based on spectroscopic analyses, including nuclear magnetic resonance (NMR), mass spectrometry (MS), circular dichroism (CD), and infrared (IR). In addition, compounds 1-4 were isolated for the first time from the root bark of M. alba in this study. PMID:27563860

  8. Determination of benzo(a)pyrene in the total particulate matter of cigarette smoke

    SciTech Connect

    Risner, C.H.

    1988-03-01

    A procedure for the isolation and determination of benzo(a)pyrene in the total particulate matter of cigarette smoke is described. Two high-pressure liquid chromatographic (HPLC) techniques are employed: a normal-phase, mu Bondapak-NH2, amino column is used for isolation of the benzo(a)pyrene fraction and a reversed-phase, Vydac 201TP54, polymeric octadecyl silane column is used for quantitation. Fluorescence detection is used in both modes of chromatography. The wavelengths of excitation and emission are evaluated for analytical detection. Extraction media and various isolation techniques are compared for their extraction efficiency and isolation from interferences, respectively. The procedure is efficient, reproducible, sensitive (3 pg), and gives results that compare favorably with other techniques reported in the literature for the B(a)P content of reference cigarettes, 1R1 and 1R4F.

  9. In situ forming hydrogels of hyaluronic acid and inulin derivatives for cartilage regeneration.

    PubMed

    Palumbo, Fabio S; Fiorica, Calogero; Di Stefano, Mauro; Pitarresi, Giovanna; Gulino, Alessandro; Agnello, Stefano; Giammona, Gaetano

    2015-05-20

    An in situ forming hydrogel obtained by crosslinking of amino functionalized hyaluronic acid derivatives with divinylsulfone functionalized inulin (INU-DV) has been here designed and characterized. In particular two hyaluronic acid derivatives bearing respectively a pendant ethylenediamino (EDA) portion (HA-EDA) and both EDA and octadecyl pendant groups (HA-EDA-C18) were crosslinked through an azo-Michael reaction with INU-DV. Gelation time and consumption of DV portions have been evaluated on hydrogel obtained using HA-EDA and HA-EDA-C18 derivatives with a concentration of 3% w/v and a ratio 80/20 w/w respect to the crosslinker INU-DV. The presence of pendant C18 chains improves mechanical performances of hydrogels and decreases the susceptibility to hyaluronidase hydrolysis. Bovine chondrocytes, encapsulated during crosslinking, sufficiently survive and efficiently proliferate until 28 days of analysis.

  10. Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

    PubMed

    Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

    2015-07-01

    Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns.

  11. Bacteria-mimicking nanoparticle surface functionalization with targeting motifs

    NASA Astrophysics Data System (ADS)

    Lai, Mei-Hsiu; Clay, Nicholas E.; Kim, Dong Hyun; Kong, Hyunjoon

    2015-04-01

    In recent years, surface modification of nanocarriers with targeting motifs has been explored to modulate delivery of various diagnostic, sensing and therapeutic molecular cargo to desired sites of interest in in vitro bioengineering platforms and in vivo pathologic tissue. However, most surface functionalization approaches are often plagued by complex chemical modifications and effortful purifications. To resolve such challenges, this study demonstrates a unique method to immobilize antibodies that can act as targeting motifs on the surfaces of nanocarriers, inspired by a process that bacteria use for immobilization of the host's antibodies. We hypothesized that alkylated Staphylococcus aureus protein A (SpA) would self-assemble with micelles and subsequently induce stable coupling of antibodies to the micelles. We examined this hypothesis by using poly(2-hydroxyethyl-co-octadecyl aspartamide) (PHEA-g-C18) as a model polymer to form micelles. The self-assembly between the micelles and alkylated SpA became more thermodynamically favorable by increasing the degree of substitution of octadecyl chains to PHEA-g-C18, due to a positive entropy change. Lastly, the mixing of SpA-PA-coupled micelles with antibodies resulted in the coating of micelles with antibodies, as confirmed with a fluorescence resonance energy transfer (FRET) assay. The micelles coated with antibodies to VCAM-1 or integrin αv displayed a higher binding affinity to substrates coated with VCAM-1 and integrin αvβ3, respectively, than other controls, as evaluated with surface plasmon resonance (SPR) spectroscopy and a circulation-simulating flow chamber. We envisage that this bacteria-inspired protein immobilization approach will be useful to improve the quality of targeted delivery of nanoparticles, and can be extended to modify the surface of a wide array of nanocarriers.In recent years, surface modification of nanocarriers with targeting motifs has been explored to modulate delivery of various

  12. van der Waals force-induced loading of proangiogenic nanoparticles on microbubbles for enhanced neovascularization

    NASA Astrophysics Data System (ADS)

    Chen, Jinrong; Lee, Min Kyung; Qin, Ellen; Misra, Sanjay; Kong, Hyunjoon

    2015-10-01

    Nanoparticles emerged as carriers of promising diagnostic and therapeutic molecules due to their unique size, injectability, and potential to sustainably release molecular cargos. However, with local injection of particles into target tissue, the significant particle loss caused by external biomechanical forces is a great challenge yet to be resolved to date. We hypothesized that nanoparticles associated with tissue-adherent microbubbles in the form of core-shell particles due to van der Waals attractive forces would stably remain on an implanted site and significantly increase therapeutic efficacy of drug cargos. To examine this hypothesis, we used 100 nm diameter nanoparticles made of poly(lactide-co-glycolic acid) (PLGA) as a model nanoparticle and 50 μm diameter microbubbles made of poly(2-hydroxyethyl aspartamide) (PHEA) grafted with octadecyl chains, PHEA-g-C18, as a model microbubble. Simple mixing of PLGA nanoparticles and PHEA-g-C18 microbubbles resulted in the core-shell particles. Following implantation, the PHEA-g-C18 microbubbles acted as glue to minimize the displacement of PLGA nanoparticles, because of the association between the octadecyl chains on PHEA-g-C18 and the epithelium of the tissue. As a consequence, the core-shell particles prepared with Angiopoietin-1 (Ang1)-encapsulated PLGA nanoparticles significantly promoted vascularization in the implanted tissue. Overall, the results of this study provide a simple but advanced strategy for improving therapeutic efficacy of drug-carrying nanoparticles without altering their surface chemistry and potential.Nanoparticles emerged as carriers of promising diagnostic and therapeutic molecules due to their unique size, injectability, and potential to sustainably release molecular cargos. However, with local injection of particles into target tissue, the significant particle loss caused by external biomechanical forces is a great challenge yet to be resolved to date. We hypothesized that nanoparticles

  13. Determination of selected azaarenes in water by bonded-phase extraction and liquid chromatography

    USGS Publications Warehouse

    Steinheimer, T.R.; Ondrus, M.G.

    1986-01-01

    A method for the rapid and simple quantitative determination of quinoline, isoquinoline, and five selected three-ring azaarenes in water has been developed. The azaarene fraction is separated from its carbon analogues on n-octadecyl packing material by edition with acidified water/acetonitrile. Concentration as great as 1000-fold is achieved readily. Instrumental analysis involves high-speed liquid chromatography on flexible-walled, wide-bore columns with fluorescence and ultraviolet detection at several wavelengths employing filter photometers in series. Method-validation data is provided as azaarene recovery efficiency from fortified samples. Distilled water, river water, contaminated ground water, and secondary-treatment effluent have been tested. Recoveries at part-per-billion levels are nearly quantitative for the three-ring compounds, but they decrease for quinoline and isoquinoline. ?? 1986 American Chemical Society.

  14. Chemical patterns of octadecyltrimethoxysilane monolayers for the selective deposition of nanoparticles on silicon substrate.

    PubMed

    Ressier, L; Viallet, B; Grisolia, J; Peyrade, J P

    2007-10-01

    The use of nano-objects to make the active part of reproducible nanodevices requires their controlled assembling on specific areas of substrates. In this work, we propose to use van der Waals interactions to assemble selectively gold particles covered by alkyl-thiol ligands on hydrophobic OctadecylTriMethoxySilane (OTMS) patterns defined on SiO(2)/Si substrates by a process combining nano-imprint lithography (NIL) or high resolution electron beam lithography (HREBL) and atmospheric chemical vapor deposition (CVD) of silane. A study by atomic force microscopy (AFM) reveals that homogeneous patterns of OTMS self-assembled monolayers, extending on several square millimeters, have been made. These OTMS patterns, with a lateral dimension ranging from 2mum down to 50nm, can be located at a precise place of a nanodevice, for example, between nanoelectrodes. Preliminary results of selective nanoparticle deposition on these chemical patterns are presented.

  15. Resonance energy transfer in a model system of membranes: application to gel and liquid crystalline phases.

    PubMed

    Loura, L M; Fedorov, A; Prieto, M

    1996-10-01

    Resonance energy transfer between octadecyl rhodamine B (donor) and 1,1',3,3,3',3'-hexamethylindotricarbocyanine (acceptor) was studied in a model system of membranes (large unilamellar vesicles of dipalmitoylphosphatidylcholine), using both steady-state and time-resolved techniques. In the fluid phase (temperature = 50 degrees C) the decay law and the steady-state theoretical curve for energy transfer in two dimensions are verified. In the gel phase (temperature = 25 degrees C) an apparent reduction of dimensionality is observed, which is explained on the basis of probe segregation to the defect lines (grain boundaries). An estimation of the domain size from the model recovered linear probe concentrations is approximately 1750-2000 lipid molecules. In both phases, the existence of a fractal geometry was ruled out. PMID:8889159

  16. Decoration of silicon nanostructures with copper particles for simultaneous selective capture and mass spectrometry detection of His-tagged model peptide.

    PubMed

    Coffinier, Yannick; Kurylo, Ievgen; Drobecq, Hervé; Szunerits, Sabine; Melnyk, Oleg; Zaitsev, Vladimir N; Boukherroub, Rabah

    2014-10-21

    We present in this work a simple and fast preparation method of a new affinity surface-assisted laser/desorption ionization mass spectrometry (SALDI-MS) substrate based on silicon nanostructures decorated with copper particles. The silicon nanostructures were fabricated by the metal-assisted chemical etching (MACE) method. Then, superhydrophilic areas surrounded by superhydrophobic regions were formed through hydrosilylation reaction of 1-octadecene, followed by local degradation of the octadecyl layer. After that, copper particles were deposited in the hydrophilic areas by using the electroless method. We have demonstrated that these surfaces were able to perform high selective capture of model His-tag peptide even in a complex mixture such as serum solution. Then, the captured peptide was detected by mass spectrometry at a femtomolar level without the need of organic matrix. PMID:25112364

  17. Comparison of the performance of different silica hydride particles for the solid-phase extraction of non-volatile analytes from dark chocolate with analysis by gas chromatography-quadrupole mass spectrometry.

    PubMed

    Nolvachai, Yada; Kulsing, Chadin; Boysen, Reinhard I; Matyska, Maria T; Pesek, Joseph J; Marriott, Philip J; Hearn, Milton T W

    2015-05-01

    The extraction capabilities of a Diamond Hydride™ phase, as well as silica hydride phases modified with bidentate octadecyl (BDC(18)), phenyl or cholesteryl groups, were evaluated for the analysis of fatty acids, amino acids, sugars and sterols in a dark chocolate extract. These batch adsorption performances were investigated using either methanol or aqueous methanol as the solvent. The compositions of the extracted fractions were assessed by gas chromatography interfaced with quadrupole mass spectrometry (GC-qMS). The batch binding propensities of the various compound classes with silica hydride particles modified with immobilised phenyl groups or larger ligands followed trends predicted from linear solvation energy relationships. Both prediction and experiment revealed that better extraction results could be obtained with the phenyl, BDC(18) and cholesteryl hydride particles for the major chocolate components. Based on these results, separations in micro-pipette tip format with these three types of stationary phase particles have been undertaken. PMID:25529702

  18. A Bilayered Structure Comprised of Functionalized Carbon Nanotubes for Desalination by Membrane Distillation.

    PubMed

    Bhadra, Madhuleena; Roy, Sagar; Mitra, Somenath

    2016-08-01

    The development of a novel carbon nanotube (CNT) immobilized membrane comprised of a double-layer structure is presented for water desalination by membrane distillation. The bilayered structure is comprised of CNTs functionalized with a hydrophobic octadecyl amine group on the feed side and carboxylated CNTs on the permeate side. The latter is more hydrophilic. The hydrophobic CNTs provide higher water vapor permeation, while the hydrophilic CNTs facilitate the condensation of water vapor. Together, these led to superior performance, and flux in a direct contact membrane distillation mode was found to be as high as 121 kg/m(2)h at 80 °C. The bilayered membrane represented an enhancement of 70% over the unmodified membrane and 37% over a membrane which had a monolayered structure where only the feed side was CNT-modified. PMID:27387851

  19. Simultaneous enantioselective quantification of fluoxetine and norfluoxetine in human milk by direct sample injection using 2-dimensional liquid chromatography-tandem mass spectrometry.

    PubMed

    Alvim-Jr, Joel; Lopes, Bianca Rebelo; Cass, Quezia Bezerra

    2016-06-17

    A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the simultaneously quantification of fluoxetine (FLX) and norfluoxetine (NFLX) enantiomers in human milk by direct injection of samples. A restricted access media of bovine serum albumin octadecyl column (RAM-BSAC18) was used in the first dimension for the milk proteins depletion, while an antibiotic-based chiral column was used in the second dimension. The results herein described show good selectivity, extraction efficiency, accuracy, and precision with limits of quantification in the order of 7.5ngmL(-1)for the FLX enantiomers and 10.0ngmL(-1) for NFLX enantiomers. Furthermore, it represents a practical tool in terms of sustainability for the sample preparation of such a difficult matrix.

  20. One-Pot Synthesis of Organic-Sulfur-Zinc Hybrid Materials via Polycondensation of a Zinc Salt and Thiols Generated in Situ from Cyclic Dithiocarbonates.

    PubMed

    Ochiai, Bungo; Konta, Hirohisa

    2015-08-17

    Soluble organic-sulfur-zinc hybrid polymers were prepared via a one-pot reaction consisting of ring-opening addition and subsequent polycondensation. The first reaction is the nucleophilic ring-opening addition of 2-ethylhexylamine to multifunctional cyclic dithiocarbonates giving multiple thiols in situ. The sequential polycondensation of the in situ generated thiols with Zn(OAc)2 gave the target hybrid polymers. This one-pot method enabled the use of a shorter amine than the previous polycondensation of Zn(OAc)2 and purified thiols, which required octadecylamine to obtain a soluble product. The obtained hybrid polymers may be cast as composite films with polystyrene and poly(methyl methacrylate). Owing to the shorter alkyl chain, the calculated nD values of the products (1.60 or 1.61) are higher than that of the previous product bearing octadecyl chains (1.53).

  1. A Bilayered Structure Comprised of Functionalized Carbon Nanotubes for Desalination by Membrane Distillation.

    PubMed

    Bhadra, Madhuleena; Roy, Sagar; Mitra, Somenath

    2016-08-01

    The development of a novel carbon nanotube (CNT) immobilized membrane comprised of a double-layer structure is presented for water desalination by membrane distillation. The bilayered structure is comprised of CNTs functionalized with a hydrophobic octadecyl amine group on the feed side and carboxylated CNTs on the permeate side. The latter is more hydrophilic. The hydrophobic CNTs provide higher water vapor permeation, while the hydrophilic CNTs facilitate the condensation of water vapor. Together, these led to superior performance, and flux in a direct contact membrane distillation mode was found to be as high as 121 kg/m(2)h at 80 °C. The bilayered membrane represented an enhancement of 70% over the unmodified membrane and 37% over a membrane which had a monolayered structure where only the feed side was CNT-modified.

  2. Decoration of silicon nanostructures with copper particles for simultaneous selective capture and mass spectrometry detection of His-tagged model peptide.

    PubMed

    Coffinier, Yannick; Kurylo, Ievgen; Drobecq, Hervé; Szunerits, Sabine; Melnyk, Oleg; Zaitsev, Vladimir N; Boukherroub, Rabah

    2014-10-21

    We present in this work a simple and fast preparation method of a new affinity surface-assisted laser/desorption ionization mass spectrometry (SALDI-MS) substrate based on silicon nanostructures decorated with copper particles. The silicon nanostructures were fabricated by the metal-assisted chemical etching (MACE) method. Then, superhydrophilic areas surrounded by superhydrophobic regions were formed through hydrosilylation reaction of 1-octadecene, followed by local degradation of the octadecyl layer. After that, copper particles were deposited in the hydrophilic areas by using the electroless method. We have demonstrated that these surfaces were able to perform high selective capture of model His-tag peptide even in a complex mixture such as serum solution. Then, the captured peptide was detected by mass spectrometry at a femtomolar level without the need of organic matrix.

  3. Semiautomated determination of pesticides in water using solid phase extraction disks and gas chromatography-mass spectrometry.

    PubMed

    Leandro, Cristiana C; Bishop, Dawn A; Fussell, Richard J; Smith, Frankie D; Keely, Brendan J

    2006-02-01

    A method based on semiautomated solid phase extraction using octadecyl-bonded silica disks and gas chromatography-mass spectrometry, operated in selected ion monitoring mode, allows detection and quantification of approximately 100 pesticides and transformation products in drinking water. Samples (500 mL) were passed through the disk, and the retained pesticides were eluted with acetone and ethyl acetate. Typical recoveries for pesticides at 0.1 microg L(-1) in water were in the range of 72-120% with relative standard deviations less than 20%. Calibration curves were linear over the range of 0.025-0.5 microg mL(-1) (equivalent to a concentration range in drinking water of 0.05-1.0 microg L(-1)).

  4. Simultaneous enantioselective quantification of fluoxetine and norfluoxetine in human milk by direct sample injection using 2-dimensional liquid chromatography-tandem mass spectrometry.

    PubMed

    Alvim-Jr, Joel; Lopes, Bianca Rebelo; Cass, Quezia Bezerra

    2016-06-17

    A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the simultaneously quantification of fluoxetine (FLX) and norfluoxetine (NFLX) enantiomers in human milk by direct injection of samples. A restricted access media of bovine serum albumin octadecyl column (RAM-BSAC18) was used in the first dimension for the milk proteins depletion, while an antibiotic-based chiral column was used in the second dimension. The results herein described show good selectivity, extraction efficiency, accuracy, and precision with limits of quantification in the order of 7.5ngmL(-1)for the FLX enantiomers and 10.0ngmL(-1) for NFLX enantiomers. Furthermore, it represents a practical tool in terms of sustainability for the sample preparation of such a difficult matrix. PMID:27208983

  5. Anomalous behavior of the J-aggregate of quinocyanine dyes in the mixed Langmuir-Blodgett films

    NASA Astrophysics Data System (ADS)

    Sluch, M. I.; Vitukhnovsky, A. G.; Yonezawa, Y.; Ishizawa, H.; Sato, T.

    1997-07-01

    The J-aggregates of quinocyanine dyes (5,6,5'6'-dibenzo-1,1'-diethyl-2,2'-cyanine chloride (Sh) and 1-methyl-1'-octadecyl-2,2'-cyanine perchlorate (S120)) have been fabricated in a Langmuir trough and transferred onto quartz substrate. The formation of the J-aggregates has been studied by methods of conventional absorption and fluorescence time resolved spectroscopy. The mixed J-aggregate of S120 and Sh shows two distinct absorption bands and one fluorescence band intermediate between those of the J-aggregates of the individual component dyes. These results have some anomaly compared with the mixed J-aggregates of quinocyanine dyes and its benzothiazole or benzoselenazole derivative formed in solutions (Scheibe et al., Naturwissenschaften 29 474 (1937)) and in Langmuir-Blodgett films (Penner and Mobius, Thin Solid Films 132 185 (1985)).

  6. Two-dimensional liquid chromatography (LC) of phenolic compounds from the shoots of Rubus idaeus 'Glen Ample' cultivar variety.

    PubMed

    Kula, Marta; Głód, Daniel; Krauze-Baranowska, Mirosława

    2016-03-20

    In this study the application of two-dimensional LC (2D LC) for qualitative analysis of polyphenols and simple phenols in the shoots of Rubus idaeus 'Glen Ample' variety is presented. In the preliminary analysis, the methanol extract of the shoots was analyzed by one-dimensional LC. One-dimensional LC separation profiles of phenolics from R. idaeus 'Glen Ample' shoots were dependent on column type, mobile phase composition and gradient program used. Two-dimensional LC system was built from connecting an octadecyl C-18 silica column in the first dimension and pentafluorophenyl column in the second dimension, coupled with DAD and MS (ESI, APCI, DUIS ionization) detectors. A total of 34 phenolic compounds belonging to the groups of phenolic acids, ellagitannins, flavan-3-ols, flavonols and ellagic acid conjugates were identified in the shoots of R. idaeus 'Glen Ample'. The established 2D LC method offers an effective tool for analysis of phenolics present in Rubus species. PMID:26799975

  7. Purification and characterization of prolixin S (nitrophorin 2), the salivary anticoagulant of the blood-sucking bug Rhodnius prolixus.

    PubMed Central

    Ribeiro, J M; Schneider, M; Guimarães, J A

    1995-01-01

    The salivary anticoagulant of the blood-sucking bug Rhodnius prolixus was purified to homogeneity using a protocol consisting of weak cation-exchange, DEAE, hydrophobic-interaction and octadecyl reverse-phase chromatography, yielding a protein with the same N-terminal sequence as nitrophorin 2, one of the four NO haem protein carriers present in the salivary glands of Rhodnius with a molecular mass of 19689 Da [D. Champagne, R.H. Nussenzveig and J.M.C. Ribeiro, (1995) J. Biol. Chem. 270, in the press]. To exclude the possibility of the nitrophorin being a contaminant, another chromatographic protocol was performed, consisting of chromatofocusing followed by strong-cation-exchange chromatography. Again the anticoagulant was eluted with nitrophorin 2. Nitrophorin 2 inhibits coagulation Factor VIII-mediated activation of Factor X and accounts for all the anti-clotting activity observed in Rhodnius salivary glands. PMID:7755571

  8. [Determination of Butroxydim in Agricultural Products by LC-MS].

    PubMed

    Minatani, Tomiaki; Nagai, Hiroyuki; Tada, Hiroyuki; Goto, Kotaro; Nemoto, Satoru

    2015-01-01

    An analytical method for the determination of butroxydim in agricultural products by LC-MS was developed. Butroxydim was extracted with acetonitrile and an aliquot of the crude extract was cleaned up on an octadecyl silanized silica gel (C18) cartridge column (1,000 mg), followed by a salting-out step to remove water. Before purification on a silica gel (SI) cartridge column (690 mg), polar matrices were precipitated by adding ethyl acetate, n-hexane and anhydrous sodium sulfate successively. This process effectively removed caffeine and catechins and improved recovery when analyzing residual butroxydim in tea leaves. Recovery and repeatability were good; the relative standard deviations were less than 5% for all 12 tested agricultural products (brown rice, soybean, potato, spinach, cabbage, apple, orange, grapefruit, lemon, tomato, peas with pods, and tea). Average recoveries for 11 agricultural products, except for lemon, were 74-92%. PMID:26699270

  9. Structural determinants of Tau aggregation inhibitor potency.

    PubMed

    Schafer, Kelsey N; Cisek, Katryna; Huseby, Carol J; Chang, Edward; Kuret, Jeff

    2013-11-01

    Small-molecule Tau aggregation inhibitors are under investigation as potential therapeutic agents against Alzheimer disease. Many such inhibitors have been identified in vitro, but their potency-driving features, and their molecular targets in the Tau aggregation pathway, have resisted identification. Previously we proposed ligand polarizability, a measure of electron delocalization, as a candidate descriptor of inhibitor potency. Here we tested this hypothesis by correlating the ground state polarizabilities of cyanine, phenothiazine, and arylmethine derivatives calculated using ab initio quantum methods with inhibitory potency values determined in the presence of octadecyl sulfate inducer under reducing conditions. A series of rhodanine analogs was analyzed as well using potency values disclosed in the literature. Results showed that polarizability and inhibitory potency directly correlated within all four series. To identify putative binding targets, representative members of the four chemotypes were added to aggregation reactions, where they were found to stabilize soluble, but SDS-resistant Tau species at the expense of filamentous aggregates. Using SDS resistance as a secondary assay, and a library of Tau deletion and missense mutants as targets, interaction with cyanine was localized to the microtubule binding repeat region. Moreover, the SDS-resistant phenotype was completely dependent on the presence of octadecyl sulfate inducer, but not intact PHF6/PH6* hexapeptide motifs, indicating that cyanine interacted with a species in the aggregation pathway prior to nucleus formation. Together the data suggest that flat, highly polarizable ligands inhibit Tau aggregation by interacting with folded species in the aggregation pathway and driving their assembly into soluble but highly stable Tau oligomers.

  10. Structural Determinants of Tau Aggregation Inhibitor Potency*

    PubMed Central

    Schafer, Kelsey N.; Cisek, Katryna; Huseby, Carol J.; Chang, Edward; Kuret, Jeff

    2013-01-01

    Small-molecule Tau aggregation inhibitors are under investigation as potential therapeutic agents against Alzheimer disease. Many such inhibitors have been identified in vitro, but their potency-driving features, and their molecular targets in the Tau aggregation pathway, have resisted identification. Previously we proposed ligand polarizability, a measure of electron delocalization, as a candidate descriptor of inhibitor potency. Here we tested this hypothesis by correlating the ground state polarizabilities of cyanine, phenothiazine, and arylmethine derivatives calculated using ab initio quantum methods with inhibitory potency values determined in the presence of octadecyl sulfate inducer under reducing conditions. A series of rhodanine analogs was analyzed as well using potency values disclosed in the literature. Results showed that polarizability and inhibitory potency directly correlated within all four series. To identify putative binding targets, representative members of the four chemotypes were added to aggregation reactions, where they were found to stabilize soluble, but SDS-resistant Tau species at the expense of filamentous aggregates. Using SDS resistance as a secondary assay, and a library of Tau deletion and missense mutants as targets, interaction with cyanine was localized to the microtubule binding repeat region. Moreover, the SDS-resistant phenotype was completely dependent on the presence of octadecyl sulfate inducer, but not intact PHF6/PH6* hexapeptide motifs, indicating that cyanine interacted with a species in the aggregation pathway prior to nucleus formation. Together the data suggest that flat, highly polarizable ligands inhibit Tau aggregation by interacting with folded species in the aggregation pathway and driving their assembly into soluble but highly stable Tau oligomers. PMID:24072703

  11. Modeling the Geometric Electronic and Redox Properties of Iron(lll)-Containing Amphiphiles with Asymmetric [NNO] Headgroups

    SciTech Connect

    R Shakya; M Allard; M Johann; M Heeg; E Rentschler; J Shearer; B McGarvey; C Verani

    2011-12-31

    Two iron(III)-containing amphiphiles 1 and 2 have been synthesized with the [NN'O] ligands HL{sup tBu-ODA} (2-((octadecyl(pyridin-2-ylmethyl)amino)methyl)-4,6-di-tert-butylphenol) and HL{sup I-ODA} (2-((octadecyl(pyridin-2-ylmethyl)amino)methyl)-4,6-diiodophenol), respectively. Compound 1 is monometallic, whereas EXAFS data suggest that 2 is a mixture of mono- and bimetallic species. The archetypical [Fe{sup III}(L{sup NN'O}){sub 2}]{sup +} complexes 3-9 have been isolated and characterized in order to understand the geometric, electronic, and redox properties of the amphiphiles. Preference for a monometallic or bimetallic nuclearity is dependent on (i) the nature of the solvent used for synthesis and (ii) the type of the substituent in the phenol moiety. In methanol, the tert-butyl-, methoxy-, and chloro-substituted 3, 4, and 5 are monometallic species, whereas the bromo- and iodo-substituted 6 and 7 form bimetallic complexes taking advantage of stabilizing methoxo bridges generated by solvent deprotonation. In dichloromethane, the bromo- and iodo-substituted 8 and 9 are monometallic species; however, these species favor meridional coordination in opposition to the facial coordination observed for the tert-butyl- and methoxy-substituted compounds. Molecular structures for species 5, 7, 8, and 9 have been solved by X-ray diffraction. Furthermore, the electronic spectrum of the amphiphile 1 was expected to be similar to those of facial/cis archetypes with similar substituents, but close resemblance was observed with the profile for those meridional/cis species, suggesting a similar coordination mode. This trend is discussed based on DFT calculations, where preference for the meridional/cis coordination mode appears related to the presence of tertiary amine nitrogen on the ligand, as when a long alkyl chain is attached to the [NN'O] headgroup.

  12. Platelet-activating factor biosynthesis induced by various stimuli in human HaCaT keratinocytes.

    PubMed

    Travers, J B; Harrison, K A; Johnson, C A; Clay, K L; Morelli, J G

    1996-07-01

    Platelet-activating factor (PAF) is a potent inflammatory mediator that is thought to play a role in cutaneous inflammation. These studies used mass spectrometry to examine the molecular species of PAF precursor glycerophosphocholine lipids (GPC) as well as the biosynthesis of PAF and other sn-2 acetyl-GPC in a human keratinocyte-derived cell line (HaCaT keratinocytes). Approximately 28% of HaCaT keratinocyte GPC consisted of 1-alkyl species, and the relative amounts of the sn-1 alkyl constituents of the PAF precursor 1-alkyl-2-acyl-GPC were as follows: hexadecyl > octadecenyl > octadecyl. Ionophore (A23187)-stimulated HaCaT keratinocytes synthesized both PAF (1-hexadecyl, 1-octadecenyl, and 1-octadecyl species) and less potent 1-acyl analogs (1-palmitoyl, 1-oleoyl, and 1-stearoyl species). PAF production was rapid and maximal by 10 min. The major species of sn-2acetyl-GPC at 2.5 min were 1-hexadecyl-2-acetyl-GPC (2.2 ng/10(6) cells) and 1-palmitoyl-2-acetyl-GPC (2.4 ng/10(6) cells). HaCaT keratinocytes also synthesized PAF and 1-acyl PAF analogs when stimulated with the peptide growth factor endothelin-1 and the nonhydrolyzable PAF receptor agonist carbamyl-PAF. Both 1-hexadecyl-2- acetyl-GPC and 1-palmitoyl-2-acetyl-GPC stimulated intracellular calcium mobilization in HaCaT cells, indicating that these sn-2 acetyl-GPC act in autocrine fashion. These studies revealed that the human keratinocyte-derived cell line HaCaT can synthesize significant amounts of PAF and 1-acyl analogs in vitro from both nonspecific (A23187) and specific (endothelin-1, carbamyl-PAF) stimulation, suggesting a role for this inflammatory lipid mediator in keratinocyte pathophysiology.

  13. The Japan Flavour and Fragrance Materials Association's (JFFMA) safety assessment of acetal food flavouring substances uniquely used in Japan.

    PubMed

    Okamura, Hiroyuki; Abe, Hajime; Hasegawa-Baba, Yasuko; Saito, Kenji; Sekiya, Fumiko; Hayashi, Shim-Mo; Mirokuji, Yoshiharu; Maruyama, Shinpei; Ono, Atsushi; Nakajima, Madoka; Degawa, Masakuni; Ozawa, Shogo; Shibutani, Makoto; Maitani, Tamio

    2015-01-01

    Using the procedure devised by the Joint FAO/WHO Expert Committee on Food Additives (JECFA), we performed safety evaluations on five acetal flavouring substances uniquely used in Japan: acetaldehyde 2,3-butanediol acetal, acetoin dimethyl acetal, hexanal dibutyl acetal, hexanal glyceryl acetal and 4-methyl-2-pentanone propyleneglycol acetal. As no genotoxicity study data were available in the literature, all five substances had no chemical structural alerts predicting genotoxicity. Using Cramer's classification, acetoin dimethyl acetal and hexanal dibutyl acetal were categorised as class I, and acetaldehyde 2,3-butanediol acetal, hexanal glyceryl acetal and 4-methyl-2-pentanone propyleneglycol acetal as class III. The estimated daily intakes for all five substances were within the range of 1.45-6.53 µg/person/day using the method of maximised survey-derived intake based on the annual production data in Japan from 2001, 2005, 2008 and 2010, and 156-720 µg/person/day using the single-portion exposure technique (SPET), based on the average use levels in standard portion sizes of flavoured foods. The daily intakes of the two class I substances were below the threshold of toxicological concern (TTC) - 1800 μg/person/day. The daily intakes of the three class III substances exceeded the TTC (90 μg/person/day). Two of these, acetaldehyde 2,3-butanediol acetal and hexanal glyceryl acetal, were expected to be metabolised into endogenous products after ingestion. For 4-methyl-2-pentanone propyleneglycol acetal, one of its metabolites was not expected to be metabolised into endogenous products. However, its daily intake level, based on the estimated intake calculated by the SPET method, was about 1/15 000th of the no observed effect level. It was thus concluded that all five substances raised no safety concerns when used for flavouring foods at the currently estimated intake levels. While no information on in vitro and in vivo toxicity for all five substances was available

  14. α-Tocopherol impact on oxy-radical induced free radical decomposition of DMSO: Spin trapping EPR and theoretical studies

    NASA Astrophysics Data System (ADS)

    Jerzykiewicz, Maria; Ćwieląg-Piasecka, Irmina; Witwicki, Maciej; Jezierski, Adam

    2011-05-01

    EPR spin trapping and theoretical methods such as density functional theory (DFT) as well as combined DFT and quadratic configuration interaction approach (DFT/QCISD) were used to identify the radicals produced in the reaction of oxy-radicals and dimethyl sulfoxide (DMSO) in the presence and absence of α-tocopherol. Additionally, the mixtures of α-tocopherol with linolenic acid and glyceryl trilinoleate as well as bioglycerols (glycerol fractions from biodiesel production) were tested. α-Tocopherol inhibited oxidation of the main decomposition product of DMSO, •CH 3 to •OCH 3 but did not prevent the transformation process of N-t-butyl- α-phenylnitrone (PBN) into 2-methyl-2-nitrosopropane (MNP). Theoretical investigations confirmed the structures of proposed spin adducts and allowed to correlate the EPR parameters observed in the experiment with the spin adducts electronic structure.

  15. [Allergic contact dermatitis in beauty parlor clients].

    PubMed

    Gottlöber, P; Gall, H; Bezold, G; Peter, R U

    2001-05-01

    Occupational contact dermatitis in hair dressers and beauticians has increased in importance in the past years. Type IV-allergies against glyceryl monothioglycate components of permanent waves are most common. Other occupational allergens include bleach components such as ammonium persulfate and hair dye ingredients such as p-phenylenediamine (PPD) and p-toluylene-diamine (PTD) base. Allergies to hair dyes in customers of hair dressers have rarely been observed. Two female patients developed allergic contact dermatitis of the scalp and face after repeated use of Polycolor intensivtönung schwarz and of Movida color. We also review the current literature on type IV-allergies to components of hair dressing products components.

  16. Encapsulation of ethylhexyl methoxycinnamate, a light-sensitive UV filter, in lipid nanoparticles.

    PubMed

    Durand, L; Habran, N; Henschel, V; Amighi, K

    2010-01-01

    The aim of this study was to encapsulate ethylhexyl methoxycinnamate (EMC), a commonly used UVB filter, in a solid lipid matrix in order to obtain microparticles and then nanoparticles to reduce its photo-instability under UV light exposure. Glyceryl behenate, rice bran wax and ozokerite were investigated for encapsulating EMC. The suspensions of nanoparticles contained 70% encapsulated EMC (relative to the lipid mass). The absorbance level at 310 nm of suspensions containing nanoparticles was more than twice that of those containing microparticles. So, decreasing the size of particles improved the efficiency of light protection, regardless of the lipid material used. Moreover, free EMC presented a 30% loss of its efficiency after 2 h of irradiation, whereas the three NLC formulations showed a loss of absorbency between 10% and 21%. The in vitro cutaneous penetration test did not show a higher potential penetration for EMC contained in nanosuspensions compared to free EMC. PMID:21034364

  17. Preparation of solid lipid nanoparticles by a solvent emulsification-diffusion technique.

    PubMed

    Trotta, Michele; Debernardi, Francesca; Caputo, Otto

    2003-05-12

    A preparation method for nanoparticles based on the emulsification of a butyl lactate or benzyl alcohol solution of a solid lipid in an aqueous solution of different emulsifiers, followed by dilution of the emulsion with water, was used to prepare glyceryl monostearate nanodispersions with narrow size distribution. To increase the lipid load the process was conducted at 47+/-2 degrees C and in order to reach submicron size a high-shear homogenizer was used. Particle size of the solid lipid nanoparticles (SLN) was affected by using different emulsifiers and different lipid loads. By using lecithin and taurodeoxycholic acid sodium salt, on increasing the GMS percentage from 2.5 to 10% an increase of the mean diameter from 205 to 695 nm and from 320 to 368nm was observed for the SLN prepared using benzyl alcohol and butyl lactate, respectively. Transmission electron micrographs of SLN reveal nanospheres with a smooth surface.

  18. Modeling accelerated and decelerated drug release in terms of fractional release rate.

    PubMed

    Weiss, Michael

    2015-02-20

    The model of a proportional change in fractional dissolution rate was used to quantify influences on the vitro dissolution process. After fitting the original dissolution profile with an empirical model (inverse Gaussian distribution), acceleration and deceleration effects due to dissolution conditions or formulation parameters could be described by one parameter only. Acceleration of dissolution due to elevated temperature and deceleration by increasing the content of glyceryl monostearate in theophylline tablets are presented as examples. Likewise, this approach was applied to in vitro-in vivo correlation (IVIVC). It is shown that the model is appropriate when the plot of the in vivo versus in vivo times is nonlinear and can be described by a power function. The results demonstrate the utility of the model in dissolution testing and IVIVC assessment.

  19. Isolation and identification of new phytoconstituents from the fruit extract of Amomum subulatum Roxb.

    PubMed

    Kumar, Gopal; Chauhan, Baby; Ali, Mohammed

    2014-01-01

    The fruits of Amomum subulatum Roxb. (Zingiberaceae) (large cardamom), cultivated in the northern Himalayas, are used to treat stomach disorders, pulmonary diseases and liver complaints. Phytochemical investigation of the fruits led to the isolation of four new chemical compounds characterised as geranil-3(10)-en-9-olyl octadec-9-enoate, geranil-3(10)-en-9-carboxyl-β-D-arabinopyranoside, geranilan-9-carboxy-α-L-arabinopyranoside and stigmast-5-en-3β-ol-3β-D-arabinopyranosyl-2'-(3″-methoxy) benzoate-3'-octadec-9‴,12‴,15‴-trienoate, along with the known compounds oleodilinolein and glyceryl trilinoleniate on the basis of spectral data analysis. PMID:24274834

  20. Encapsulation of ethylhexyl methoxycinnamate, a light-sensitive UV filter, in lipid nanoparticles.

    PubMed

    Durand, L; Habran, N; Henschel, V; Amighi, K

    2010-01-01

    The aim of this study was to encapsulate ethylhexyl methoxycinnamate (EMC), a commonly used UVB filter, in a solid lipid matrix in order to obtain microparticles and then nanoparticles to reduce its photo-instability under UV light exposure. Glyceryl behenate, rice bran wax and ozokerite were investigated for encapsulating EMC. The suspensions of nanoparticles contained 70% encapsulated EMC (relative to the lipid mass). The absorbance level at 310 nm of suspensions containing nanoparticles was more than twice that of those containing microparticles. So, decreasing the size of particles improved the efficiency of light protection, regardless of the lipid material used. Moreover, free EMC presented a 30% loss of its efficiency after 2 h of irradiation, whereas the three NLC formulations showed a loss of absorbency between 10% and 21%. The in vitro cutaneous penetration test did not show a higher potential penetration for EMC contained in nanosuspensions compared to free EMC.

  1. Comprehension of direct extraction of hydrophilic antioxidants using vegetable oils by polar paradox theory and small angle X-ray scattering analysis.

    PubMed

    Li, Ying; Fabiano-Tixier, Anne Sylvie; Ruiz, Karine; Rossignol Castera, Anne; Bauduin, Pierre; Diat, Olivier; Chemat, Farid

    2015-04-15

    Since the polar paradox theory rationalised the fact that polar antioxidants are more effective in nonpolar media, extractions of phenolic compounds in vegetable oils were inspired and achieved in this study for obtaining oils enriched in phenolic compounds. Moreover, the influence of surfactants on the extractability of phenolic compounds was experimentally studied first, followed by the small angle X-ray scattering analysis for the oil structural observation before and after extraction so as to better understand the dissolving mechanism underpinning the extraction. The results showed a significant difference on the extraction yield of phenolic compounds among oils, which was mainly dependent on their composition instead of the unsaturation of fatty acids. Appropriate surfactant additions could significantly improve extraction yield for refined sunflower oils, which 1% w/w addition of glyceryl oleate was determined as the optimal. Besides, 5% w/w addition of lecithin performed the best in oil enrichments compared with mono- and di-glycerides. PMID:25466101

  2. Comprehension of direct extraction of hydrophilic antioxidants using vegetable oils by polar paradox theory and small angle X-ray scattering analysis.

    PubMed

    Li, Ying; Fabiano-Tixier, Anne Sylvie; Ruiz, Karine; Rossignol Castera, Anne; Bauduin, Pierre; Diat, Olivier; Chemat, Farid

    2015-04-15

    Since the polar paradox theory rationalised the fact that polar antioxidants are more effective in nonpolar media, extractions of phenolic compounds in vegetable oils were inspired and achieved in this study for obtaining oils enriched in phenolic compounds. Moreover, the influence of surfactants on the extractability of phenolic compounds was experimentally studied first, followed by the small angle X-ray scattering analysis for the oil structural observation before and after extraction so as to better understand the dissolving mechanism underpinning the extraction. The results showed a significant difference on the extraction yield of phenolic compounds among oils, which was mainly dependent on their composition instead of the unsaturation of fatty acids. Appropriate surfactant additions could significantly improve extraction yield for refined sunflower oils, which 1% w/w addition of glyceryl oleate was determined as the optimal. Besides, 5% w/w addition of lecithin performed the best in oil enrichments compared with mono- and di-glycerides.

  3. Synthesis of ethers by GaBr3 -catalyzed reduction of carboxylic acid esters and lactones by siloxanes.

    PubMed

    Biermann, Ursula; Metzger, Jürgen O

    2014-02-01

    Ethers were synthesized by reduction of the respective esters catalyzed by gallium bromide (GaBr3 ) and using siloxanes, preferentially 1,1,3,3-tetramethyldisiloxane, as reductant. Methyl oleate, triglycerides, that is, tributyrine and glyceryl triundec-10-enoate as well as γ- and δ-lactones were converted into the respective ethers in high to moderate yields. γ-Lactones were reduced with high selectivity in the presence of a methyl ester functionality. The reduction has been carried out at room temperature or moderately elevated temperature of up to 60 °C using stoichiometric amounts of the reductant and 0.005-0.01 equiv of GaBr3 as catalyst per ester functionality without any solvent added. After a reaction time of 1-4 h the conversion of the substrate was 100 %. The product was separated from polymeric siloxanes formed as coupled product by simple distillation. PMID:24488681

  4. Synthesis of ethers by GaBr3 -catalyzed reduction of carboxylic acid esters and lactones by siloxanes.

    PubMed

    Biermann, Ursula; Metzger, Jürgen O

    2014-02-01

    Ethers were synthesized by reduction of the respective esters catalyzed by gallium bromide (GaBr3 ) and using siloxanes, preferentially 1,1,3,3-tetramethyldisiloxane, as reductant. Methyl oleate, triglycerides, that is, tributyrine and glyceryl triundec-10-enoate as well as γ- and δ-lactones were converted into the respective ethers in high to moderate yields. γ-Lactones were reduced with high selectivity in the presence of a methyl ester functionality. The reduction has been carried out at room temperature or moderately elevated temperature of up to 60 °C using stoichiometric amounts of the reductant and 0.005-0.01 equiv of GaBr3 as catalyst per ester functionality without any solvent added. After a reaction time of 1-4 h the conversion of the substrate was 100 %. The product was separated from polymeric siloxanes formed as coupled product by simple distillation.

  5. [Allergic contact dermatitis in beauty parlor clients].

    PubMed

    Gottlöber, P; Gall, H; Bezold, G; Peter, R U

    2001-05-01

    Occupational contact dermatitis in hair dressers and beauticians has increased in importance in the past years. Type IV-allergies against glyceryl monothioglycate components of permanent waves are most common. Other occupational allergens include bleach components such as ammonium persulfate and hair dye ingredients such as p-phenylenediamine (PPD) and p-toluylene-diamine (PTD) base. Allergies to hair dyes in customers of hair dressers have rarely been observed. Two female patients developed allergic contact dermatitis of the scalp and face after repeated use of Polycolor intensivtönung schwarz and of Movida color. We also review the current literature on type IV-allergies to components of hair dressing products components. PMID:11405157

  6. High-Throughput Quantification of Bioactive Lipids by MALDI Mass Spectrometry: Application to Prostaglandins

    PubMed Central

    Manna, Joseph D.; Reyzer, Michelle L.; Latham, Joey C.; Weaver, C. David; Marnett, Lawrence J.; Caprioli, Richard M.

    2011-01-01

    Analysis and quantification of analytes in biological systems is a critical component of metabolomic investigations of cell function. The most widely used methods employ chromatographic separation followed by mass spectrometric analysis, which requires significant time for sample preparation and sequential chromatography. We introduce a novel high-throughput, separation-free methodology based on MALDI mass spectrometry that allows for the parallel analysis of targeted metabolomes. Proof-of-concept is demonstrated by analysis of prostaglandins and glyceryl prostaglandins. Derivatization to incorporate a charged moiety into ketone-containing prostaglandins dramatically increases the signal-to-noise ratio relative to underivatized samples. This resulted in an increased dynamic range (15 fmol – 2000 fmol on plate) and improved linearity (r2= 0.99). The method was adapted for high-throughput screening methods for enzymology and drug discovery. Application to cellular metabolomics was also demonstrated. PMID:21770391

  7. Thickness fluctuations in black lipid membranes.

    PubMed Central

    Hladky, S B; Gruen, D W

    1982-01-01

    Because a black lipid membrane is compressible, there will be spontaneous fluctuations in its thickness. Qualitative arguments are given that the preferred configuration of the membranes is flat and that thickness fluctuations are smaller in amplitude than the differences in mean thickness observed using different hydrocarbon solvents. Fluctuations with short characteristic lengths will not be large as a result of the large amounts of oil-water contact these would entail. Quantitative analysis based on an extension of the treatment for soap films, predicts that the root mean square (rms) amplitude for fluctuations of wavelength longer than approximately 10 nm is negligible for glyceryl monooleate membranes with squalene (less than 3%) but may be approximately 20% with n-decane. rms fluctuations of 20% would lead to a discrepancy between the rms thickness of the core and the mean reciprocal thickness of only 6%. PMID:7104437

  8. Innovations in chronic anal fissure treatment: A systematic review

    PubMed Central

    Poh, Aaron; Tan, Kok-Yang; Seow-Choen, Francis

    2010-01-01

    A chronic anal fissure is a common perianal condition. This review aims to evaluate both existing and new therapies in the treatment of chronic fissures. Pharmacological therapies such as glyceryl trinitrate (GTN), Diltiazem ointment and Botulinum toxin provide a relatively non-invasive option, but with higher recurrence rates. Lateral sphincterotomy remains the gold standard for treatment. Anal dilatation has no role in treatment. New therapies include perineal support devices, Gonyautoxin injection, fissurectomy, fissurotomy, sphincterolysis, and flap procedures. Further research is required comparing these new therapies with existing established therapies. This paper recommends initial pharmacological therapy with GTN or Diltiazem ointment with Botulinum toxin as a possible second line pharmacological therapy. Perineal support may offer a new dimension in improving healing rates. Lateral sphincterotomy should be offered if pharmacological therapy fails. New therapies are not suitable as first line treatments, though they can be considered if conventional treatment fails. PMID:21160880

  9. A dramatic drop in blood pressure following prehospital GTN administration.

    PubMed

    Boyle, Malcolm J

    2007-03-01

    A male in his sixties with no history of cardiac chest pain awoke with chest pain following an afternoon sleep. The patient did not self medicate. The patient's observations were within normal limits, he was administered oxygen via a face mask and glyceryl trinitrate (GTN). Several minutes after the GTN the patient experienced a sudden drop in blood pressure and heart rate, this was rectified by atropine sulphate and a fluid challenge. There was no further deterioration in the patient's condition during transport to hospital. There are very few documented case like this in the prehospital scientific literature. The cause appears to be the Bezold-Jarish reflex, stimulation of the ventricular walls which in turn decreases sympathetic outflow from the vasomotor centre. Prehospital care providers who are managing any patient with a syncopal episode that fails to recover within a reasonable time frame should consider the Bezold-Jarisch reflex as the cause and manage the patient accordingly.

  10. Effects of ascorbic acid supplementation on male reproductive system during exposure to hypoxia

    NASA Astrophysics Data System (ADS)

    Havazhagan, G.; Riar, S. S.; Kain, A. K.; Bardhan, Jaya; Thomas, Pauline

    1989-09-01

    Two groups of male rats were exposed to simulated altitudes of 6060 m and 7576 m for 6 h/day for 7 days (intermittent exposure). In two additional groups of animals exposed to the same altitude, 100 mg of ascorbic acid (AA) was fed daily for 5 days prior to the exposure period and also during the exposure period. Rats that did not receive AA showed loss of body weight and weight of reproductive organs after exposure. Sex organs showed atrophy on histological examination and there was a deterioration in spermatozoal quality. There was an increase in alkaline and acid phosphatase, and decrease in protein, sialic acid and glyceryl phosphorylcholine content in various reproductive tissues after exposure. All the above changes in histology and biochemical composition could be partially prevented by AA supplementation. AA supplementation can therefore protect the male reproductive system from deleterious effects of hypoxia. The probable mechanism of action of AA is discussed.

  11. Microemulsion formed by alkyl polyglucoside and an alkyl glycerol ether with weakly charged films.

    PubMed

    Fukuda; Olsson; Ueno

    2001-02-01

    We have studied the effects on phase equilibria of a nonionic surfactant mixture-water-oil system when replacing small amount of surfactant molecules by ionic surfactant, sodium dodecyl sulfate (SDS). The nonionic surfactant system contains dodecyl-beta-D-maltoside (C(12)AG2) and iso-octyl glyceryl ether (i-C(8)GE) as cosurfactant, water and cyclohexane at constant water to oil ratio of 60/40 (w/w). Adding a small amount of SDS has large impact on the phase behavior. Clear liquid crystalline phase and upper microemulsion phase are added to the phase sequence at high i-C(8)GE/(C(12)AG2+i-C(8)GE) ratio. We also compare the phase equilibria of pure dodecyl maltoside system with polyglucosides mixture system. PMID:11087985

  12. Effect of sterilization on the physical stability of brimonidine-loaded solid lipid nanoparticles and nanostructured lipid carriers.

    PubMed

    El-Salamouni, Noha S; Farid, Ragwa M; El-Kamel, Amal H; El-Gamal, Safaa S

    2015-12-30

    Nanoparticulate delivery systems have recently been under consideration for topical ophthalmic drug delivery. Brimonidine base-loaded solid lipid nanoparticles and nanostructured lipid carrier formulations were prepared using glyceryl monostearate as solid lipid and were evaluated for their physical stability following sterilization by autoclaving at 121°C for 15min. The objective of this work was to evaluate the effect of autoclaving on the physical appearance, particle size, polydispersity index, zeta potential, entrapment efficiency and particle morphology of the prepared formulations, compared to non-autoclaved ones. Results showed that, autoclaving at 121°C for 15min allowed the production of physically stable formulations in nanometric range, below 500nm suitable for ophthalmic application. Moreover, the autoclaved samples appeared to be superior to non-autoclaved ones, due to their increased zeta potential values, indicating a better physical stability. As well as, increased amount of brimonidine base entrapped in the tested formulations.

  13. IN VITRO ORGANIC NITRATE BIOACTIVATION TO NITRIC OXIDE BY RECOMBINANT ALDEHYDE DEHYDROGENASE 3A1

    PubMed Central

    Lin, Shunxin; Page, Nathaniel A.; Fung, Sun Mi; Fung, Ho-Leung

    2013-01-01

    Organic nitrates (ORNs) are commonly used anti-ischemic and anti-anginal agents, which serve as an exogenous source of the potent vasodilator nitric oxide (NO). Recently, both mitochondrial aldehyde dehydrogenase-2 (ALDH2) and cytosolic aldehyde dehydrogenase-1a1 (ALDH1A1) have been shown to exhibit the ability to selectively bioactivate various ORNs in vitro. The objective of the present research was to examine the potential role of ALDH3A1, another major cytosolic isoform of ALDH, in the in vitro bioactivation of various ORNs, and to estimate the enzyme kinetic parameters toward ORNs through mechanistic modeling. The extent of bioactivation was assayed by exposing recombinant ALDH3A1 to various concentrations of ORNs, and measuring the concentration-time profiles of released NO via a NO-specific electrode. Metabolite formation kinetics was monitored for nitroglycerin (NTG) using LC/MS/MS. Our results showed that ALDH3A1 mRNA and protein were highly expressed in C57BL/6 mouse aortic, cardiac, and hepatic tissues, and it was able to release NO from several ORNs, including NTG, isosorbide dinitrate (ISDN), isosorbide-2-mononitrate (IS-2-MN), and nicorandil with similar Vmax (0.175 – 0.503 nmol/min/mg of ALDH3A1), and Km values of 4.01, 46.5, 818 and 5.75 × 103 μM respectively. However, activation of isosorbide-5-mononitrate (IS-5-MN) by ALDH3A1 was undetectable in vitro. ALDH3A1 was also shown to denitrate NTG, producing primarily glyceryl 1, 2-dinitrate (1, 2-GDN) in preference to glyceryl 1, 3-dinitrate (1, 3-GDN). Therefore, ALDH3A1 may contribute to the bioactivation of ORNs in vivo. PMID:24126018

  14. Dobutamine echocardiography and thallium-201 imaging predict functional improvement after revascularisation in severe ischaemic left ventricular dysfunction.

    PubMed Central

    Senior, R.; Glenville, B.; Basu, S.; Sridhara, B. S.; Anagnostou, E.; Stanbridge, R.; Edmondson, S. J.; Handler, C. E.; Raftery, E. B.; Lahiri, A.

    1995-01-01

    OBJECTIVES--To evaluate the concordance between thallium-201 uptake and echocardiographic wall thickening, which are both indicators of potentially reversible myocardial dysfunction, in patients with chronic ischaemic left ventricular failure and to assess their relative contribution to predicting improvement in regional function after revascularisation in a subgroup. PATIENTS AND METHODS--45 patients with chronic ischaemic left ventricular dysfunction (mean (SD) ejection fraction 25 (8)%) underwent echocardiography before and after dobutamine infusion (10 micrograms/kg/min). Of these, 22 patients underwent rest echocardiography at a mean (SD) of 9 (1) weeks after revascularisation. 201Tl imaging was performed during dobutamine echocardiography and at rest, 1, and 4 h after treatment with sublingual glyceryl trinitrate on two separate days. Potentially reversible dysfunction was thought to be present when a myocardial segment contained a Tl score of > or = 3 (ascending score 1-4), or showed improved wall thickening of a dysynergic segment during dobutamine stimulation. RESULTS--Of the 201Tl protocols, the redistribution scan 1 h after treatment with glyceryl trinitrate best demonstrated myocardial viability. Concordance between 201Tl and dobutamine induced wall thickening was 82% (kappa = 0.59) for detecting potentially reversible myocardial dysfunction before revascularisation (n = 45). Regional function improved in 18 of 22 patients after revascularisation. There were 168 dysynergic segments before intervention. The sensitivity of echocardiography and 201Tl imaging for detecting "recoverable" or viable segments after revascularisation was 87% and 92% respectively and specificity was 82% and 78% respectively (P = NS). CONCLUSIONS--Dobutamine echocardiography and 201Tl imaging may be used to predict mechanical improvement in dysynergic segments after revascularisation in patients with chronic ischaemic left ventricular dysfunction. Images PMID:7488446

  15. Comparison of metoprolol tartrate multiple-unit lipid matrix systems produced by different technologies.

    PubMed

    Aleksovski, Aleksandar; Van Bockstal, Pieter-Jan; Roškar, Robert; Sovány, Tamás; Regdon, Géza; De Beer, Thomas; Vervaet, Chris; Dreu, Rok

    2016-06-10

    The aim of this study was to develop, evaluate and compare extended release mini-matrices based on metoprolol tartrate (MPT) and either glyceryl behenate (GB) or glyceryl palmitostearate (GPS). Mini-matrices were produced by three different techniques: hot melt extrusion, compression of melt granulates and prilling. Hot-melt extrusion and compression of granules obtained from melted material proved to be reliable, robust and reproducible techniques with aim of obtaining extended release matrices. Prilling tended to be susceptible to increased melt viscosity. Direct compression was not applicable for mini-matrix production due to poor powder flow. In general MPT release from all matrices was affected by its loading and the size of the units/particles. Processing of GB-MPT mixtures by different techniques did not lead to different drug release rates and patterns, while in case of GPS differently obtained matrices provided diverse MPT release outcomes. Matrices based on GB tended to have higher porosity compared to ones composed of GPS and thus most of the GB-based formulations showed faster drug delivery. FT-IR analysis revealed no interactions between primary components used for matrix production and Raman mapping outlined uniform MPT distribution throughout the units. DSC and X-ray studies revealed significant changes in the crystallinity of glycerides after storage under room conditions (GPS samples) and at increased temperature (GB and GPS samples), which was correlated to the changes seen in drug release rate and pattern after storage. Media composition in general tended to insignificantly affect GB matrices, while in case of GPS matrices increasing the pH and presence of biorelevant compounds induced faster drug release.

  16. The effect of some general anaesthetics on the surface potential of lipid monolayers.

    PubMed

    Bangham, A D; Mason, W

    1979-06-01

    1 This study sought to investigate the report by Ginsberg (1978) that 0.7 M ethanol brought about a + 100 mV change (DeltaDeltaV) in the surface potential of glyceryl monooleate (GMO) monolayers formed on KCl, although he predicted that a DeltaDeltaV of -10 mV should have been found.2 The effect of general anaesthetics such as n-alkyl alcohols and pentobarbitone on surface potential (DeltaV) and surface tension (gamma) of lipid monolayers formed on 145 mM KCl from either glyceryl monooleate (GMO) or phosphatidyl choline (PC) was examined with an Americium-241 air electrode assembly (DeltaV) and a platinized platinum dipping plate and force balance (gamma).3 It was found that, as predicted by Ginsberg (1978), addition of 0.7 M ethanol to the aqueous phase bathing either PC or GMO monolayers brings about a negative-going change in interfacial potential (DeltaDeltaV).4 The magnitude of DeltaDeltaV is dependent in a linear fashion on ethanol concentration.5 Longer chain length alcohols up to n-decanol also bring about a negative going change in DeltaDeltaV, and the dependence of DeltaDeltaV on anaesthetic activity, with respect to increasing chain length of anaesthetic, is consistent with Traube's law.6 Pentobarbitone added to the aqueous phase bathing the monolayer also elicits a negative DeltaDeltaV, a finding which rules out the possibility of adsorption of the volatile alcohols to the measuring electrode.7 The findings are discussed in terms of the proposition that increasing disorder in an array of fixed dipoles, such as might occur in a bilayer exposed to anaesthetic, would result in a lowering of the electrostatic barrier to the predominantly impermeable cation.

  17. Abiotic Condensation Synthesis of Glyceride Lipids and Wax Esters Under Simulated Hydrothermal Conditions

    NASA Astrophysics Data System (ADS)

    Rushdi, Ahmed I.; Simoneit, Bernd R. T.

    2006-04-01

    Precursor compounds for abiotic proto cellular membranes are necessary for the origin of life. Amphipathic compounds such as fatty acids and acyl glycerols are important candidates for micelle/bilayer/vesicle formation. Two sets of experiments were conducted to study dehydration reactions of model lipid precursors in aqueous media to form acyl polyols and wax esters, and to evaluate the stability and reactions of the products at elevated temperatures. In the first set, mixtures of n-nonadecanoic acid and ethylene glycol in water, with and without oxalic acid, were heated at discrete temperatures from 150 ∘C to 300 ∘C for 72 h. The products were typically alkyl alkanoates, ethylene glycolyl alkanoates, ethylene glycolyl bis-alkanoates and alkanols. The condensation products had maximum yields between 150 ∘C and 250 ∘C, and were detectable and thus stable under hydrothermal conditions to temperatures < 300 ∘C. In the second set of experiments, mixtures of n-heptanoic acid and glycerol were heated using the same experimental conditions, with and without oxalic acid, between 100 ∘C and 250 ∘C. The main condensation products were two isomers each of monoacylglycerols and diacylglycerols at all temperatures, as well as minor amounts of the fatty acid anhydride and methyl ester. The yield of glyceryl monoheptanoates generally increased with increasing temperature and glyceryl diheptanoates decreased noticeably with increasing temperature. The results indicate that condensation reactions and abiotic synthesis of organic lipid compounds under hydrothermal conditions occur easily, provided precursor concentrations are sufficiently high.

  18. Vascular Bioactivation of Nitroglycerin by Aldehyde Dehydrogenase-2

    PubMed Central

    Lang, Barbara S.; Gorren, Antonius C. F.; Oberdorfer, Gustav; Wenzl, M. Verena; Furdui, Cristina M.; Poole, Leslie B.; Mayer, Bernd; Gruber, Karl

    2012-01-01

    Aldehyde dehydrogenase-2 (ALDH2) catalyzes the bioactivation of nitroglycerin (glyceryl trinitrate, GTN) in blood vessels, resulting in vasodilation by nitric oxide (NO) or a related species. Because the mechanism of this reaction is still unclear we determined the three-dimensional structures of wild-type (WT) ALDH2 and of a triple mutant of the protein that exhibits low denitration activity (E268Q/C301S/C303S) in complex with GTN. The structure of the triple mutant showed that GTN binds to the active site via polar contacts to the oxyanion hole and to residues 268 and 301 as well as by van der Waals interactions to hydrophobic residues of the catalytic pocket. The structure of the GTN-soaked wild-type protein revealed a thionitrate adduct to Cys-302 as the first reaction intermediate, which was also found by mass spectrometry (MS) experiments. In addition, the MS data identified sulfinic acid as the irreversibly inactivated enzyme species. Assuming that the structures of the triple mutant and wild-type ALDH2 reflect binding of GTN to the catalytic site and the first reaction step, respectively, superposition of the two structures indicates that denitration of GTN is initiated by nucleophilic attack of Cys-302 at one of the terminal nitrate groups, resulting in formation of the observed thionitrate intermediate and release of 1,2-glyceryl dinitrate. Our results shed light on the molecular mechanism of the GTN denitration reaction and provide useful information on the structural requirements for high affinity binding of organic nitrates to the catalytic site of ALDH2. PMID:22988236

  19. [Endocrine disease in adrenoleukodystrophy].

    PubMed

    Girard, S; Bruckert, E; Turpin, G

    2001-02-01

    X-linked adrenoleukodysrophy is the most frequent genetic disorder affecting central and peripheral nervous system myelin. One of the biochemical abnormalities is the accumulation of very long chain fatty acids (VLCFA) in tissues and body fluids subsequent to defective catabolism in the peroxysomes. The principal characteristic of the disease is an association between a neurological disorder and an endocrine disorder: primary adrenal insufficiency and testicular failure. Clinical manifestations are variable. There are two main forms, one affecting boys between the age of 5 and 10 years with severe rapidly fatal cerebral involvement, and the other affecting young adults between the age of 20 and 30 years with degeneration of the anterior and posterior long spinal cord tracts, similar to the disorders observed in multiple sclerosis. About 20% of the heterozygous women may develop a syndrome which resembles adrenomyeloneuropathy, rarely adrenal insufficiency. Adrenal insufficiency is present in 85% of the childhood cerebral forms and in about 70% of the adult forms. It may occur before, after or at the same time as the neurological disease but is not correlated with the severity of the neurological disorder. Careful screening is required to avoid missing subclinical forms. Adrenoleukodystrophy should be envisaged in young boys with primary adrenal insufficiency, accounting for about 30% of the cases of primary adrenal insufficiency in children under 3 years of age and about 13% of those in adults. Experience with dietary therapy (low-VLCFA diet and supplementation with unsaturated fatty acids such as glyceryl trioleate (GTO) and glyceryl trierucate (GTE), commonly called Lorenzo's oil) has not demonstrated any clinical improvement in the cerebral forms. Bone marrow transplantation is recommended for children who show early evidence of cerebral involvement. Gene therapy is a promising perspective. Lovastatin and 4-phenlbutyrate have recently been shown to normalize

  20. Intestinal absorption of retinol and retinyl palmitate in the rat. Effects of tetrahydrolipstatin

    SciTech Connect

    Fernandez, E.; Borgstroem, B. )

    1990-09-01

    The aim of the present study was to characterize the intestinal absorption of retinol and retinyl palmitate in thoracic duct and bile duct fistulated rats and to investigate the effect of a simultaneously administered lipase inhibitor, tetrahydrolipstatin (THL). Absorption was determined as lymphatic recovery over a 24-hr period, including an initial 12-hr continuous intraduodenal infusion of either (11,12-3H)retinol or (11,12-3H)retinyl palmitate given in emulsified glyceryl trioleate or in mixed micellar solution of monoolein and oleic acid. From micellar dispersion, labeled retinol and retinyl palmitate were recovered in the lymph to 50-60% and both to the same extent. Administered in emulsified form, labeled retinol from fed retinyl palmitate was recovered to 47%, but retinol from fed retinol to only 18%. THL (10(-4) M) in the infusate had no significant effect on the recovery of 14C-labeled oleic acid. The recovery of label from emulsified glyceryl tri(1-14C)oleate was significantly decreased at this concentration of THL (76.5% vs 19.6% recovery). When administered in emulsified form, retinol absorption was not significantly affected by THL at 10(-4) M, while retinyl palmitate absorption was very significantly decreased (5.0% compared to 47.8%). In the presence of THL, retinol absorption from retinyl palmitate in micellar solution was decreased (from 58% to 17%). Most of the retinol in the lymph extracts (72.2 to 91.3) was present as retinyl ester, regardless of the chemical and physical form of administration. Furthermore, THL did not induce any change in this pattern.

  1. Self-Assembled Cubic Liquid Crystalline Nanoparticles for Transdermal Delivery of Paeonol

    PubMed Central

    Li, Jian-Chun; Zhu, Na; Zhu, Jin-Xiu; Zhang, Wen-Jing; Zhang, Hong-Min; Wang, Qing-Qing; Wu, Xiao-Xiang; Wang, Xiu; Zhang, Jin; Hao, Ji-Fu

    2015-01-01

    Background The aim of this study was to optimize the preparation method for self-assembled glyceryl monoolein-based cubosomes containing paeonol and to characterize the properties of this transdermal delivery system to improve the drug penetration ability in the skin. Material/Methods In this study, the cubic liquid crystalline nanoparticles loaded with paeonol were prepared by fragmentation of glyceryl monoolein (GMO)/poloxamer 407 bulk cubic gel by high-pressure homogenization. We evaluated the Zeta potential of these promising skin-targeting drug-delivery systems using the Malvern Zeta sizer examination, and various microscopies and differential scanning calorimetry were also used for property investigation. Stimulating studies were evaluated based on the skin irritation reaction score standard and the skin stimulus intensity evaluation standard for paeonol cubosomes when compared with commercial paeonol ointment. In vitro tests were performed on excised rat skins in an improved Franz diffusion apparatus. The amount of paeonol over time in the in vitro penetration and retention experiments both was determined quantitatively by HPLC. Results Stimulating studies were compared with the commercial ointment which indicated that the paeonol cubic liquid crystalline nanoparticles could reduce the irritation in the skin stimulating test. Thus, based on the attractive characteristics of the cubic crystal system of paeonol, we will further exploit the cosmetic features in the future studies. Conclusions The transdermal delivery system of paeonol with low-irritation based on the self-assembled cubic liquid crystalline nanoparticles prepared in this study might be a promising system of good tropical preparation for skin application. PMID:26517086

  2. New alternatives to cosmetics preservation.

    PubMed

    Papageorgiou, S; Varvaresou, A; Tsirivas, E; Demetzos, C

    2010-01-01

    In recent years, there is a considerable interest in the development of preservative-free or self-preserving cosmetics. The aim of our work was to develop new cosmetic formulations by replacing chemical preservatives with ingredients with antimicrobial properties that are not legislated as preservatives according to Annex VI of Commission Directive 76/768/EEC. This paper describes the preservative efficacy of the well-known antimicrobial extracts of Lonicera caprifoleum and Lonicera japonica in combination with glyceryl caprylate and/or levulinic acid, p-anisic acid, and ethanol. We prepared a series of acidic (pH = 5.5) aqueous and O/W formulations, i.e., tonic lotion, shampoo, shower gel, conditioning cream, anticellulite cream, cleansing milk and peeling cream, containing (0.2% w/w) Lonicera extracts, alone in the case of tonic lotion and in combination with (1% w/w) glyceryl caprylate in the other products, and we performed challenge tests according to the European Pharmacopoeia procedures and criteria. Formulations such as shampoo, shower gel, and conditioning cream fulfilled criterion A, while tonic lotion, anticellulite cream, cleansing milk, and peeling cream fulfilled criterion B, in regard to contamination from A. niger. Furthermore, we evaluated the efficacy of the antimicrobial systems in two states of use: the intact product and after three weeks of consumer use. The results showed that A. niger was also detected during use by consumers in the products that satisfied only criterion B in challenge tests. The addition of antimicrobial fragrance ingredients such (< or = 0.3% w/w) levulinic acid or (0.1% w/w) p-anisic acid and/or (5% w/w) ethanol afforded products that met criterion A in challenge tests and were also microbiologically safe during use. The small quantity (5% w/w) of ethanol gave an important assistance in order to boost the self-preserving system and to produce stable and safe products.

  3. Abiotic condensation synthesis of glyceride lipids and wax esters under simulated hydrothermal conditions.

    PubMed

    Rushdi, Ahmed I; Simoneit, Bernd R T

    2006-04-01

    Precursor compounds for abiotic proto cellular membranes are necessary for the origin of life. Amphipathic compounds such as fatty acids and acyl glycerols are important candidates for micelle/bilayer/vesicle formation. Two sets of experiments were conducted to study dehydration reactions of model lipid precursors in aqueous media to form acyl polyols and wax esters, and to evaluate the stability and reactions of the products at elevated temperatures. In the first set, mixtures of n-nonadecanoic acid and ethylene glycol in water, with and without oxalic acid, were heated at discrete temperatures from 150 ( composite function)C to 300 ( composite function)C for 72 h. The products were typically alkyl alkanoates, ethylene glycolyl alkanoates, ethylene glycolyl bis-alkanoates and alkanols. The condensation products had maximum yields between 150 ( composite function)C and 250 ( composite function)C, and were detectable and thus stable under hydrothermal conditions to temperatures < 300 ( composite function)C. In the second set of experiments, mixtures of n-heptanoic acid and glycerol were heated using the same experimental conditions, with and without oxalic acid, between 100 ( composite function)C and 250 ( composite function)C. The main condensation products were two isomers each of monoacylglycerols and diacylglycerols at all temperatures, as well as minor amounts of the fatty acid anhydride and methyl ester. The yield of glyceryl monoheptanoates generally increased with increasing temperature and glyceryl diheptanoates decreased noticeably with increasing temperature. The results indicate that condensation reactions and abiotic synthesis of organic lipid compounds under hydrothermal conditions occur easily, provided precursor concentrations are sufficiently high. PMID:16642268

  4. Characterization of a Novel Alkaline Family VIII Esterase with S-Enantiomer Preference from a Compost Metagenomic Library.

    PubMed

    Lee, Hyun Woo; Jung, Won Kyeong; Kim, Yong Ho; Ryu, Bum Han; Kim, T Doohun; Kim, Jungho; Kim, Hoon

    2016-02-01

    A novel esterase gene, est7K, was isolated from a compost metagenomic library. The gene encoded a protein of 411 amino acids and the molecular mass of the Est7K was estimated to be 44,969 Da with no signal peptide. Est7K showed the highest identity of 57% to EstA3, which is an esterase from a drinking water metagenome, when compared with the enzymes with reported properties. Est7K had three motifs, SMTK, YSV, and WGG, which correspond to the typical motifs of family VIII esterases, SxxK, Yxx, and WGG, respectively. Est7K did not have the GxSxG motif in most lipolytic enzymes. Three additional motifs, LxxxPGxxW, PLGMxDTxF, and GGxG, were found to be conserved in family VIII enzymes. The results of the phylogenetic analysis and the alignment study suggest that family VIII enzymes could be classified into two subfamilies, VIII.1 and VIII.2. The purified Est7K was optimally active at 40°C and pH 10.0. It was activated to exhibit a 2.1-fold higher activity by the presence of 30% methanol. It preferred short-length p-nitrophenyl esters, particularly p-nitrophenyl butyrate, and efficiently hydrolyzed glyceryl tributyrate. It did not hydrolyze β-lactamase substrates, tertiary alcohol esters, glyceryl trioleate, fish oil, and olive oil. Est7K preferred an Senantiomer, such as (S)-methyl-3-hydroxy-2-methylpropionate, as the substrate. The tolerance to methanol and the substrate specificity may provide potential advantage in the use of the enzyme in pharmaceutical and other biotechnological processes.

  5. Formulation Development, Process Optimization, and In Vitro Characterization of Spray-Dried Lansoprazole Enteric Microparticles.

    PubMed

    Vora, Chintan; Patadia, Riddhish; Mittal, Karan; Mashru, Rajashree

    2016-01-01

    This research focuses on the development of enteric microparticles of lansoprazole in a single step by employing the spray drying technique and studies the effects of variegated formulation/process variables on entrapment efficiency and in vitro gastric resistance. Preliminary trials were undertaken to optimize the type of Eudragit and its various levels. Further trials included the incorporation of plasticizer triethyl citrate and combinations of other polymers with Eudragit S 100. Finally, various process parameters were varied to investigate their effects on microparticle properties. The results revealed Eudragit S 100 as the paramount polymer giving the highest gastric resistance in comparison to Eudragit L 100-55 and L 100 due to its higher pH threshold and its polymeric backbone. Incorporation of plasticizer not only influenced entrapment efficiency, but diminished gastric resistance severely. On the contrary, polymeric combinations reduced entrapment efficiency for both sodium alginate and glyceryl behenate, but significantly influenced gastric resistance for only sodium alginate and not for glyceryl behenate. The optimized process parameters were comprised of an inlet temperature of 150°C, atomizing air pressure of 2 kg/cm(2), feed solution concentration of 6% w/w, feed solution spray rate of 3 ml/min, and aspirator volume of 90%. The SEM analysis revealed smooth and spherical shape morphologies. The DSC and PXRD study divulged the amorphous nature of the drug. Regarding stability, the product was found to be stable under 3 months of accelerated and long-term stability conditions as per ICH Q1A(R2) guidelines. Thus, the technique offers a simple means to generate polymeric enteric microparticles that are ready to formulate and can be directly filled into hard gelatin capsules. PMID:27222612

  6. Simultaneous determination of nitroglycerin and dinitrate metabolites in metabolism studies using liquid chromatography-mass spectrometry with electrospray ionization.

    PubMed

    Miyayama, Takashi; Tsou, Pei-Suen; Fung, Sun-Mi; Fung, Ho-Leung

    2006-05-01

    We have developed a liquid chromatographic-mass spectrometric method for the simultaneous determination of nitroglycerin (NTG) and its active metabolites, glyceryl 1,2-dinitrate (1,2-GDN) and glyceryl 1,3-dinitrate (1,3-GDN), for metabolism studies in cell cultures. 1,2,4-Butanetriol-1,4-dinitrate was chosen as an internal standard. Using a linear gradient of water/methanol containing 0.025 mM NH(4)Cl, the compounds were eluted within 12.5 min on an Allure Aqueous C(18) column (100 mm x 2.1 mm). Detection and quantification was achieved with multiple reaction monitoring in the negative ion mode. Intra- and inter-day variabilities for simultaneous determination of the three nitrates were below 10 and 18%, respectively, over a range of NTG and GDN concentrations of 0.5-15 ng/ml. The lower limit of quantification was found to be about 0.01 ng on column. Application of this method was illustrated through in vitro metabolism studies of NTG in culture media bathing LLC-PK1 cells and human vascular smooth muscle cells (HA-VSMC) at 37 degrees C. The degradation half-life of NTG was found to be 4.5 +/- 0.4 h and 39.2 +/- 0.02 h, respectively, for LLC-PK1 cells versus HA-VSMC. At 5 h, the 1,2-GDN versus 1,3-GDN metabolite distribution ratio in the bathing medium was found to be 1.5 +/- 0.1 and 0.2 +/- 0.02 for LLC-PK1 and HA-VSMC cells, respectively. With this method, the degradation half-life of NTG in rat plasma at 37 degrees C was shown to be 26.8 +/- 1.8 min, consistent with previous values obtained using gas chromatography.

  7. Comparison of metoprolol tartrate multiple-unit lipid matrix systems produced by different technologies.

    PubMed

    Aleksovski, Aleksandar; Van Bockstal, Pieter-Jan; Roškar, Robert; Sovány, Tamás; Regdon, Géza; De Beer, Thomas; Vervaet, Chris; Dreu, Rok

    2016-06-10

    The aim of this study was to develop, evaluate and compare extended release mini-matrices based on metoprolol tartrate (MPT) and either glyceryl behenate (GB) or glyceryl palmitostearate (GPS). Mini-matrices were produced by three different techniques: hot melt extrusion, compression of melt granulates and prilling. Hot-melt extrusion and compression of granules obtained from melted material proved to be reliable, robust and reproducible techniques with aim of obtaining extended release matrices. Prilling tended to be susceptible to increased melt viscosity. Direct compression was not applicable for mini-matrix production due to poor powder flow. In general MPT release from all matrices was affected by its loading and the size of the units/particles. Processing of GB-MPT mixtures by different techniques did not lead to different drug release rates and patterns, while in case of GPS differently obtained matrices provided diverse MPT release outcomes. Matrices based on GB tended to have higher porosity compared to ones composed of GPS and thus most of the GB-based formulations showed faster drug delivery. FT-IR analysis revealed no interactions between primary components used for matrix production and Raman mapping outlined uniform MPT distribution throughout the units. DSC and X-ray studies revealed significant changes in the crystallinity of glycerides after storage under room conditions (GPS samples) and at increased temperature (GB and GPS samples), which was correlated to the changes seen in drug release rate and pattern after storage. Media composition in general tended to insignificantly affect GB matrices, while in case of GPS matrices increasing the pH and presence of biorelevant compounds induced faster drug release. PMID:26980237

  8. Targeted delivery of a model immunomodulator to the lymphatic system: comparison of alkyl ester versus triglyceride mimetic lipid prodrug strategies.

    PubMed

    Han, Sifei; Quach, Tim; Hu, Luojuan; Wahab, Anisa; Charman, William N; Stella, Valentino J; Trevaskis, Natalie L; Simpson, Jamie S; Porter, Christopher J H

    2014-03-10

    A lipophilic prodrug approach has been used to promote the delivery of a model immunomodulator, mycophenolic acid (MPA), to the lymphatic system after oral administration. Lymphatic transport was employed to facilitate enhanced drug uptake into lymphocytes, as recent studies demonstrate that targeted drug delivery to lymph resident lymphocytes may enhance immunomodulatory effects. Two classes of lymph-directing prodrugs were synthesised. Alkyl chain derivatives (octyl mycophenolate, MPA-C8E; octadecyl mycophenolate, MPA-C18E; and octadecyl mycophenolamide, MPA-C18AM), to promote passive partitioning into lipids in lymphatic transport pathways, and a triglyceride mimetic prodrug (1,3-dipalmitoyl-2-mycophenoloyl glycerol, 2-MPA-TG) to facilitate metabolic integration into triglyceride deacylation-reacylation pathways. Lymphatic transport, lymphocyte uptake and plasma pharmacokinetics were assessed in mesenteric lymph and carotid artery cannulated rats following intraduodenal infusion of lipid-based formulations containing MPA or MPA prodrugs. Patterns of prodrug hydrolysis in rat digestive fluid, and cellular re-esterification in vivo, were evaluated to examine the mechanisms responsible for lymphatic transport. Poor enzyme stability and low absorption appeared to limit lymphatic transport of the alkyl derivatives, although two of the three alkyl chain prodrugs - MPA-C18AM (6-fold) and MPA-C18E (13-fold) still increased lymphatic drug transport when compared to MPA. In contrast, 2-MPA-TG markedly increased lymphatic drug transport (80-fold) and drug concentrations in lymphocytes (103-fold), and this was achieved via biochemical incorporation into triglyceride deacylation-reacylation pathways. The prodrug was hydrolysed rapidly to 2-mycophenoloyl glycerol (2-MPA-MG) in the presence of rat digestive fluid, and 2-MPA-MG was subsequently re-esterified in the enterocyte with oleic acid (most likely originating from the co-administered formulation) prior to accessing the

  9. Targeted delivery of a model immunomodulator to the lymphatic system: comparison of alkyl ester versus triglyceride mimetic lipid prodrug strategies.

    PubMed

    Han, Sifei; Quach, Tim; Hu, Luojuan; Wahab, Anisa; Charman, William N; Stella, Valentino J; Trevaskis, Natalie L; Simpson, Jamie S; Porter, Christopher J H

    2014-03-10

    A lipophilic prodrug approach has been used to promote the delivery of a model immunomodulator, mycophenolic acid (MPA), to the lymphatic system after oral administration. Lymphatic transport was employed to facilitate enhanced drug uptake into lymphocytes, as recent studies demonstrate that targeted drug delivery to lymph resident lymphocytes may enhance immunomodulatory effects. Two classes of lymph-directing prodrugs were synthesised. Alkyl chain derivatives (octyl mycophenolate, MPA-C8E; octadecyl mycophenolate, MPA-C18E; and octadecyl mycophenolamide, MPA-C18AM), to promote passive partitioning into lipids in lymphatic transport pathways, and a triglyceride mimetic prodrug (1,3-dipalmitoyl-2-mycophenoloyl glycerol, 2-MPA-TG) to facilitate metabolic integration into triglyceride deacylation-reacylation pathways. Lymphatic transport, lymphocyte uptake and plasma pharmacokinetics were assessed in mesenteric lymph and carotid artery cannulated rats following intraduodenal infusion of lipid-based formulations containing MPA or MPA prodrugs. Patterns of prodrug hydrolysis in rat digestive fluid, and cellular re-esterification in vivo, were evaluated to examine the mechanisms responsible for lymphatic transport. Poor enzyme stability and low absorption appeared to limit lymphatic transport of the alkyl derivatives, although two of the three alkyl chain prodrugs - MPA-C18AM (6-fold) and MPA-C18E (13-fold) still increased lymphatic drug transport when compared to MPA. In contrast, 2-MPA-TG markedly increased lymphatic drug transport (80-fold) and drug concentrations in lymphocytes (103-fold), and this was achieved via biochemical incorporation into triglyceride deacylation-reacylation pathways. The prodrug was hydrolysed rapidly to 2-mycophenoloyl glycerol (2-MPA-MG) in the presence of rat digestive fluid, and 2-MPA-MG was subsequently re-esterified in the enterocyte with oleic acid (most likely originating from the co-administered formulation) prior to accessing the

  10. Innovative combination of QuEChERS extraction with on-line solid-phase extract purification and pre-concentration, followed by liquid chromatography-tandem mass spectrometry for the determination of non-steroidal anti-inflammatory drugs and their metabolites in sewage sludge.

    PubMed

    Rossini, D; Ciofi, L; Ancillotti, C; Checchini, L; Bruzzoniti, M C; Rivoira, L; Fibbi, D; Orlandini, S; Del Bubba, M

    2016-09-01

    For the first time QuEChERS extraction of sewage sludge was combined with the automatic solid-phase pre-concentration and purification of the extract (following indicated as SPE) and LC-MS/MS analysis, for the determination of the non-steroidal anti-inflammatory drugs acetylsalicylic acid (ASA), diclofenac (DIC), fenbufen (FEN), flurbiprofen (FLU), ketoprofen (KET), ibuprofen (IBU) and naproxen (NAP), and their metabolites salicylic acid (SAL), 4'-hydroxydiclofenac (4'-HYDIC), 1-hydroxyibuprofen (1-HYIBU), 2-hydroxyibuprofen (2-HYIBU), 3-hydroxyibuprofen (3-HYIBU) and o-desmethylnaproxen (O-DMNAP). Various commercial pellicular stationary phases (i.e. silica gel functionalized with octadecyl, biphenyl, phenylhexyl and pentafluorophenyl groups) were preliminarily investigated for the resolution of target analytes and different sorbent phases (i.e. octyl or octadecyl functionalized silica gel and a polymeric phase functionalized with N-benzylpyrrolidone groups) were tested for the SPE phase. The optimized method involves the QuEChERS extraction of 1 g of freeze-dried sludge with 15 mL of water/acetonitrile 1/2 (v/v), the SPE of the extract with the N-benzylpyrrolidone polymeric phase and the water/acetonitrile gradient elution on the pentafluorophenyl stationary phase at room temperature. Matrix effect was always suppressive and in most cases low, being it ≤20% for ASA, DIC, FLU, KET, IBU, 1-HYIBU, 2-HYIBU, 3-HYIBU, NAP and O-DMNAP, and included in the range of 35-47% for the other analytes. Recoveries were evaluated at three spiking levels, evidencing almost quantitative values for HYIBUs and O-DMNAP; for ASA, SAL and KET the recoveries were included in between 50 and 76%, whereas for the other compounds they ranged from 36% to 55%. The proposed method showed better analytical performances than those so far published, being suitable for target compound determination in real samples from tens of pg g(-1) to ng g(-1) of freeze-dried sludge, with a total analysis

  11. Restricted access magnetic materials prepared by dual surface modification for selective extraction of therapeutic drugs from biological fluids

    NASA Astrophysics Data System (ADS)

    Wang, Yu; Wang, Yuxia; Chen, Lei; Wan, Qian-Hong

    2012-02-01

    Magnetic porous particles with dual functionality have been prepared by a two-step procedure and evaluated as novel restricted access materials for extraction of therapeutic agents from biological fluids. The magnetic silica particles served as scaffolds were first modified with diol groups, which were then converted to octadecyl esters through reaction with stearoyl chloride. In the second step, the octadecyl esters on the exterior surface were hydrolyzed by the action of lipase to yield magnetic particles with hydrophobic reversed-phase ligands on the inner surface and biocompatible diol groups on the outer surface. The restricted access behavior of the resulting materials was confirmed by differential binding of small molecules such as methotrexate (MTX), leucovorin (LV) and folic acid (FA) relative to bovine serum albumin. While MTX, LV and FA were all bound to the magnetic particles with high affinity, the adsorption of the protein was markedly reduced due to size exclusion effect. The utility of the magnetic particles for sample preparation was tested in solid-phase extraction of MTX, LV and FA from spiked human serum and the effects of the SPE conditions on the recovery of the analytes were systematically studied. Moreover, the magnetic particle-based sample preparation procedure coupled with reversed-phase liquid chromatography analysis was validated in terms of specificity, linearity and reproducibility. The method was shown to be free from interference of endogenous compounds and linear over the concentration range of 0.5-10 μg/mL for the three drugs studied. The limits of detection for the three drugs in serum were in the range of 0.160-0.302 μg/mL. Reproducibility expressed as the RSD of the recovery for ten replicated extractions at three different concentrations was found to be less than 8.93%. With a unique combination of surface functionality with magnetic cores, the restricted access magnetic particles may be adapted in automated and high

  12. Steam pretreatment for coal liquefaction

    NASA Astrophysics Data System (ADS)

    Ivanenko, Olga

    The objectives of this work are to test the application of steam pretreatment to direct coal liquefaction, to investigate the reaction of model compounds with water, and to explore the use of zeolites in these processes. Previous work demonstrated the effectiveness of steam pretreatment in a subsequent flash pyrolysis. Apparently, subcritical steam ruptures nearly all of the ether cross links, leaving a partially depolymerized structure. It was postulated that very rapid heating of the pretreated coal to liquefaction conditions would be required to preserve the effects of such treatment. Accordingly, a method was adopted in which coal slurry is injected into a hot autoclave containing solvent. Since oxygen is capable of destroying the pretreatment effect, precautions were taken for its rigorous exclusion. Tests were conducted with Illinois No. 6 coal steam treated at 340sp°C, 750 psia for 15 minutes. Both raw and pretreated samples were liquified in deoxygenated tetralin at high severity (400sp°C, 30 min.) and low severity (a: 350sp°C, 30 min., and b: 385sp°C, 15 min.) conditions under 1500 psia hydrogen. Substantial improvement in liquid product quality was obtained and the need for rapid heating and oxygen exclusion demonstrated. Under low severity conditions, the oil yield was more than doubled, going from 12.5 to 29 wt%. Also chemistry of the pretreatment process was studied using aromatic ethers as model compounds. alpha-Benzylnaphthyl ether (alpha-BNE), alpha-naphthylmethyl phenyl (alpha-NMPE), and 9-phenoxyphenanthrene were exposed to steam and inert gas at pretreatment conditions and in some cases to liquid water at 315sp°C. alpha-BNE and alpha-NMPE showed little difference in conversion in inert gas and in steam. Hence, these compounds are poor models for coal in steam pretreatment. Thermally stable 9-phenoxyphenanthrene, however, was completely converted in one hour by liquid water at 315sp°C. At pretreatment conditions mostly rearranged starting

  13. Comprehensive analytical methodology to determine hydrocarbons in marine waters using extraction disks coupled to glass fiber filters and compound-specific isotope analyses.

    PubMed

    Ternon, Eva; Tolosa, Imma

    2015-07-24

    Solid-phase extraction of both aliphatic (AHs) and aromatic polycyclic hydrocarbons (PAHs) from seawater samples was evaluated using a GFF filter stacked upon an octadecyl bonded silica (C18) disk. Stable-isotope measurements were developed on hydrocarbons extracted from both GFF and C18-disks in order to characterize the source of hydrocarbons. A clear partition of hydrocarbon compounds between the dissolved and the particulate phase was highlighted. PAHs showed a higher affinity with the dissolved phase (recoveries efficiency of 48-71%) whereas AHs presented strong affinity with the particulate phase (up to 76% of extraction efficiency). Medium volumes of seawater samples were tested and no breakthrough was observed for a 5L sample. Isotopic fractionation was investigated within all analytical steps but none was evidenced. This method has been applied to harbor seawater samples and very low AH and PAH concentrations were achieved. Due to the low concentration levels of hydrocarbons in the samples, the source of hydrocarbons was determined by molecular indices rather than isotopic measurements and a pyrolytic origin was evidenced. The aliphatic profile also revealed the presence of long-chain linear alkylbenzenes (LABs). The methodology presented here would better fit to polluted coastal environments affected by recent oil spills.

  14. Effect of the precise branching of polyethylene at each 21st CH2 group on its phase transitions, crystal structure, and morphology

    SciTech Connect

    Qui, Wulin; Sworen, John; Pyda, Marek {nmn}; Nowak-Pyda, Elisabieta; Habenschuss, Anton {Tony}; Wagener, Kenneth; Wunderlich, Bernhard {nmn}

    2006-01-01

    Three linear polyethylenes with branches at every 21st backbone atom have been analyzed by differential scanning calorimetry (DSC) and quasi-isothermal, temperature-modulated DSC. The branches were methyl (PE1M), dimethyl (PE2M), and ethyl groups (PE1E). Linear polyethylene (HDPE) and atactic poly(octadecyl acrylate) (PODA) were also analyzed. All were compared to a random poly(ethylene-co-octene-1) of similar branch concentration (LLDPE) and poly(4,4'-phthaloimidobenzoyldoeicosyleneoxycarbonyl) (PEIM-22). The HDPE has the highest melting temperature and crystallinity with relatively large contributions of reversing melting when grown as folded-chain crystals. The precisely branched polyethylenes and copolymers have lower melting temperatures and heats of fusion. Of the branched samples, PE1M crystallizes more readily, followed by PE1E and PE2M, with PE2M showing cold crystallization. In contrast to paraffins of equal length which melt fully reversibly, the precisely designed, branched polymers melt largely irreversibly with small amounts of reversing melting, which is least for the best-grown crystals. The PE1M forms monoclinic, PE1E, pseudohexagonal, or triclinic crystals, and PE2M has a multitude of crystal structures.

  15. Online polar two phase countercurrent chromatography×high performance liquid chromatography for preparative isolation of polar polyphenols from tea extract in a single step.

    PubMed

    Chen, Wei-Bin; Li, Shu-Qi; Chen, Long-Jiang; Fang, Mei-Juan; Chen, Quan-Cheng; Wu, Zhen; Wu, Yun-Long; Qiu, Ying-Kun

    2015-08-01

    Herein, we report an on-line two-dimensional system constructed by counter-current chromatography (CCC) coupling with preparative high-performance liquid chromatography (prep-HPLC) for the separation and purification of polar natural products. The CCC was used as the first dimensional isolation column, where an environmental friendly polar two-phase solvent system of isopropanol and 16% sodium chloride aqueous solution (1:1.2, v/v) was introduced for low toxicity and favorable resolution. In addition, by applying the stop-and-go flow technique, effluents pre-fractionated by CCC was further purified by a preparative column packed with octadecyl silane (ODS) as the second dimension. The interface between the two dimensions was comprised of a 6-port switching valve and an electronically controlled 2-position 10-port switching valve connected with two equivalent holding columns. To be highlighted here, this rationally designed interface for the purpose of smooth desalination, absorption and desorption, successfully solved the solvent compatibility problem between the two dimensional separation systems. The present integrated system was successfully applied in a one-step preparative separation and identification of 10 pure compounds from the water extracts of Tieguanyin tea (Chinese oolong tea). In short, all the results demonstrated that the on-line 2D CCC×LC method is an efficient and green approach for harvesting polar targets in a single step, which showed great promise in drug discovery.

  16. Analysis of nucleic acids by capillary ion-pair reversed-phase HPLC coupled to negative-ion electrospray ionization mass spectrometry.

    PubMed

    Huber, C G; Krajete, A

    1999-09-01

    Ion-pair reversed-phase high-performance liquid chromatography was successfully coupled to negative-ion electrospray ionization mass spectrometry by using 60 × 0.20 mm i.d. capillary columns packed with 2.3-μm micropellicular, octadecylated poly(styrene/divinylbenzene) particles as stationary phase and gradients of acetonitrile in 50 mM aqueous triethylammonium bicarbonate as mobile phase. Systematic variation of the eluent composition, such as concentration of ion-pair reagent, anion in the ion-pair reagent, solution pH, and acetonitrile concentration led to the conclusion that most parameters have opposite effects on chromatographic and mass spectrometric performances. The use of acetonitrile as sheath liquid enabled the rapid and highly efficient separation and detection of phosphorylated and nonphosphorylated oligonucleotides ranging in size from 8 to 40 nucleotides. High-quality full-scan mass spectra showing little cation adduction were acquired from which the molecular masses of the separated oligonucleotides were calculated with an accuracy of 0.011%. With calibration curves being linear over at least 2 orders of magnitude, the lower limits of detection for a oligodeoxythymidine 16-mer were 104 fmol with full scan and 710 amol with selected-ion-monitoring data acquisition. The potential of ion-pair reversed-phase high-performance liquid chromatography-electrospray ionization mass spectrometry was demonstrated for mixed-sequence oligomers by the characterization of a reaction mixture from solid-phase synthesis of a 40-mer oligonucleotide.

  17. Magnetic alignment study of rare-earth-containing liquid crystals.

    PubMed

    Galyametdinov, Yury G; Haase, Wolfgang; Goderis, Bart; Moors, Dries; Driesen, Kris; Van Deun, Rik; Binnemans, Koen

    2007-12-20

    The liquid-crystalline rare-earth complexes of the type [Ln(LH)3(DOS)3]-where Ln is Tb, Dy, Ho, Er, Tm, or Yb; LH is the Schiff base N-octadecyl-4-tetradecyloxysalicylaldimine; and DOS is dodecylsulfate-exhibit a smectic A phase. Because of the presence of rare-earth ions with a large magnetic anisotropy, the smectic A phase of these liquid crystals can be easier aligned in an external magnetic field than smectic A phases of conventional liquid crystals. The magnetic anisotropy of the [Ln(LH)3(DOS)3] complexes was determined by measurement of the temperature-dependence of the magnetic susceptibility using a Faraday balance. The highest value for the magnetic anisotropy was found for the dysprosium(III) complex. The magnetic alignment of these liquid crystals was studied by time-resolved synchrotron small-angle X-ray scattering experiments. Depending on the sign of the magnetic anisotropy, the director of the liquid-crystalline molecules was aligned parallel or perpendicular to the magnetic field lines. A positive value of the magnetic anisotropy (and parallel alignment) was found for the thulium(III) and the ytterbium(III) complexes, whereas a negative value of the magnetic anisotropy (and perpendicular alignment) was observed for the terbium(III) and dysprosium(III) complexes. PMID:18044875

  18. A new phenanthrene derivative and two diarylheptanoids from the roots of Brassica rapa ssp. campestris inhibit the growth of cancer cell lines and LDL-oxidation.

    PubMed

    Wu, Qian; Cho, Jin-Gyeong; Yoo, Ki-Hyun; Jeong, Tae-Sook; Park, Ji-Hae; Kim, Su-Yeon; Kang, Ji-Hyun; Chung, In-Sik; Choi, Myung-Sook; Lee, Kyung-Tae; Chung, Hae-Gon; Bang, Myun-Ho; Baek, Nam-In

    2013-04-01

    Brassica rapa ssp. campestris (Brassicaceae) is a conical, deep purple, edible root vegetable commonly known as a turnip. We initiated phytochemical and pharmacological studies to search for biological active compounds from the roots of B. rapa ssp. campestris. We isolated a novel phenanthrene derivative, 6-methoxy-1-[10-methoxy-7-(3-methylbut-2-enyl)phenanthren-3-yl]undecane-2,4-dione, named brassicaphenanthrene A (3) along with two known diarylheptanoid compounds, 6-paradol (1) and trans-6-shogaol (2), through the repeated silica gel (SiO2), octadecyl silica gel, and Sephadex LH-20 column chromatography. The chemical structures of the compounds were determined by spectroscopic data analyses including nuclear magnetic resonance, mass spectrometry, ultraviolet spectroscopy, and infra-red spectroscopy. All compounds exhibited high inhibitory activity against the growth of human cancer lines, HCT-116, MCF-7, and HeLa, with IC50 values ranging from 15.0 to 35.0 μM and against LDL-oxidation with IC50 values ranging from 2.9 to 7.1 μM.

  19. A simple and efficient multi-residue method based on QuEChERS for pesticides determination in palm oil by liquid chromatography time-of-flight mass spectrometry.

    PubMed

    Sobhanzadeh, Elham; Abu Bakar, Nor Kartini; Bin Abas, Mhd Radzi; Nemati, Keivan

    2012-09-01

    In this study, a rapid, specific and sensitive multi-residue method based on acetonitrile extraction followed by dispersive solid-phase extraction (d-SPE) clean-up was implemented and validated for multi-class pesticide residues determination in palm oil for the first time. Liquid-liquid extraction followed by low-temperature precipitation procedure was evaluated in order to study the freezing-out clean-up efficiency to obtain high recovery yield and low co-extract fat residue in the final extract. For clean-up step, d-SPE was carried out using a combination of anhydrous magnesium sulphate (MgSO(4)), primary secondary amine, octadecyl (C(18)) and graphitized carbon black. Recovery study was performed at two concentration levels (10 and 100 ng g(-1)), yielding recovery rates between 74.52% and 97.1% with relative standard deviation values below 10% (n = 6) except diuron. Detection and quantification limits were lower than 5 and 9 ng g(-1), respectively. In addition, soft matrix effects (≤±20%) were observed for most of the studied pesticides except malathion that indicated medium (20-50%) matrix effects. The proposed method was successfully applied to the analysis of suspected palm oil samples.

  20. Interaction of planar and nonplanar organic contaminants with coal fly ash: Effects of polar and nonpolar solvent solutions

    SciTech Connect

    Burgess, R.M.; Ryba, S.A.; Cantwell, M.G.; Gundersen, J.L.; Tien, R.; Perron, M.M.

    2006-08-15

    Coal fly ash has a very high sorption capacity for a variety of anthropogenic contaminants and has been used to cleanse wastewater of pollutants for approximately 40 years. Like other black carbons, the planar structure of the residual carbon in fly ash results in elevated affinities for planar organic contaminants, such as polycyclic aromatic hydrocarbons (PAHs) and some polychlorinated biphenyls (PCBs). The present study was performed to understand better the mechanisms affecting the strong interaction between planar contaminants and coal fly ash. The removal of 10 PCBs and 10 PAHs by several fly ashes and other sorbents was evaluated under different experimental conditions to highlight the intermolecular forces influencing adsorption. Varying fly ash concentration and solvent system composition indicated that dispersive interactions were most prevalent. For the PCBs, empirical results also were compared to molecular modeling estimates of the energy necessary for the PCB molecule to assume a planar conformation (PCe). The PCe levels ranged from 8 to 25 kcal/mol, depending on the degree of ortho-substituted chlorination of the PCB. A significant correlation between PCe and PCB removal from solution was observed for the fly ashes and activated carbon, whereas the nonplanar sorbent octadecyl (C{sub 18}) indicated no relationship. These findings demonstrate the strong interaction between black carbon fly ash and planar organic contaminants. Furthermore, as exemplified by the PCBs, these results show how this interaction is a function of a contaminant's ability to assume a planar conformation.

  1. Greening pharmaceutical applications of liquid chromatography through using propylene carbonate-ethanol mixtures instead of acetonitrile as organic modifier in the mobile phases.

    PubMed

    Tache, Florentin; Udrescu, Stefan; Albu, Florin; Micăle, Florina; Medvedovici, Andrei

    2013-03-01

    Substitution of acetonitrile (ACN) as organic modifier in mobile phases for liquid chromatography by mixtures of propylene carbonate (PC) and ethanol (EtOH) may be considered a greener approach for pharmaceutical applications. Such a replacement is achievable without any major compromise in terms of elution order, chromatographic retention, efficiency and peak symmetry. This has been equally demonstrated for reverse phase (RP), ion pair formation (IP) and hydrophilic interaction liquid chromatography (HILIC) separation modes. The impact on the sensitivity induced by the replacement between these organic solvents is discussed for UV-vis and mass spectrometric detection. A comparison between Van Deemter plots obtained under elution conditions based on ACN and PC/EtOH is presented. The alternative elution modes were also compared in terms of thermodynamic parameters, such as standard enthalpy (ΔH⁰) and entropic contributions to the partition between the mobile and the stationary phases, for some model compounds. Van't Hoff plots demonstrated that differences between the thermodynamic parameters are minor when shifting from ACN/water to PC/EtOH/water elution on an octadecyl chemically modified silicagel stationary phase. As long as large volume injection (LVI) of diluents non-miscible with the mobile phase is a recently developed topic having a high potential of greening the sample preparation procedures through elimination of the solvent evaporation stage, this feature was also assessed in the case of ACN replacement by PC/EtOH. PMID:23277155

  2. Interfacial Modification of Silica Surfaces Through gamma-Isocyanatopropyl Triethoxy Silane-Amine Coupling Reactions

    SciTech Connect

    Vogel,B.; DeLongchamp, D.; Mahoney, C.; Lucas, L.; Fischer, D.; Lin, E.

    2008-01-01

    The development of robust, cost-effective methods to modify surfaces and interfaces without the specialized synthesis of unique coupling agents could provide readily accessible routes to optimize and tailor interfacial properties. We demonstrate that -isocyanatopropyl triethoxysilane (ISO) provides a convenient route to functionalize silica surfaces through coupling reactions with readily available reagents. ISO coupling agents layers (CALs) can be prepared from toluene with triethylamine (TEA), but the coupling reaction of an amine to the ISO CAL does not proceed. We use near edge X-ray absorption fine structure (NEXAFS), time-of-flight secondary ion mass spectrometry (TOF-SIMS) and sessile drop contact angle to demonstrate the isocyanate layer is not degraded under coupling conditions. Access to silanes with chemical functionality is possible with ISO by performing the coupling reaction in solution and then depositing the product onto the surface. Two model CAL surfaces are prepared to demonstrate the ease and robust nature of this procedure. The surfaces prepared using this method are the ISO reacted with octadecylamine to produce a hydrocarbon surface of similar quality to octadecyl trichlorosilane (OTS) CALs and with 9-aminofluorene (AFL), an aromatic amine functionality whose silane is otherwise unavailable commercially.

  3. Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

    2015-09-30

    A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

  4. Impact of fatty acid chain length of rosmarinate esters on their antimicrobial activity against Staphylococcus carnosus LTH1502 and Escherichia coli K-12 LTH4263.

    PubMed

    Suriyarak, Sarisa; Bayrasy, Christelle; Schmidt, Herbert; Villeneuve, Pierre; Weiss, Jochen

    2013-09-01

    The effect of the addition of a newly synthesized series of rosmarinic acid (RA) estes (REs) and alcohols with chain lengths of 1, 4, 8, 10, 12, 16, and 18 carbons (RE1 to 18) on the growth behavior of Staphylococcus carnosus LTH1502 and Escherichia coli K-12 LTH4263 was investigated. An initial microtiter dilution assay indicated activity of compounds against S. carnosus LTH1502, whereas esters with chain lengths, RA, n-methyl rosmarinate (RE1), n-dodecyl rosmarinate (RE12), and n-octadecyl rosmarinate (RE18) were used in a time-kill assay S. carnosus LTH1502. Compounds were added at 0.75 mM in the log phase, 5 mM in the exponential phase, 10 mM in the stationary phase. RA had no effect in the lag and exponential phase but decreased cell counts during the stationary phase. In contrast, RE1 and RE12 decreased cell number in all three phase, will RE12 reducing counts most rapidly. Addition of RE18 did not affect regardless of the growth phase. Appearance and physiological state of S. carnosus LTH1502 cells indicated difference in the way the compounds interacted with and damaged cells. Results were attributed to the different physicochemical properties of RA and its esters.

  5. In vitro angiotensin I converting enzyme inhibition by a peptide isolated from Chiropsalmus quadrigatus Haeckel (box jellyfish) venom hydrolysate.

    PubMed

    So, Pamela Berilyn T; Rubio, Peter; Lirio, Stephen; Macabeo, Allan Patrick; Huang, Hsi-Ya; Corpuz, Mary Jho-Anne T; Villaflores, Oliver B

    2016-09-01

    The anti-angiotensin I converting enzyme activity of box jellyfish, Chiropsalmus quadrigatus Haeckel venom hydrolysate was studied. The venom extract was obtained by centrifugation and ultrasonication. Protein concentration of 12.99 μg/mL was determined using Bradford assay. The pepsin and papain hydrolysate was tested for its toxicity by Limit test following the OECD Guideline 425 using 5 female Sprague-Dawley rats. Results showed that the hydrolysate is nontoxic with an LD50 above 2000 mg/kg. In vitro angiotensin I converting enzyme (ACE) inhibitory activity was determined using ACE kit-WST. Isolation of ACE inhibitory peptides using column chromatography with SP-Sephadex G-25 yielded 8 pooled fractions with fraction 3 (86.5%) exhibiting the highest activity. This was followed by reverse phase - high performance liquid chromatography (RP-HPLC) with an octadecyl silica column (Inertsil ODS-3) using methanol:water 15:85 at a flow rate of 1.0 mL/min. Among the 13 fractions separated with the RP-HPLC, fraction 3.5 exhibited the highest ACE inhibitory activity (84.1%). The peptide sequence ACPGPNPGRP (IC50 2.03 μM) from fraction 3.5 was identified using Matrix-assisted laser desorption/ionization with time-of-flight tandem mass spectroscopy analysis (MALDI-TOF/MS). PMID:27163886

  6. Mechanistic study for immobilization of cysteine-labeled oligopeptides on UV-activated surfaces.

    PubMed

    Ong, Lian Hao; Ding, Xiaokang; Yang, Kun-Lin

    2014-10-01

    In this study, we report immobilization of cysteine-labeled oligopeptides on UV activated surfaces decorated with N,N-dimethyl-n-octadecyl-3-aminopropyltrimethoxysilyl chloride (DMOAP). Our result shows that cysteine group, regardless of its position in the oligopeptide, is essential for successful immobilization of oligopeptide on the UV-activated surface. A possible reaction mechanism is nucleophilic addition of thiolates to surface aldehyde groups generated during UV activation. By using this technique, we are able to incorporate anchoring points into oligopeptides through cysteine residues. Furthermore, immobilized oligopeptides on the UV-activated surface is very stable even under harsh washing conditions. Finally, we show that an HPQ-containing oligopeptide can be immobilized on the UV-activated surface, but the final surface density and its ability to bind streptavidin are affected by the position of cysteine and HPQ. An oligopeptide with a cysteine at the N-terminus and a HPQ motif at the C-terminus gives the highest binding signal in the streptavidin-binding assay. This result is potentially useful for the development of functional oligopeptide microarrays for detecting target protein molecules.

  7. Development and validation of a liquid chromatography method for anthocyanins in strawberry (Fragaria spp.) and complementary studies on stability, kinetics and antioxidant power.

    PubMed

    Canuto, Gisele A B; Oliveira, Daniel R; da Conceição, Lucas S M; Farah, João P S; Tavares, Marina F M

    2016-02-01

    A RPLC-DAD method for the analysis of eight anthocyanins was developed, validated and applied to strawberry extracts. The chromatographic method was conducted under gradient elution in acidulated water-methanol mobile phase and octadecyl-silica columns. An ultrasound extraction procedure was optimized by a 3(2) factorial design (%HCl in methanol, temperature, and time) and response surface methodology. Method validation was performed according to the following parameters: linearity (R(2)>0.99, p-value<10(-4), F>725), LOD (3-7 μmol L(-1)) and LOQ (9-22 μmol L(-1)), selectivity/specificity (baseline separation of all analytes and peak purity), instrumental precision (<6.4%CV), repeatability (<6.3%CV) and intermediate precision (<9.9%CV), recovery (83-99%), robustness (mobile phase pH, column temperature and flow rate) and stability (high temperatures and storage; 1st order kinetics). The antioxidant power of anthocyanins was measured on-line (ABTS(+) reaction; Trolox as reference). Ten strawberry extracts were quantified (average values: 24.2 μg/g for cyanidin-3-glucoside and 49.1 μg/g for pelargonidin-3-glucoside).

  8. Alkyl-chain-grafted hexagonal boron nitride nanoplatelets as oil-dispersible additives for friction and wear reduction.

    PubMed

    Kumari, Sangita; Sharma, Om P; Gusain, Rashi; Mungse, Harshal P; Kukrety, Aruna; Kumar, Niranjan; Sugimura, Hiroyuki; Khatri, Om P

    2015-02-18

    Hexagonal boron nitride (h-BN), an isoelectric analogous to graphene multilayer, can easily shear at the contact interfaces and exhibits excellent mechanical strength, higher thermal stability, and resistance toward oxidation, which makes it a promising material for potential lubricant applications. However, the poor dispersibility of h-BN in lube base oil has been a major obstacle. Herein, h-BN powder was exfoliated into h-BN nanoplatelets (h-BNNPs), and then long alkyl chains were chemically grafted, targeting the basal plane defect and edge sites of h-BNNPs. The chemical and structural features of octadecyltriethoxysilane-functionalized h-BNNPs (h-BNNPs-ODTES) were studied by FTIR, XPS, XRD, HRTEM, and TGA analyses. The h-BNNPs-ODTES exhibit long-term dispersion stability in synthetic polyol ester lube base oil because of van der Waals interaction between the octadecyl chains of h-BNNPs-ODTES and alkyl functionalities of polyol ester. Micro- and macrotribology results showed that h-BNNPs-ODTES, as an additive to synthetic polyol ester, significantly reduced both the friction and wear of steel disks. Elemental mapping of the worn area explicitly demonstrates the transfer of h-BNNPs-ODTES on the contact interfaces. Furthermore, insight into the lubrication mechanism for reduction in both friction and wear is deduced based on the experimental results. PMID:25625695

  9. Fast analysis of flavonoids in plant extracts by liquid chromatography-ultraviolet absorbance detection on poly(carboxylic acid)-coated silica and electrospray ionization tandem mass spectrometric detection.

    PubMed

    Huck, C W; Buchmeiser, M R; Bonn, G K

    2002-01-11

    A highly hydrophilic poly(7-oxonorbornene-5,6-dicarboxylic acid-block-norbornene) [=poly-(ONDCA-b-NBE)]-coated silica was investigated for the liquid chromatographic (LC) determination of flavonoids in plant extracts of complex biological origin using UV absorbance and mass spectrometric (MS) detection. Compared to the most commonly used octadecyl derivatized silica this sorbent allowed fast separations even at extreme pH values. Furthermore, UV absorbance and MS detection were evaluated. As we found, UV detection at 254 nm allows the determination of flavonoids down to the ng range with a linearity of R2>0.9906. For the more selective characterization the validated LC system was coupled to a quadrupole ion trap mass spectrometer via an electrospray ionization (ESI) interface. MS detection showed high linearity (R2>0.9904) for all investigated flavonoids. Due to the relatively high flow-rate of 1 ml/min the limits of detection were found in the lower-microg range. Collision induced dissociation was applied to obtain characteristic fragmentation fingerprints. Finally, the validated LC-ESI-MS-MS method demonstrated that this poly-(ONDCA-b-NBE) stationary phase allows fast characterization and quantitation in onion, elderflower blossom, lime blossom, St. John's Wort and red wine.

  10. Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    USGS Publications Warehouse

    Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

    1992-01-01

    A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

  11. Semi-targeted analysis of metabolites using capillary-flow ion chromatography coupled to high-resolution mass spectrometry.

    PubMed

    Burgess, Karl; Creek, Darren; Dewsbury, Paul; Cook, Ken; Barrett, Michael P

    2011-11-30

    This work describes a novel application of capillary-flow ion chromatography mass spectrometry for metabolomic analysis, and comparison of the technique to octadecyl silica and hydrophilic interaction chromatography (HILIC)-based mass spectrometry. While liquid chromatography/mass spectrometry (LC/MS) is rapidly becoming the standard technique for metabolomic analysis, metabolomic samples are extremely heterogeneous, leading to a requirement for multiple methods of analysis and separation techniques to perform a 'global' metabolomic analysis. While C18 is suitable for hydrophobic metabolites and has been used extensively in pharmaceutical drug metabolism studies, HILIC is, in general, efficient at separating polar metabolites. Phosphorylated species and organic acids are challenging to analyse and effectively quantitate on both systems. There is therefore a requirement for an MS-compatible analytical technique that can separate negatively charged compounds, such as ion-exchange chromatography. Evaluation of capillary flow ion chromatography with electrolytic suppression was performed on a library of metabolite standards and was shown to effectively separate organic acids and sugar di- and tri-phosphates. Limits of detection for these compounds range from 0.01 to 100 pmol on-column. Application of capillary ion chromatography to a comparative analysis of energy metabolism in procyclic forms of the parasitic protozoan Trypanosoma brucei where cells were grown on glucose or proline as a carbon source was demonstrated to be more effective than HILIC for detection of the organic acids that comprise glucose central metabolism and the tricarboxylic acid (TCA) cycle.

  12. New analytical method for the determination of musks in personal care products by Quick, Easy, Cheap, Effective, Rugged, and Safe extraction followed by GC-MS.

    PubMed

    Homem, Vera; Silva, José Avelino; Cunha, Carina; Alves, Arminda; Santos, Lúcia

    2013-07-01

    Synthetic musks are organic compounds used as fragrance additives and fixative compounds in a diversity of personal care products. A new method based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction followed by GC-MS for the analysis of 12 musks in personal care products was developed and validated. Some experimental parameters, such as total QuEChERS mass, sample mass/solvent volume ratio, type of extraction solvent, as well as salts and sorbents amount were investigated and optimized. The final method involves the musks extraction using acetonitrile, followed by the addition of anhydrous magnesium sulphate and sodium acetate. The clean-up step was performed using dispersive SPE with primary and secondary amine and octadecyl-silica sorbents. This extraction procedure is fast (about 10 min) when compared to other traditional approaches. The method was robust for the matrices studied and shows a high precision (%RSD < 15%) and accuracy (average recovery of 85%), allowing the detection of musks in minimum concentrations between 0.01 ng/g (galaxolide) and 15.80 ng/g (musk xylene). The developed method was applied to the analysis of 12 samples, which revealed musks concentrations ranging from 2 ng/g (toothpaste) to 882,340 ng/g (perfumed body lotion).

  13. A solid-phase extraction procedure for the clean-up of thiram from aqueous solutions containing high concentrations of humic substances.

    PubMed

    Filipe, O M S; Vidal, M M; Duarte, A C; Santos, E B H

    2007-05-15

    A simple solid-phase extraction (SPE) procedure with an octadecyl bonded phase silica (C(18)) was developed for clean-up of the fungicide thiram from aqueous solutions containing high concentrations of humic substances, for future studies of thiram adsorption onto solid humic substances or soils. Suspensions of humic acids and soil, in aqueous 0.01M CaCl(2) solution, were prepared and used as samples. These extracts were spiked with thiram and immediately applied to a C(18)-SPE cartridge. Thiram was eluted with chloroform and its concentration measured by spectrophotometry at 283nm. Non-spiked aqueous extracts (blanks) and a control sample of thiram in 0.01M CaCl(2) aqueous solution were also prepared and submitted to the same SPE procedure. The results show that humic substances are extensively retained by the C(18) cartridge but are not eluted with CHCl(3). Recoveries of 100-104% were obtained for thiram in the presence of humic substances. The SPE procedure described in this work is an efficient clean-up step to remove the interference of humic substances absorbance and to be coupled to any spectrophotometric or HPLC-UV method, usually used for thiram analysis in food extracts.

  14. Porosity in polysilsesquioxane xerogels

    SciTech Connect

    LOY,DOUGLAS A.; SCHNEIDER,DUANE A.; BAUGHER,BRIGITTA M.; RAHIMIAN,KAMYAR

    2000-05-09

    Polysilsesquioxanes, [RSiO{sub 1.5}]{sub n} are a class of hybrid organic-inorganic materials in which silicon atoms are linked with up to three siloxane bonds to other monomer units in the polymer and the organic group is a pendent functionality. Polysilsesquioxanes are prepared by the hydrolysis and condensation of organotrialkoxysilanes (Scheme l). Organotrialkoxysilanes RSi(OR{prime}){sub 3}, have been extensively used as coupling agents for composites or surface treatments for materials. Polysilsesquioxanes have become increasingly popular for generating specialty coatings such as low k dielectric materials for microelectronic applications. While there is extensive information on the formation of polysilsesquioxanes, there has not been a survey of the ability of organotrialkoxysilanes to form gels until recently. The formation of polysilsesquioxanes gels has been shown to be very sensitive to the nature of the organic group. Many monomers will only form soluble oligomers or polymers upon hydrolysis and condensation, even when the reaction is conducted solvent-free with neat monomer and aqueous catalyst. Furthermore, there is little information concerning the influence of the organic group, R, on the porosity of the polysilsesquioxanes gels that are formed. In this paper the authors describe the preparation of polysilsesquioxane gels where R = H, methyl, ethyl, cyanoethyl, vinyl, dodecyl, hexadecyl, octadecyl, chloromethyl, and chloromethylphenyl, and the characterization of the porosity of the respective xerogels. Gels were prepared from the hydrolysis and condensation of organotrimethoxysilanes, RSi(OEt){sub 3}, and organotriethoxy-silanes, RSi(OEt){sub 3}.

  15. One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks.

    PubMed

    Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Marina, María Luisa; Sierra, Isabel

    2016-01-01

    A new procedure for the determination of 12 naturally occurring hormones and some related synthetic chemicals in milk, commonly used as growth promoters in cattle, is reported. The method is based on liquid-liquid extraction followed by solid-phase extraction (SPE) using a new one-pot synthesized ordered mesoporous silica (of the SBA-15 type) functionalized with octadecyl groups (denoted as SBA-15-C18-CO) as reversed-phase sorbent. The analytes were eluted with methanol and then submitted to HPLC with diode array detection. Under optimal conditions, the method quantification limit for the analytes ranged from 0.023 to 1.36μg/mL. The sorbent affored the extraction of estrone, 17β-estradiol, estriol, progesterone, hexestrol, diethylstilbestrol, 4-androstene-3,17-dione, ethinylestradiol, 17α-methyltestosterone, nandrolone, prednisolone and testosterone with mean recoveries ranging from 72% to 105% (except for diethylstilbestrol) with RSD<11%. These results were comparable and, in some cases, even better than those obtained with other extraction methods, therefore SBA-15-C18-CO mesoporous silica possess a high potential as a reversed-phase sorbent for SPE of the 12 mentioned endocrine disrupting compounds in milk samples.

  16. 1-Alkyl-1-methylpiperazine-1,4-diium salts: Synthetic, acid-base, XRD-analytical, FT-IR, FT-Raman spectral and quantum chemical study

    NASA Astrophysics Data System (ADS)

    Němečková, Dana; Mary, Y. Sheena; Panicker, C. Yohannan; Varghese, Hema Tresa; Van Alsenoy, Christian; Procházková, Markéta; Pazdera, Pavel; Al-Saadi, Abdulaziz A.

    2015-08-01

    We report the preparation and results of vibrational spectral analysis, which were obtained using both FT-IR and FT-Raman spectroscopy, for three 1-alkyl-1-methylpiperazine-1,4-diium salts (AMPSs), where alkyl is benzyl 4a, n-octadecyl 4b, and methyl 4c, respectively. These were prepared by multistep synthesis from piperazine. The acid-base study of AMPSs was performed and corresponding acid-base constants were obtained. Single crystals of AMPSs suitable for XRD-analysis were obtained and analyzed. The complete vibrational assignments of wavenumbers were made on the basis of a potential energy distribution. The HOMO and LUMO analysis was used to determine the charge transfer within the molecules. The calculated first hyperpolarizabilities of AMPSs 4a-4c are 48.34, 57.77 and 123.41 times that of urea. As can be seen from the MEP plots, the negative electrostatic potential regions are mainly localized over the chlorine and oxygen atoms for compounds 4a and 4b and chlorine and iodine atoms of compound 4c, and are possible sites for electrophilic attack.

  17. Reduction of water surface tension significantly impacts gecko adhesion underwater.

    PubMed

    Stark, Alyssa Y; McClung, Brandon; Niewiarowski, Peter H; Dhinojwala, Ali

    2014-12-01

    The gecko adhesive system is dependent on weak van der Waals interactions that are multiplied across thousands of fine hair-like structures (setae) on geckos' toe pads. Due to the requirements of van der Waals forces, we expect that any interruption between the setae and substrate, such as a water layer, will compromise adhesion. Our recent results suggest, however, that the air layer (plastron) surrounding the superhydrophobic toe pads aid in expelling water at the contact interface and create strong shear adhesion in water when in contact with hydrophobic surfaces. To test the function of the air plastron, we reduced the surface tension of water using two surfactants, a charged anionic surfactant and a neutral nonionic surfactant. We tested geckos on three substrates: hydrophilic glass and two hydrophobic surfaces, glass with a octadecyl trichlorosilane self-assembled monolayer (OTS-SAM) and polytetrafluoroethylene (PTFE). We found that the anionic surfactant inhibited the formation of the air plastron layer and significantly reduced shear adhesion to all three substrates. Interestingly, the air plastron was more stable in the nonionic surfactant treatments than the anionic surfactant treatments and we found that geckos adhered better in the nonionic surfactant than in the anionic surfactant on OTS-SAM and PTFE but not on glass. Our results have implications for the evolution of a superhydrophobic toe pad and highlight some of the challenges faced in designing synthetic adhesives that mimic geckos' toes.

  18. Stimulation and release from neurons via a dual capillary collection device interfaced to mass spectrometry.

    PubMed

    Fan, Yi; Lee, Chang Young; Rubakhin, Stanislav S; Sweedler, Jonathan V

    2013-11-01

    Neuropeptides are cell to cell signaling molecules that modulate a wide range of physiological processes. Neuropeptide release has been studied in sample sizes ranging from single cells and neuronal clusters, to defined brain nuclei and large brain regions. We have developed and optimized cell stimulation and collection approaches for the efficient measurement of neuropeptide release from neuronal samples using a dual capillary system. The defining feature is a capillary that contains octadecyl-modified silica nanoparticles on its inner wall to capture and extract releasates. This collection capillary is inserted into another capillary used to deliver solutions that chemically stimulate the cells, with solution flowing up the inner capillary to facilitate peptide collection. The efficiency of peptide collection was evaluated using six peptide standards mixed in physiological saline. The extracted peptides eluted from these capillaries were characterized via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) with low femtomole detection limits. Using the capillary collection system in small custom-fabricated culturing chambers, individual cultured neurons and neuronal clusters from the model animal Aplysia californica were stimulated with distinct neuronal secretagogues and the releasates were collected and characterized using MALDI-TOF MS.

  19. Speciation analysis of tellurium by solid-phase extraction in the presence of ammonium pyrrolidine dithiocarbamate and inductively coupled plasma mass spectrometry.

    PubMed

    Yu, Chunhai; Cai, Qiantao; Guo, Zhong-Xian; Yang, Zhaoguang; Khoo, Soo Beng

    2003-05-01

    Under acidic conditions tellurium(IV) formed a complex with ammonium pyrrolidine dithiocarbamate (APDC). The tellurium(IV) complex was completely retained on a non-polar Isolute silica-based octadecyl (C(18)) sorbent-containing solid-phase extraction (SPE) cartridge, while the uncomplexed Te(VI) passed through the cartridge and remained as a free species in the solution. Only partial Te(IV) was retained on the SPE cartridge for samples without addition of APDC. On the basis of different retention behaviours of the complexed Te(IV) and uncomplexed Te(VI), a simple and highly sensitive method is proposed for the determination of total tellurium and Te(VI) by SPE separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The Te(IV) concentration was calculated as the difference between total tellurium and Te(VI) concentrations. The detection limit (3 sigma) is 3 ng L(-1) tellurium. Factors affecting the separation and detection of tellurium species were investigated. Coexisting ions did not show significant interferences with the Te(IV)-APDC complex retention and the subsequent ICP-MS detection of Te. The method has been successfully applied to the tellurium speciation analysis in waters with spiked recoveries for Te(IV) and Te(VI) of 86.0-108% and 87.1-97.4%, respectively.

  20. SPE coupled with dispersive liquid-liquid microextraction followed by GC with flame ionization detection for the determination of ultra-trace amounts of benzodiazepines.

    PubMed

    Ghobadi, Masoomeh; Yamini, Yadollah; Ebrahimpour, Behnam

    2014-02-01

    SPE combined with dispersive liquid-liquid microextration was used for the extraction of ultra-trace amounts of benzodiazepines (BZPs) including, diazepam, midazolam, and alprazolam, from ultra-pure water, tap water, fruit juices, and urine samples. The analytes were adsorbed from large volume samples (60 mL) onto octadecyl silica SPE columns. After the elution of the desired compounds from sorbents with 2.0 mL acetone, 0.5 mL of eluent containing 40.0 μL chloroform was injected rapidly into 4.5 mL pure water. After extraction and centrifugation, 2 μL of the sedimented phase was injected into a GC equipped with a flame ionization detector. Several parameters affecting this process were investigated and optimized. Under the optimal conditions, LODs ranged from 0.02 to 0.05 μg/L, a linear dynamic range of 0.1-100 μg/L and relative SDs in the range of 4.4-10.7% were attained. Very high preconcentration factors ranging from 3895-7222 were achieved. The applicability of the method for the extraction of BZPs from different types of complicated matrices, such as tap water, fruit juices, and urine samples, was studied. The obtained results reveal that the proposed method is a good technique for the extraction and determination of BZPs in complex matrices.

  1. Alkyl ether lipids, ion channels and lipid raft reorganization in cancer therapy.

    PubMed

    Jaffrès, Paul-Alain; Gajate, Consuelo; Bouchet, Ana Maria; Couthon-Gourvès, Hélène; Chantôme, Aurélie; Potier-Cartereau, Marie; Besson, Pierre; Bougnoux, Philippe; Mollinedo, Faustino; Vandier, Christophe

    2016-09-01

    Synthetic alkyl lipids, such as the ether lipids edelfosine (1-O-octadecyl-2-O-methyl-rac-glycero-3-phosphocholine) and ohmline (1-O-hexadecyl-2-O-methyl-rac-glycero-3-β-lactose), are forming a class of antitumor agents that target cell membranes to induce apoptosis and to decrease cell migration/invasion, leading to the inhibition of tumor and metastasis development. In this review, we present the structure-activity relationship of edelfosine and ohmline, and we point out differences and similarities between these two amphiphilic compounds. We also discuss the mechanisms of action of these synthetic alkyl ether lipids (involving, among other structures and molecules, membrane domains, Fas/CD95 death receptor signaling, and ion channels), and highlight a key role for lipid rafts in the underlying process. The reorganization of lipid raft membrane domains induced by these alkyl lipids affects the function of death receptors and ion channels, thus leading to apoptosis and/or inhibition of cancer cell migration. The possible therapeutic use of these alkyl lipids and the clinical perspectives for these lipids in prevention or/and treatment of tumor development and metastasis are also discussed.

  2. Modeling of alkyl quaternary ammonium cations intercalated into montmorillonite lattice

    SciTech Connect

    Daoudi, El Mehdi; Boughaleb, Yahia; El Gaini, Layla; Meghea, Irina; Bakasse, Mina

    2013-05-15

    Highlights: ► The modification of montmorillonites by three surfactants increases the basal spacing. ► The model proposed show a bilayer conformation for the surfactant ODTMA. ► The DODMA and TOMA surfactants adopt a paraffin type arrangement. ► Behavior of surfactants in interlayer space was confirmed by TGA and ATR analysis. - Abstract: The objective of this work was to study the conformation of the quaternary ammonium cations viz., octadecyl trimethyl ammonium (ODTMA), dioctadecyl dimethyl ammonium (DMDOA) and trioctadecyl methyl ammonium (TOMA) intercalated within montmorillonite. The modified montmorillonite was characterized by X-ray diffraction in small angle (SAXS), thermal analysis (TGA) and infrared spectroscopy of attenuated total reflection (ATR). The modification of organophilic montmorillonites by the three surfactants ODTMA, DMDOA and TOMA increases the basal spacing from their respective intercalated distances of 1.9 nm, 2.6 nm and 3.4 nm respectively. The increase in the spacing due to the basic organic modification was confirmed by the results of thermal analysis (TGA) and infrared spectroscopy (ATR), and also supported by theoretical calculations of longitudinal and transversal chain sizes of these alkyl quaternary ammonium cations.

  3. Carbonaceous nanomaterials immobilised mixed matrix membrane microextraction for the determination of polycyclic aromatic hydrocarbons in sewage pond water samples.

    PubMed

    Mukhtar, Nurul Hazirah; See, Hong Heng

    2016-08-10

    In this study, the potential for carbonaceous nanomaterials to be used as adsorbents for the mixed matrix membrane (MMM) microextraction and preconcentration of organic pollutants was demonstrated. For this method, multiwall carbon nanotubes (MWCNT) and single layer graphene (SLG) nanoparticles were individually incorporated through dispersion in a cellulose triacetate (CTA) polymer matrix to form a MWCNT-MMM and SLG-MMM, respectively. The prepared membranes were evaluated for the extraction of selected polycyclic aromatic hydrocarbons (PAHs) present in sewage pond water samples. The extraction was performed by dipping a small piece of membrane (7 mm × 7 mm) in a stirred 7.5 mL sample solution to initiate the analyte adsorption. This step was followed by an analyte desorption into 60 μL of methanol prior to high performance liquid chromatography (HPLC) analysis. When the optimum SLG-MMM microextraction technique was applied to spiked sewage pond water samples, the detection limit of the method for the PAHs were in the range of 0.02-0.09 ng/mL, with relative standard deviations of between 1.4% and 7.8%. Enrichment factors of 54-100 were achieved with relative recoveries of 99%-101%. A comparison was also made between the proposed approach and standard solid phase extraction using polymeric bonded octadecyl (C18) cartridges. PMID:27282751

  4. Analytical issues in HPLC/MS/MS simultaneous assay of furosemide, spironolactone and canrenone in human plasma samples.

    PubMed

    Sora, Daniela Iuliana; Udrescu, Stefan; Albu, Florin; David, Victor; Medvedovici, Andrei

    2010-09-01

    A new sensitive HPLC/MS/MS method for simultaneous determination of furosemide, spironolactone and canrenone in human plasma samples is presented. Electrospray ionization source (ESI) has been used. The tandem MS detection was performed under MRM conditions, in the negative ion mode for furosemide and indapamide (internal standard 1) and in the positive ion mode for spironolactone, canrenone and nitrazepam (internal standard 2). A simple plasma protein precipitation with acetonitrile was used as sample preparation technique. The chromatographic separation was carried out under the reversed phase mechanism, on a 250 mm length column packed with octadecyl modified silicagel and thermostated at 35 degrees C. The column was operated under isocratic conditions (3:7 aqueous 0.1% formic acid and methanol, v/v) at a flow rate of 0.8 mL/min. Quantitation intervals of 20-1600 ng/mL for furosemide and 2-100 ng/mL for spironolactone and canrenone have been concluded through validation. Precision and accuracy were situated within the accepted thresholds (maximum 15% relative standard deviation and +/-15% percentage bias). The most sensitive aspects relating to the analytical method development and validation were highlighted and critically assessed in order to reach an objective opinion about the real performances and inherent applicability of the method in bioanalysis. PMID:20307949

  5. Time- and temperature-dependent migration studies of Irganox 1076 from plastics into foods and food simulants.

    PubMed

    Beldì, G; Pastorelli, S; Franchini, F; Simoneau, C

    2012-01-01

    The study provides an exhaustive set of migration data for octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate (Irganox 1076) from low-density polyethylene (LDPE) in several food matrices. Irganox 1076 was used as a model migrant because it represents one of the typical substances used as an antioxidant in food packaging polymers. Kinetic (time-dependent) migration studies of Irganox 1076 were performed for selected foodstuffs chosen with different physical-chemical properties and in relation to the actual European food consumption market. The effect of fat content and of the temperature of storage on the migration from plastic packaging was evaluated. The results show that migration increased with fat content and storage temperature. All data obtained from real foods were also compared with data obtained from simulants tested in the same conditions. In all studied cases, the kinetics in simulants were higher than those in foodstuffs. The work provides data valuable for the extension of the validation of migration model developed on simulants to foodstuffs themselves.

  6. Hydrophobic high surface area zeolites derived from fly ash for oil spill remediation.

    PubMed

    Sakthivel, Tamilselvan; Reid, David L; Goldstein, Ian; Hench, Larry; Seal, Sudipta

    2013-06-01

    Fly ash, a coal combustion byproduct with a predominantly aluminosilicate composition, is modified to develop an inexpensive sorbent for oil spill remediation. The as-produced fly ash is a hydrophilic material with poor sorption capacity. A simple two-step chemical modification process is designed to improve the oil sorption capacity. First, the fly ash was transformed to a zeolitic material via an alkali treatment, which increased the specific surface area up to 404 m(2) g(-1). Then, the material was surface functionalized to form a hydrophobic material with high contact angle up to 147° that floats on the surface of an oil-water mixture. The reported oil sorption capacities of X-type zeolite sorbent with different surface functionalization (propyl-, octyl-, octadecyl-trimethoxysilane and esterification) were estimated to 1.10, 1.02, 0.86, and 1.15 g g(-1), respectively. Oil sorption was about five times higher than the as-received fly ash (0.19 g g(-1)) and also had high buoyancy critical for economic cleanup of oil over water.

  7. [Analysis of trichothecenes in barley tea and beer by liquid chromatography/tandem mass spectrometry].

    PubMed

    Suga, Keiko; Mochizuki, Naoki; Harayama, Koichi; Yamashita, Hiroshi

    2004-12-01

    A simple method for analysis of trichothecenes [Type A: diacetoxyscirpenol, neosolaniol, HT-2 toxin, and T-2 toxin, Type B: deoxynivalenol, nivalenol, fusarenon-X, 3-acetyldeoxynivalenol, 15-acetyldeoxynivarenol] in barley tea and beer using liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed. Trichothecenes were extracted with ethyl acetate-methanol (19:1). The solvent was evaporated to dryness and the residue was dissolved in water-methanol (3:1) for injection into the LC/MS/MS. The LC separation was performed with an octadecylated silica column at a flow-rate of 0.2 mL/min, using a mobile phase consisting of water, methanol and acetonitrile. MS/MS was used in multiple reaction monitoring, employing electrospray ionization (ESI-MRM). The recoveries of trichothecenes from drinks at 1 microg/L (Type A) and 10 microg/L (Type B) were 52.5-115.2% (barley tea) and 68.1-127.5% (beer). Five barley tea and ten beer samples were analyzed by this method. Trichothecenes were not detected in them. This method may have applications in quality assurance.

  8. [Analysis of fumonisin B1 and B2 in beer and raw materials of beer by liquid chromatography/tandem mass spectrometry].

    PubMed

    Suga, Keiko; Mochizuki, Naoki; Yamashita, Hiroshi

    2004-10-01

    A simple method for analysis of fumonisin B1 (FB1) and fumonisin B2 (FB2) in beer and raw materials of beer using liquid chromatography-electrospray ionization tandem mass spectrometry (LC/MS/MS) was developed. Samples were prepared and purified by using solid-phase extraction columns (SAX). The LC separation was performed with an octadecylated silica column at a flow-rate of 0.2 mL/min, using a mobile phase consisting of water and acetonitrile. MS/MS was used in multiple reaction monitoring, employing electrospray ionization (ESI-MRM). Recoveries of spiked FB1 and FB2 from beer were 64% and 52%, respectively, at the level of 5 microg/kg. Recoveries of spiked FB1 and FB2 from malt, cornstarch, and corn grit, at the level of 50 microg/kg, were 87.9% and 86.4%, 89.5% and 87.9%, 86.6% and 81.1%, respectively. This method may have applications in quality assurance.

  9. Nanocomposites prepared from acrylonitrile butadiene rubber and organically modified montmorillonite with vinyl groups

    NASA Astrophysics Data System (ADS)

    Han, Mijeong; Kim, Hoonjung; Kim, Eunkyoung

    2006-01-01

    Nanocomposites were prepared from acrylonitrile-butadiene rubber (NBR), vinyl groups containing organically modified montmorillonite and additives, such as zinc oxide, stearic acid, and sulfur. The organically modified montmorillonites used in these nanocomposites were prepared by ion exchange reactions of N,N'-dimethylalkyl-(p-vinylbenzyl)-ammonium chlorides (DAVBAs, alkyl = octyl, dodecyl, and octadecyl) with sodium montmorillonite (Na+-MMT). NBR nanocomposites were obtained by controlling both the mixing and vulcanization conditions, by using a Brabender mixer and hot-press process. X-ray diffraction (XRD) analysis shows that, depending on the amount of montmorillonite that is added, both exfoliated and intercalated nanocomposite structures are formed. The NBR/DAVBA-MMT nanocomposites exhibit much higher mechanical properties (e.g., tensile strength, Young's modulus, 300% modulus, and hardness) as well as gas barrier properties as compared to NBR Na+-MMT or NBR composites generated from modified montmorillonites without vinyl groups. Consistent with the results of XRD, transmission electron microscopy (TEM) reveals that the intercalation and exfoliation structures of the nanocomposites coexist and that the DAVBA-MMT layers are well dispersed in NBR.

  10. Alkyl-chain-grafted hexagonal boron nitride nanoplatelets as oil-dispersible additives for friction and wear reduction.

    PubMed

    Kumari, Sangita; Sharma, Om P; Gusain, Rashi; Mungse, Harshal P; Kukrety, Aruna; Kumar, Niranjan; Sugimura, Hiroyuki; Khatri, Om P

    2015-02-18

    Hexagonal boron nitride (h-BN), an isoelectric analogous to graphene multilayer, can easily shear at the contact interfaces and exhibits excellent mechanical strength, higher thermal stability, and resistance toward oxidation, which makes it a promising material for potential lubricant applications. However, the poor dispersibility of h-BN in lube base oil has been a major obstacle. Herein, h-BN powder was exfoliated into h-BN nanoplatelets (h-BNNPs), and then long alkyl chains were chemically grafted, targeting the basal plane defect and edge sites of h-BNNPs. The chemical and structural features of octadecyltriethoxysilane-functionalized h-BNNPs (h-BNNPs-ODTES) were studied by FTIR, XPS, XRD, HRTEM, and TGA analyses. The h-BNNPs-ODTES exhibit long-term dispersion stability in synthetic polyol ester lube base oil because of van der Waals interaction between the octadecyl chains of h-BNNPs-ODTES and alkyl functionalities of polyol ester. Micro- and macrotribology results showed that h-BNNPs-ODTES, as an additive to synthetic polyol ester, significantly reduced both the friction and wear of steel disks. Elemental mapping of the worn area explicitly demonstrates the transfer of h-BNNPs-ODTES on the contact interfaces. Furthermore, insight into the lubrication mechanism for reduction in both friction and wear is deduced based on the experimental results.

  11. Hydrophobic aggregation of fine particles in high muddied coal slurry water.

    PubMed

    Chen, Jun; Min, Fanfei; Liu, Lingyun; Peng, Chenliang; Lu, Fangqin

    2016-01-01

    The hydrophobic aggregation of fine particles in high muddied coal slurry water in the presence of four quaternary ammonium salts of 1231(dodecyl trimethyl ammonium chloride), 1431(tetradecyl trimethyl ammonium chloride), 1631(cetyl trimethyl ammonium chloride) and 1831(octadecyl trimethyl ammonium chloride) was investigated through the measurement of contact angles, zeta potentials, aggregation observation, adsorption and sedimentation. The results show that quaternary ammonium salts can enhance the hydrophobicity and reduce the electronegativity of particle surface, and thus induce a strong hydrophobic aggregation of slurry fine particles which promotes the settlement of coal slurry water. The adsorption of quaternary ammonium salts on slurry particles increases with the increase of alkyl chain length and reagent dosage, and will reach equilibrium when the dosage reaches a certain value. Weak alkaline conditions also can promote quaternary ammonium salts to be adsorbed on the coal slurry fine particles. In addition, reasonable energy input and a chemical environment of weak alkaline solution are conducive to hydrophobic aggregation settlement of high muddied coal slurry water with quaternary ammonium salts. The main mechanism of hydrophobic aggregation of coal slurry particles with quaternary ammonium salts is 'adsorption charge neutralization' and hydrophobic interaction.

  12. Ellipsoidal Polyaspartamide Polymersomes with Enhanced Cell-Targeting Ability.

    PubMed

    Lai, Mei-Hsiu; Jeong, Jae Hyun; Devolder, Ross J; Brockman, Christopher; Schroeder, Charles; Kong, Hyunjoon

    2012-08-01

    Nano-sized polymersomes functionalized with peptides or proteins are being increasingly studied for targeted delivery of diagnostic and therapeutic molecules. Earlier computational studies have suggested that ellipsoidal nanoparticles, compared to spherical ones, display enhanced binding efficiency with target cells, but this has not yet been experimentally validated. We hypothesize that hydrophilic polymer chains coupled to vesicle-forming polymers would result in ellipsoidal polymersomes. In addition, ellipsoidal polymersomes modified with cell adhesion peptides bind with target cells more actively than spherical ones. We examine this hypothesis by substituting polyaspartamide with octadecyl chains and varying numbers of poly(ethylene glycol) (PEG) chains. Increasing the degree of substitution of PEG from 0.5 to 1.0 mol% drives the polymer to self-assemble into an ellipsoidal polymersome with an aspect ratio of 2.1. Further modification of these ellipsoidal polymersomes with peptides containing an Arg-Gly-Asp sequence (RGD peptides) lead to a significant increase in the rate of association and decrease in the rate of dissociation with a substrate coated with αvβ3 integrins. In addition, in a circulation-mimicking flow, the ellipsoidal polymersomes linked with RGD peptides adhere to target tissues more favorably than their spherical equivalents do. Overall, the results of this study will greatly serve to improve the efficiency of targeted delivery of a wide array of polymersomes loaded with various biomedical modalities.

  13. Solid phase extraction using magnetic core mesoporous shell microspheres with C18-modified interior pore-walls for residue analysis of cephalosporins in milk by LC-MS/MS.

    PubMed

    Liu, Xiaodan; Yu, Yingjia; Zhao, Meiyan; Zhang, Haiying; Li, Yan; Duan, Gengli

    2014-05-01

    A fast and effective extraction method has been developed for measuring the residue of cephalosporins (cefalexin, cefazolin, cefoperazone) in milk by using magnetic core-mesoporous shell microspheres with C18-functionalized interior pore-walls (C18-Fe3O4@mSiO2) as adsorbent. With no need for any protein precipitation procedure, the cephalosporins were directly adsorbed onto the C18-Fe3O4@mSiO2 microspheres through hydrophobic interaction with C18-groups (Octadecyl functional groups) functionalized in the interior walls of mesopore channels while the abundant proteins in milk sample were excluded out of the channel due to the size exclusion effect. Thereafter, the cephalosporins-absorbed C18-Fe3O4@mSiO2 microspheres were rapidly isolated by placing a magnet, and followed by liquid chromatography-tandem mass spectrometry analysis after eluted by methanol. Various parameters which could affect the extraction performance were optimised. The newly developed extraction method was successfully applied in determination of cephalosporin residues in milk samples, offering a valuable alternative to simplify and speed up the sample preparation step.

  14. Effect of surface-modified polyimide gate insulator through hybridization on the performance of organic thin-film transistors

    NASA Astrophysics Data System (ADS)

    Pyo, Seungmoon; Choi, Joongkeun; Oh, Youngnam; Son, Hyunsam; Yi, Mi Hye

    2006-04-01

    Surface modification of the gate insulator is a key to performance improvement of organic thin-film transistors (OTFTs). To date, the surface modification of a gate insulator is based on a primer or buffer layer deposition on top of a gate insulator. We report an approach to modify the surface of a gate insulator without a primer and/or buffer layer deposition. In order to obtain polymer gate insulators with well-controlled surface properties, a hybridization method was used and some gate insulators were prepared by varying the hybridization ratio of polyimide with a nonpolar octadecyl side chain to poly(amic acid). The surface property of the hybrid gate insulator varies according to the hybridization ratio. We believe that the long alkyl side chain of the hybrids protrudes from the surface, and makes the surface more hydrophobic. The modified hydrophobic surface strongly affects an initial growth mechanism of pentacene and subsequently the performance of OTFTs. The performance of pentacene OTFTs with the hybrids is superior to that of the OTFTs with only poly(amic acid) and exhibited a carrier mobility of 0.94cm2/Vs, an on/off current ratio of around 106, and a subthreshold slope of 3.1V/dec.

  15. Effect of surface property of polyimide substrate on the formation of pentacene thin-film

    NASA Astrophysics Data System (ADS)

    Yu, Chung-Jong; Choi, Youngill; Pyo, Seungmoon; Yi, Mihye; Kim, Jong Soo; Cho, Kilwon; Lee, Dong Ryeol

    2009-04-01

    We investigated the effect of surface property of polyimide substrate on the formation of pentacene thin-film by using atomic force microscopy (AFM) and X-ray reflectivity (XRR) and diffuse scattering (XDS). Two types of polymer films were prepared: (1) polyimide (PAA-PI) from poly(amic acid) (PAA) (2) polyimide hybrid (PAA-PI-H) prepared by hybridizing the PAA and soluble polyimide (PI) with a octadecyl side chain. The hybridization ratio of PI to PAA was 2/98 in wt%. The water contact angle for PAA-PI-H and PAA-PI were around 80° and 64°, respectively. Morphology of pentacene with a ropelike structure and (1 1 0) peak around 1.4 Å in qz was found when it was deposited on PAA-PI thin-film. Different pentacene morphology was observed when it was deposited on PAA-PI-H thin-film. The different morphology might be due to a 5-6 nm thick additional layer (˜0.95 ρfilm) at the interface between pentacene and PAA-PI-H thin-film caused by a long alkyl side chain introduced to the polymer main chain.

  16. Detergent Induction of HEK 293A Cell Membrane Permeability Measured under Quiescent and Superfusion Conditions Using Whole Cell Patch Clamp

    PubMed Central

    2015-01-01

    Detergents have several biological applications but present cytotoxicity concerns, since they can solubilize cell membranes. Using the IonFlux 16, an ensemble whole cell planar patch clamp, we observed that anionic sodium dodecyl sulfate (SDS), cationic cetyltrimethylammonium bromide (CTAB), and cationic, fluorescent octadecyl rhodamine B (ORB) increased the membrane permeability of cells substantially within a second of exposure, under superfusion conditions. Increased permeability was irreversible for 15 min. At subsolubilizing detergent concentrations, patched cells showed increased membrane currents that reached a steady state and were intact when imaged using fluorescence microscopy. SDS solubilized cells at concentrations of 2 mM (2× CMC), while CTAB did not solubilize cells even at concentrations of 10 mM (1000× CMC). The relative activity for plasma membrane current induction was 1:20:14 for SDS, CTAB, and ORB, respectively. Under quiescent conditions, the relative ratio of lipid to detergent in cell membranes at the onset of membrane permeability was 1:7:5 for SDS, CTAB, and ORB, respectively. The partition constants (K) for SDS, CTAB, and ORB were 23000, 55000, and 39000 M–1, respectively. Combining the whole cell patch clamp data and XTT viability data, SDS ≤ 0.2 mM and CTAB and ORB ≤ 1 mM induced cell membrane permeability without causing acute toxicity. PMID:24548291

  17. Phelligridins C-F: cytotoxic pyrano[4,3-c][2]benzopyran-1,6-dione and furo[3,2-c]pyran-4-one derivatives from the fungus Phellinus igniarius.

    PubMed

    Mo, Shunyan; Wang, Sujuan; Zhou, Guangxiong; Yang, Yongchun; Li, Yan; Chen, Xiaoguang; Shi, Jiangong

    2004-05-01

    Three unique pyrano[4,3-c][2]benzopyran-1,6-dione derivatives and a new furo[3,2-c]pyran-4-one, named phelligridins C-F (2-5), together with hispolon (8), (E)-4-(3,4-dihydroxyphenyl)but-3-en-2-one (9), 4-hydroxybenzaldehyde, protocatechualdehyde, syringic acid, protocatechuic acid, caffeic acid, isoergosterone, and octadecyl ferulate were isolated and identified from the ethanolic extract of Phellinus igniarius. Their structures were determined by spectroscopic methods including IR, MS, and 1D and 2D NMR experiments. The structures of the new compounds were characterized as 3-(4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (2), 3-(3,4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (3), 8,9-dihydroxy-3-[5',6'-dihydroxy-5' '-methyl-3' '-oxo-spiro[fural-2' '(3' 'H),1'-indene]-2'-yl]-1H,6H-pyrano[4,3-c][2]benzopyran-1,6-dione (4), and (3Z)-3-(3,4-dihydroxybenzylidene)-6-(3,4-dihydroxystyryl)-2,3-dihydro-2-methoxy-2-(2-oxo-propyl)furo[3,2-c]pyran-4-one (5), respectively. Some compounds including 2 and 3 showed in vitro selective cytotoxicity against a human lung cancer cell line (A549) and a liver cancer cell line (Bel7402). Possible biogenetic sequences to the formation of 1-9 are postulated. PMID:15165144

  18. Preparation, characterization, and antitumor activity of paclitaxel-loaded folic acid modified and TAT peptide conjugated PEGylated polymeric liposomes.

    PubMed

    Niu, Ruifang; Zhao, Peiqi; Wang, Hanjie; Yu, Man; Cao, Shuzhen; Zhang, Fei; Chang, Jin

    2011-06-01

    Targeting therapy is a promising strategy for enhancing the therapeutic potential of chemotherapeutic agents. In this study, we report the construction of a multifunctional drug delivery system, termed folic acid modified and TAT peptide conjugated PEGylated polymeric liposomes (FA-TATp-PLs), which is originally derived from octadecyl-quaternized lysine modified chitosan and cholesterol. Our data revealed that FA-TATp-PLs have a particle size of about 60 nm with a zeta potential of about 30 mV, a low burst release effect within the first day, a sustained release for the next 14 days in vitro as well as an instant cellular uptake by folate receptor-overexpressing KB human nasopharyngeal carcinoma cells. In vitro cytotoxicity of paclitaxel-loaded FA-TATp-PLs in KB cells was superior to that of Taxol(®). Furthermore, a comparable antitumor efficacy of paclitaxel-loaded FA-TATp-PLs and Taxol(®) was observed at the same doses in murine models bearing nasopharyngeal carcinoma. These results demonstrate that the paclitaxel formulation not only exhibits a higher antitumor activity but also significantly reduces the toxicity and improves the bioavailability as compared to that of free paclitaxel for the treatment of nasopharyngeal carcinoma. Taken together, our findings indicate that paclitaxel-loaded FA-TATp-PLs are a promising nano-sized drug formulation for future cancer therapy. PMID:20677917

  19. Multifunctional electroactive electrospun nanofiber structures from water solution blends of PVA/ODA–MMT and poly(maleic acid-alt-acrylic acid): effects of Ag, organoclay, structural rearrangement and NaOH doping factors

    NASA Astrophysics Data System (ADS)

    Şimşek, Murat; Rzayev, Zakir M. O.; Bunyatova, Ulviya

    2016-06-01

    Novel multifunctional colloidal polymer nanofiber electrolytes were fabricated by green reactive electrospinning nanotechnology from various water solution/dispersed blends of poly (vinyl alcohol-co-vinyl acetate) (PVA)/octadecyl amine-montmorillonite (ODA–MMT) as matrix polymer nanocomposite and poly(maleic acid-alt-acrylic acid) (poly(MAc-alt-AA) and/or its Ag-carrying complex as partner copolymers. Polymer nanofiber electrolytes were characterized using FTIR, XRD, thermal (DSC, TGA–DTG), SEM, and electrical analysis methods. Effects of partner copolymers, organoclay, in situ generated silver nanoparticles (AgNPs), and annealing procedure on physical and chemical properties of polymer composite nanofibers were investigated. The electrical properties (resistance, conductivity, activation energy) of nanofibers with/without NaOH doping agent were also evaluated. This work presented a structural rearrangement of nanofiber mats by annealing via decarboxylation of anhydride units with the formation of new conjugated double bond sites onto partner copolymer main chains. It was also found that the semiconductor behaviors of nanofiber structures were essentially improved with increasing temperature and fraction of partner copolymers as well as presence of organoclay and AgNPs in nanofiber composite.

  20. Isolation and Bioactivity Analysis of Ethyl Acetate Extract from Acer tegmentosum Using In Vitro Assay and On-Line Screening HPLC-ABTS+ System

    PubMed Central

    Song, Na-Young; Oh, You Chang; Cho, Won-Kyung; Ma, Jin Yeul

    2014-01-01

    The Acer tegmentosum (3 kg) was extracted using hot water, and the freeze-dried extract powder was partitioned successively using dichloromethane (DCM), ethyl acetate (EA), butyl alcohol (n-BuOH), and water. From the EA extract fraction (1.24 g), five phenolic compounds were isolated by the silica gel, octadecyl silica gel, and Sephadex LH-20 column chromatography. Based on spectroscopic methods such as 1H-NMR, 13C-NMR, and LC/MS the chemical structures of the compounds were confirmed as feniculin (1), avicularin (2), (+)-catechin (3), (−)-epicatechin (4), and 6′-O-galloyl salidroside (5). Moreover, a rapid on-line screening HPLC-ABTS+ system for individual bioactivity of the EA-soluble fraction (five phenolic compounds) was developed. The results indicated that compounds 1 and 2 were first isolated from the A. tegmentosum. The anti-inflammatory activities and on-line screening HPLC-ABTS+ assay method of these compounds in LPS-stimulated murine macrophages were rapid and efficient for the investigation of bioactivity of A. tegmentosum. PMID:25386382

  1. Activation of the Kelch-like ECH-associated protein 1 (Keap1)/NF-E2-related factor 2 (Nrf2) pathway through covalent modification of the 2-alkenal group of aliphatic electrophiles in Coriandrum sativum L.

    PubMed

    Abiko, Yumi; Mizokawa, Mai; Kumagai, Yoshito

    2014-11-12

    Phytochemicals able to activate the transcription factor NF-E2-related factor 2 (Nrf2) were isolated from an extract of Coriandrum sativum L. (C. sativum) leaves by preparative octadecyl silica column chromatography. Ultraperformance liquid chromatography and liquid chromatography-tandem mass spectrometry analysis of the isolated components after derivatization with 2-diphenylacetyl-1,3-inandione-1-hydrazone and experiments with HepG2 cells revealed that (E)-2-alkenals with different carbon numbers play a role in Nrf2 activation in these cells. Such Nrf2 activation appears to be attributable to S-alkylation of Kelch-like ECH-associated protein 1 (Keap1), the negative regulator for Nrf2, as determined by a biotin-PEAC5-maleimide assay. Interestingly, (E)-2-butenal caused Keap1 modification and Nrf2 activation, whereas butanal did not. These results suggest that (E)-2-alkenals with an α,β-unsaturated aldehyde moiety, which is a common substituent in phytochemicals isolated from C. sativum leaves, activate the Keap1/Nrf2 pathway associated with cellular protection.

  2. Rapid liquid chromatographic-mass spectrometric assay for oxymetazoline in whole rat blood.

    PubMed

    Hayes, F J; Baker, T R; Dobson, R L; Tsueda, M S

    1995-02-10

    A rapid HPLC-electrospray mass spectrometric assay for the quantitation of oxymetazoline in whole rat blood has been developed. Sample preparation was a single liquid-liquid extraction after addition of a deuterated internal standard (IS) and pH adjustment. An aliquot of reconstituted extract was injected onto a narrow-bore octadecyl reversed-phase column at a flow-rate of 400 microliters/min. Using a 20:1 post-column split, 5% of the eluent was introduced into the mass spectrometer interface. Elution of the analyte and IS occurred in less than 2 min. This rapid separation was made possible because of the sample cleanup and the selectivity of the mass spectrometric detection. The [M+H]+ ions for oxymetazoline (m/z 261) and [2H9]oxymetazoline (m/z 270) were detected using selected ion monitoring. The linear range of the assay was 0.67-167 ng/g of blood and the limit of quantitation with a 0.30-g sample was 1.0 ng/g. The assay permitted the analysis of nine samples per hour with the requisite sensitivity and selectivity and was used to determine the blood pharmacokinetics of oxymetazoline in rats dosed via intravenous and intranasal routes.

  3. A redox-responsive mesoporous silica nanoparticle capped with amphiphilic peptides by self-assembly for cancer targeting drug delivery.

    PubMed

    Xiao, Dong; Jia, Hui-Zhen; Ma, Ning; Zhuo, Ren-Xi; Zhang, Xian-Zheng

    2015-06-14

    A redox-responsive mesoporous silica nanoparticle (RRMSN) was developed as a drug nanocarrier by noncovalent functionalization of MSNs with amphiphilic peptides containing the RGD ligand. The alkyl chain stearic acid (C18) with a thiol terminal group was anchored on the surface of MSNs via a disulfide bond, and the amphiphilic peptide (AP) C18-DSDSDSDSRGDS was coated by self-assembly through hydrophobic interactions between the octadecyl groups of MSNs and alkyl chains of AP, which played the role of a gatekeeper collectively. In vitro drug release profiles demonstrated that the anticancer drug (DOX) could be entrapped with nearly no leakage in the absence of dithiothreitol (DTT) or glutathione (GSH). With the addition of DTT or GSH, the entrapped drug released quickly due to the cleavage of the disulfide bond. It was found that after the internalization of MSNs by cancer cells via the receptor-mediated endocytosis, the surface amphiphilic peptides and alkyl chain of RRMSN/DOX were removed to induce rapid drug release intracellularly after the cleavage of the disulfide bond, triggered by GSH secreted in cancer cells. This novel intelligent RRMSN/DOX drug delivery system using self-assembly of amphiphilic peptides around the MSNs provides a facile, but effective strategy for the design and development of smart drug delivery for cancer therapy.

  4. Global and specific migration of antioxidants from polypropylene films into food simulants.

    PubMed

    Garde, J A; Catalá, R; Gavara, R

    1998-08-01

    Global migration and specific migration of antioxidants (AOs--Irgafos 168 [tris(2,4-di-tert-butylphenyl) phosphite], Irganox 1076 [octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl-propionate], and Hostanox SE2 (distery thiodipropionate)--from polypropylene (PP) films into food simulants (water, 3% acetic acid, 95% ethanol, olive oil, and heptane) were studied. Films (50, 100, and 200 microns thick) were exposed to simulants at temperature-time conditions simulating migration under retorting and long-term storage. Global migration into aqueous simulants was independent of film thickness and conditions of exposure, so it seems as if the migration process was limited to the dissolution of migrants on the contacting surface. Global migration to fatty food simulants was dependent on simulant, conditions of exposure, and in some cases film thickness. Specific AO migration was analyzed from dry residues obtained from global migration analysis. Migration of AOs into aqueous simulants was below the detection limit (0.01 mg/dm2). Migration into fatty food simulants was dependent on the simulant. The extractive power of simulants was similar to that observed in global migration studies. Specific migration into heptane was independent of the polymer mass, though dependent on the thickness. Migration into ethanol was dependent on both mass and thickness. A theoretical discussion about the controversial effect of thickness on migration results, based on the kinetics of the process, is presented.

  5. Lipid nanoparticles for alkyl lysophospholipid edelfosine encapsulation: development and in vitro characterization.

    PubMed

    Estella-Hermoso de Mendoza, Ander; Rayo, Marta; Mollinedo, Faustino; Blanco-Prieto, María J

    2008-02-01

    The ether lipid 1-O-octadecyl-2-O-methyl-rac-glycero-3-phosphocholine, edelfosine (ET-18-OCH(3)) is the prototype molecule of a promising class of antitumor drugs named alkyl-lysophospholipid analogues (ALPs) or antitumor ether lipids. This drug presents a very important drawback as can be the dose dependent haemolysis when administered intravenously. Lipid nanoparticles have been lately proposed for different drug encapsulation as an alternative to other controlled release delivery systems, such as liposomes or polymeric nanoparticles. The aim of this study was to develop a lipid nanoparticulate system that would decrease systemic toxicity as well as improve the therapeutic potential of the drug. Lipids employed were Compritol 888 ATO and stearic acid. The nanoparticles were characterized by photon correlation spectroscopy for size and size distribution, and atomic force microscopy (AFM) was used for the determination of morphological properties. By both differential scanning calorimetry (DSC) and X-ray diffractometry, crystalline behaviour of lipids and drug was assessed. The drug encapsulation efficiency and the drug release kinetics under in vitro conditions were measured by HPLC-MS. It was concluded that Compritol presents advantages as a matrix material for the manufacture of the nanoparticles and for the controlled release of edelfosine. PMID:17707618

  6. Raman Spectroscopic Studies of Clathrate Hydrate Formation in the Presence of Hydrophobized Particles.

    PubMed

    Li, Huijuan; Stanwix, Paul; Aman, Zachary; Johns, Michael; May, Eric; Wang, Liguang

    2016-01-28

    In the present work, Raman spectroscopy was used to study the structure of water molecules in the vicinity of glass particles with different hydrophobicity, immersed in water and in tetrahydrofuran and cyclopentane hydrates. The glass particle surfaces were clean (hydrophilic), coated with N,N-dimethyl-N-octadecyl-3-aminopropyl trimethoxysilyl chloride (partially hydrophobic), or coated with octadecyltrichlorosilane (hydrophobic). The Raman spectra indicate that, prior to nucleation, water molecules in the vicinity of hydrophobic surfaces are more ice-like ordered than those in the bulk liquid or near either hydrophilic or partially hydrophobic surfaces. Furthermore, the degree of hydrogen-bond ordering of water observed prior to hydrate nucleation, as measured by the ratio of the inter- and intramolecular Raman OH bands, was found to have an inverse relationship with the mean induction time for hydrate formation. Following hydration formation, no significant difference in the water molecule structure was observed in the hydrate phase based on their Raman OH bands, irrespective of surface hydrophobicity. These observations made with Raman spectroscopy provide the foundations for a quantitative link between hydrate nucleation promotion and water-ordering near solid surfaces, which could enable direct comparisons with results from corresponding molecular dynamics simulations. PMID:26731126

  7. Collective fluorescence switching of counterion-assembled dyes in polymer nanoparticles

    NASA Astrophysics Data System (ADS)

    Reisch, Andreas; Didier, Pascal; Richert, Ludovic; Oncul, Sule; Arntz, Youri; Mély, Yves; Klymchenko, Andrey S.

    2014-06-01

    The current challenge in the field of fluorescent nanoparticles (NPs) for bioimaging is to achieve extreme brightness and external control of their emission using biodegradable materials. Here we propose a new concept of fluorescent polymer NPs, doped with ionic liquid-like salts of a cationic dye (octadecyl rhodamine B) with a bulky hydrophobic counterion (fluorinated tetraphenylborate) that serves as spacer minimizing dye aggregation and self-quenching. The obtained 40-nm poly(D,L-lactide-co-glycolide) NPs containing up to 500 dyes are brighter than quantum dots and exhibit photo-induced reversible on/off fluorescence switching, never reported for dye-doped NPs. We show that this collective switching of hundreds of dyes is due to ultrafast excitation energy transfer and can be used for super-resolution imaging. These NPs, being spontaneously endocytosed by living cells, feature high signal-to-noise ratio and absence of toxicity. The counterion-based concept opens the way to a new class of nanomaterials for sensing, imaging and light harvesting.

  8. Asphaltene Adsorption onto Self-Assembled Monolayers of Mixed Aromatic

    SciTech Connect

    Turgman-Cohen, S.; Smith, M; Fischer, D; Kilpatrick, P; Genzer, J

    2009-01-01

    The adsorption of asphaltenes onto flat solid surfaces modified with mixed self-assembled monolayers (SAMs) of aliphatic and aromatic trichlorosilanes with varying wettabilities, aromaticities, and thicknesses is tested. The mixed SAMs are characterized by means of contact angle to assess hydrophobicity and molecular and chemical uniformity, spectroscopic ellipsometry to measure the thickness of the films, and near edge X-ray absorption fine structure (NEXAFS) spectroscopy to assess chemical and molecular composition. The molecular characteristics of the adsorbed asphaltene layer and the extent of asphaltene adsorption are determined using NEXAFS and spectroscopic ellipsometry, respectively. The SAMs are formed by depositing phenyl-, phenethyl-, butyl-, and octadecyl- trichlorosilanes from toluene solutions onto silica-coated substrates; the chemical composition and the wettability of the SAM surface is tuned systematically by varying the trichlorosilane composition in the deposition solutions. The adsorption of asphaltenes on the substrates does not correlate strongly with the SAM chemical composition. Instead, the extent of asphaltene adsorption decreases with increasing SAM thickness. This observation suggests that the leading interaction governing the adsorption of asphaltenes is their interaction with the polar silica substrate and that the chemical composition of the SAM is of secondary importance.

  9. Label-free liquid crystal biosensor based on specific oligonucleotide probes for heavy metal ions.

    PubMed

    Yang, Shengyuan; Wu, Chao; Tan, Hui; Wu, Yan; Liao, Shuzhen; Wu, Zhaoyang; Shen, Guoli; Yu, Ruqin

    2013-01-01

    In this study, to enhance the capability of metal ions disturbing the orientation of liquid crystals (LCs), we designed a new label-free LC biosensor for the highly selective and sensitive detection of heavy metal ions. This strategy makes use of the target-induced DNA conformational change to enhance the disruption of target molecules for the orientation of LC leading to an amplified optical signal. The Hg(2+) ion, which possesses a unique property to bind specifically to two DNA thymine (T) bases, is used as a model heavy metal ion. In the presence of Hg(2+), the specific oligonucleotide probes form a conformational reorganization of the oligonucleotide probes from hairpin structure to duplex-like complexes. The duplex-like complexes are then bound on the triethoxysilylbutyraldehyde/N,N-dimethyl-N-octadecyl (3-aminopropyl) trimethoxysilyl chloride (TEA/DMOAP)-coated substrate modified with capture probes, which can greatly distort the orientational profile of LC, making the optical image of LC cell birefringent as a result. The optical signal of LC sensor has a visible change at the Hg(2+) concentration of low to 0.1 nM, showing good detection sensitivity. The cost-effective LC sensing method can translate the concentration signal of heavy metal ions in solution into the presence of DNA duplexes and is expected to be a sensitive detection platform for heavy metal ions and other small molecule monitors. PMID:23214408

  10. Thallium (III) determination in the Baltic seawater samples by ICP MS after preconcentration on SGX C18 modified with DDTC.

    PubMed

    Krasnodębska-Ostręga, Beata; Sadowska, Monika; Piotrowska, Katarzyna; Wojda, Marta

    2013-08-15

    The main difficulty of speciation analysis of thallium lies in extremely low concentrations of Tl(III) in comparison to Tl(I), which is the dominating form of thallium in environmental samples. In this study, a sensitive method is presented for separation of trace amounts of Tl(III) from Tl(I) and preconcentration of Tl(III) using octadecyl silica gel modified with diethyldithiocarbamate (DDTC). Under optimal conditions, only Tl(III) is retained on the sorbent, and then eluted with 96% ethanol. After chemical decomposition of Tl(III)-DDTC complex, thallium is determined by inductively coupled plasma mass spectrometry. High performance liquid chromatography with ICP MS detection was used to control the correctness of the obtained results. Parameters affecting solid phase extraction (SPE) such as pH, type, concentration and volume of eluent, breakthrough volume, and the impact of sample salinity (chlorides) and other interfering ions (Cd(II), Zn(II), Pb(II), Cu(II), Sn(II)) were investigated. The limit of detection (LOD), evaluated for 2 mL of sample solution, was 0.10 ng for Tl(I) and 0.43 ng for Tl(III). The method was applied to the determination of Tl(I) and Tl(III) in the Baltic seawater samples enriched in both thallium species.

  11. High-performance liquid chromatographic determination of azaarenes and their metabolites in groundwater affected by creosote wood preservatives.

    PubMed

    Ondrus, M G; Steinheimer, T R

    1990-06-01

    Polynuclear azaheterocyclic compounds (azaarenes) are nitrogen-containing analogs of polycyclic aromatic hydrocarbons (PAHs). The nitrogen atom in the ring system causes these compounds to be slightly polar and considerably more water soluble than related PAHs. A method using a solid-surface sorption technique to extract and concentrate azaarenes and their principle metabolites present in groundwater that contains creosote waste is described. Analyte isolation and concentration is accomplished by solid-phase extraction on n-octadecyl cartridges followed by instrumental determination involving high-performance liquid chromatography. Separations and detection are achieved using flexible-walled, wide-bore columns with ultraviolet and fluorescence photometric detectors connected in series. Fluorescence detection alone is insufficient because the fluorescence response produced by two-ring azaarenes is limited. Short wavelength (229 nm) absorbance detection provides improved sensitivity for these compounds and peak rationing for more definitive identification. In this study, oxygen-containing metabolites of quinoline, isoquinoline, and acridine are detected in groundwater from hazardous waste sites in Pensacola, Florida and St. Louis Park, Minnesota. Concentrations ranging from mg/L to ng/L are measured. The dependence of measured octanol-water partition coefficients on pH is discussed in the context of the isolation chemistry. As a direct bacterial degradation product of acridine with a relatively long environmental persistence, 9-acridinone may serve as a biogenic marker signaling creosote contamination of groundwater.

  12. Acrylate ester-based monolithic columns for capillary electrochromatography separation of triacylglycerols in vegetable oils.

    PubMed

    Lerma-García, M J; Vergara-Barberán, M; Herrero-Martínez, J M; Simó-Alfonso, E F

    2011-10-21

    A simple and reliable method for the evaluation of triacylglycerols (TAGs) in vegetable oils by capillary electrochromatography (CEC) with UV-Vis detection, using octadecyl acrylate (ODA) ester-based monolithic columns, has been developed. The percentages of the porogenic solvents in the polymerization mixture, and the mobile phase composition, were optimized. The optimum monolith was obtained at the following ratios: 40:60% (wt/wt) monomers/porogens, 60:40% (wt/wt) ODA/1,3-butanediol diacrylate and 23:77% (wt/wt) 1,4-butanediol/1-propanol (14 wt% 1,4-butanediol in the polymerization mixture). A satisfactory resolution between TAGs was achieved in less than 12 min with a 65:35 (v/v) acetonitrile/2-propanol mixture containing 5 mM ammonium acetate. The method was applied to the analysis of TAGs of vegetable oil samples. Using linear discriminant analysis of the CEC TAG profiles, the vegetable oils belonging to six different botanical origins (corn, extra virgin olive, hazelnut, peanut, soybean and sunflower) were correctly classified with an excellent resolution among all the categories.

  13. One-Pot Approach to Prepare Organo-silica Hybrid Capillary Monolithic Column with Intact Mesoporous Silica Nanoparticle as Building Block

    PubMed Central

    Liu, Shengju; Peng, Jiaxi; Liu, Zheyi; Liu, Zhongshan; Zhang, Hongyan; Wu, Ren’an

    2016-01-01

    A facile “one-pot” approach to prepare organo-silica hybrid capillary monolithic column with intact mesoporous silica nanoparticle (IMSN) as crosslinker and building block was described. An IMSN crosslinked octadecyl-silica hybrid capillary monolithic column (IMSN-C18 monolithic column) was successfully prepared, and the effects of fabrication conditions (e.g. concentration of intact mesoporous silica nanoparticle, polycondensation temperature, content of vinyltrimethoxysilane and stearyl methacrylate) on the structures of the IMSN-C18 monolithic column were studied in detail. The IMSN-C18 hybrid monolithic column possessed uniform morphology, good mechanical and pH stability (pH 1.1–11), which was applied to the separations of alkyl benzenes, polycyclic aromatic hydrocarbons (PAHs), as well as proteins. The minimum plate height of 10.5 μm (corresponding to 95000 N m−1) for butylbenzene and high reproducibility were achieved. The analysis of tryptic digest of bovine serum albumin (BSA) was carried out on the IMSN-C18 monolithic column by cLC coupled mass spectrometry (cLC-MS/MS), with the protein sequence coverage of 87.5% for BSA, demonstrating its potential application in proteomics. PMID:27698475

  14. One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks.

    PubMed

    Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Marina, María Luisa; Sierra, Isabel

    2016-01-01

    A new procedure for the determination of 12 naturally occurring hormones and some related synthetic chemicals in milk, commonly used as growth promoters in cattle, is reported. The method is based on liquid-liquid extraction followed by solid-phase extraction (SPE) using a new one-pot synthesized ordered mesoporous silica (of the SBA-15 type) functionalized with octadecyl groups (denoted as SBA-15-C18-CO) as reversed-phase sorbent. The analytes were eluted with methanol and then submitted to HPLC with diode array detection. Under optimal conditions, the method quantification limit for the analytes ranged from 0.023 to 1.36μg/mL. The sorbent affored the extraction of estrone, 17β-estradiol, estriol, progesterone, hexestrol, diethylstilbestrol, 4-androstene-3,17-dione, ethinylestradiol, 17α-methyltestosterone, nandrolone, prednisolone and testosterone with mean recoveries ranging from 72% to 105% (except for diethylstilbestrol) with RSD<11%. These results were comparable and, in some cases, even better than those obtained with other extraction methods, therefore SBA-15-C18-CO mesoporous silica possess a high potential as a reversed-phase sorbent for SPE of the 12 mentioned endocrine disrupting compounds in milk samples. PMID:26362809

  15. Development of new multifunctional terpolymer sorbent for proteomics applications.

    PubMed

    Najam-ul-Haq, Muhammad; Saeed, Adeela; Jabeen, Fahmida; Hussain, Dilshad; Khan, Naseem; Shabir, Maryam; Raza, Nadeem; Ashiq, Muhammad Naeem; Malana, Muhammad Aslam; Zafar, Zafar Iqbal

    2015-07-01

    Determination of the availability of phases for specific separations is an important task achieved by a separation chemist. This becomes vital when the complex samples like biofluids are dealt with in proteome science. The work presented here involves the synthesis and application of terpolymeric sorbent with different functionalizations adopted for the selective enrichment of biomolecules of interest from biological fluids. Synthesis of terpolymer was carried out by the radical polymerization of monomers: methyl acrylate, acrylic acid and vinyl acetate with diethylene glycol dimethacrylate as cross-linking agent, benzoyl peroxide as initiator and chloroform as a porogenic solvent. Characterization was done through Fourier transform infrared spectroscopy, scanning electron microscopy and nitrogen adsorption porosimetry. The polymer was further modified to immobilized metal ion affinity chromatographic material, with immobilized Fe(3+)/La(3+) ions that allowed phosphopeptide enrichment from tryptic digests of standard proteins as well as milk, egg yolk and human serum. Sensitivity of enrichment down to 50 fmol was achieved in the presence of complex protein background as bovine serum albumin. Hydrophobicity was introduced through octadecyl amine, which provides comparable results to ZipTip C18/C4 for desalting of complex mixtures of all caseins. Analysis of the enriched content was performed by Matrix Assisted Laser Desorption Ionization Mass Spectrometry (MALDI-MS). PMID:25402016

  16. Microstructure and rheology of a thermoreversible gel under large amplitude oscillatory shear (LAOS) deformation using time-resolved oscillatory rheo-small-angle neutron scattering (tOr-SANS)

    NASA Astrophysics Data System (ADS)

    Kim, Jung Min; Gurnon, A. Kate; Wagner, Norman; Eberle, Aaron

    2013-03-01

    Large amplitude oscillatory shear (LAOS) rheology is an effective way of studying the nonlinear dynamics of complex fluids. Here, we present a new method for a direct, quantitative study of the microstructure under LAOS deformation in the framework of the alignment factor, Af. We use a model thermoreversible adhesive hard-sphere system composed of octadecyl-coated silica particles suspended in n-tetradecane. With temperature the particle potential is controlled and the system is shifted from behaving as a near hard-sphere to an adhesive hard-sphere system leading to aggregation and ultimately a dynamical arrest transition to macroscopic gelation. Time-resolved oscillatory rheo-small-angle neutron scattering (tOr-SANS) measurements in the 1-3 plane are performed by stroboscopically probing the structural evolution as a function of time during LAOS. Under strong shear, the 2D scattering pattern of the system in the gelled state exhibits a strong anisotropy commonly known as a ``butterfly'' pattern, which corresponds to the stretching of the microstructure along the flow direction. The first structure-Lissajous plots of this model system are presented in terms of an order parameter and Af as a function of instantaneous strain and strain rate. This new analysis demonstrates a novel method for simultaneously measuring the rheology and microstructure during a time-dependent deformation (LAOS).

  17. A Case of Occupational Asthma in a Plastic Injection Process Worker

    PubMed Central

    2013-01-01

    Objectives We report a case of death due to asthma attack in a plastic injection process worker with a history of asthma. Methods To assess task relevance, personal history including occupational history and medical records were reviewed. Samples of the substances utilized in the injection process were collected by visiting the patient’s workplace. The work environment with the actual process was reproduced in the laboratory, and the released substances were evaluated. Results The medical records confirmed that the patient’s conventional asthma was in remission. The analysis of the resins discharged from the injection process simulation revealed styrene, which causes occupational asthma, and benzenepropanoic acid, 3,5-bis(1,1-dimethylethyl)-4-hydroxy-, and octadecyl ester. Even though it was not the case in the present study, various harmful substances capable of inducing asthma such as formaldehyde, acrolein, and acetic acid are released during resin processing. Conclusion A worker was likely to occur occupational asthma as a result of the exposure to the harmful substances generated during the plastic injection process. PMID:24472161

  18. In vitro angiotensin I converting enzyme inhibition by a peptide isolated from Chiropsalmus quadrigatus Haeckel (box jellyfish) venom hydrolysate.

    PubMed

    So, Pamela Berilyn T; Rubio, Peter; Lirio, Stephen; Macabeo, Allan Patrick; Huang, Hsi-Ya; Corpuz, Mary Jho-Anne T; Villaflores, Oliver B

    2016-09-01

    The anti-angiotensin I converting enzyme activity of box jellyfish, Chiropsalmus quadrigatus Haeckel venom hydrolysate was studied. The venom extract was obtained by centrifugation and ultrasonication. Protein concentration of 12.99 μg/mL was determined using Bradford assay. The pepsin and papain hydrolysate was tested for its toxicity by Limit test following the OECD Guideline 425 using 5 female Sprague-Dawley rats. Results showed that the hydrolysate is nontoxic with an LD50 above 2000 mg/kg. In vitro angiotensin I converting enzyme (ACE) inhibitory activity was determined using ACE kit-WST. Isolation of ACE inhibitory peptides using column chromatography with SP-Sephadex G-25 yielded 8 pooled fractions with fraction 3 (86.5%) exhibiting the highest activity. This was followed by reverse phase - high performance liquid chromatography (RP-HPLC) with an octadecyl silica column (Inertsil ODS-3) using methanol:water 15:85 at a flow rate of 1.0 mL/min. Among the 13 fractions separated with the RP-HPLC, fraction 3.5 exhibited the highest ACE inhibitory activity (84.1%). The peptide sequence ACPGPNPGRP (IC50 2.03 μM) from fraction 3.5 was identified using Matrix-assisted laser desorption/ionization with time-of-flight tandem mass spectroscopy analysis (MALDI-TOF/MS).

  19. Β-hydroxymyristic acid as a chemical marker to detect endotoxins in dialysis water.

    PubMed

    Mishra, Rupesh K; Robert-Peillard, Fabien; Ravier, Sylvain; Coulomb, Bruno; Boudenne, Jean-Luc

    2015-02-01

    An analytical chemical method has been developed for determination of β-hydroxymyristic acid (β-HMA), a component of lipopolysaccharides (LPSs/endotoxins) in dialysis water. In our investigation, the β-HMA component was used as a chemical marker for endotoxin presence in dialysis water because it is available in the molecular subunit (lipid A) and responsible for toxicity. It is the most abundant saturated fatty acid in that subunit. The developed method is based on fluorescence derivatization with 4-nitro-7-piperazino-2,1,3-benzoxadiazole (NBD-PZ). A high-performance liquid chromatographic separation of the β-HMA derivative was achieved using an octadecyl silica column in gradient elution. A wide dynamic range of β-HMA was tested and a calibration curve was constructed with accuracy of 90% and variability of less than 10%. The limits of detection and quantification obtained were 2 and 5μM, respectively. The developed method was applied to detect endotoxins in dialysis water by alkaline hydrolysis of LPS using NaOH (0.25M) at 60°C for 2h. After hydrolysis, free acid was detected as its NBD-PZ derivative using high-performance liquid chromatography/mass spectrometry (HPLC/MS). Good recovery rates ranging from 98 to 105% were obtained for β-HMA in dialysis water.

  20. Liquid chromatographic fractionations of mixtures of polystyrene oligomers

    SciTech Connect

    Curtis, M A; Webb, J W; Warren, D C; Brandt, V O; Gerberich, F G; Raut, K B; Rogers, L B

    1980-05-24

    Oligomer mixtures of 800, 2200, and 4000 molecular weight polystyrene have been fractionated using silica and bonded phase columns under similar conditions of solvent gradient and flow rate. Using a hexane/tetrahydrofuran gradient, the silica and nitro phases were best in that they separated 41 and 43 oligomers, respectively. At the other extreme, a phenyl bonded phase column gave virtually no resolution using a water/THF gradient and a cyano bonded phase column, using the earlier hexane/tetrahydrofuran system, resolved only 10 oligomers. Amino and octadecyl bonded phase columns gave results intermediate between these two extremes. The strength of the solvent used to dissolve the sample was found to be of critical importance. Use of too good a sample solvent seriously degraded the attainable resolution. When number average and weight average molecular weights for an 800 molecular weight polystyrene sample were calculated from the oligomer distribution, the silica column gave values which were most consistent with those reported from other methods.

  1. Analysis of creams. IV. Application of high performance liquid chromatography. Part I.

    PubMed

    Lake, O A; Hulshoff, A; Van De Vaart, F J; Indemans, A W

    1983-02-25

    The possibilities of applying reversed-phase high performance liquid chromatography to the analysis of o/w emulsion type creams without preceding sample clean-up were investigated. The chromatographic behaviour of cream base components and active compounds in reversed phase systems consisting of methanol-water mixtures as the mobile phase and a chemically bonded octadecyl stationary phase, was studied. A number of active compounds and the preservative (sorbic acid) could be determined--often in one chromatographic run--without complications, by simply dissolving the sample in a suitable solvent mixture and injecting an aliquot of the solution into the chromatograph. Separation was achieved by the proper choice of methanol content, pH and ionic strength of the eluent. The compounds were detected by UV absorption. Some of the lipophilic cream base components could easily be determined in the same manner, with methanol as the eluent and with refraction index detection. The developed procedure was applied to the analysis of a number of creams. Some of the results are presented as examples, demonstrating the suitability of the method for quality control purposes. PMID:6844121

  2. Chemical composition and anti-inflammatory activities of the essential oils from Acacia mearnsii de Wild.

    PubMed

    Avoseh, Opeyemi N; Oyedeji, Ope-oluwa O; Aremu, Kayode; Nkeh-Chungag, Benedicta N; Songca, Sandile P; Oluwafemi, Samuel O; Oyedeji, Adebola O

    2015-01-01

    The volatile oils of the leaves and the stem bark of Acacia mearnsii de Wild obtained by hydro-distillation were analysed by gas chromatography-mass spectrometry. A total of 20, 38, 29 and 38 components accounted for 93.8%, 92.1%, 78.5% and 90.9% of the total oils of the fresh, dry leaves and fresh, dry stem bark, respectively. The major components of the oil were octadecyl alcohol (25.5%) and phytol (10.5%); cis-verbenol (29.5%); phytol (10.1%) and phytol (23.4%) for the fresh leaves, dried leaves, fresh stem, dry stem bark, respectively. Oral administration of essential oils at a dose of 2% showed significant (p < 0.05) anti-inflammatory properties in the albumin-induced test model in rats. Oils from the fresh leaves and dry stems inhibited inflammation beyond 4 h post treatment. The potent anti-inflammatory activity of essential oils of A. mearnsii hereby confirmed its traditional use in treating various inflammatory diseases.

  3. Self-assembled monolayer-functionalized half-metallic manganite for molecular spintronics.

    PubMed

    Tatay, Sergio; Barraud, Clément; Galbiati, Marta; Seneor, Pierre; Mattana, Richard; Bouzehouane, Karim; Deranlot, Cyrile; Jacquet, Eric; Forment-Aliaga, Alicia; Jegou, Pascale; Fert, Albert; Petroff, Frédéric

    2012-10-23

    (La,Sr)MnO(3) manganite (LSMO) has emerged as the standard ferromagnetic electrode in organic spintronic devices due to its highly spin-polarized character and air stability. Whereas organic semiconductors and polymers have been mainly envisaged to propagate spin information, self-assembled monolayers (SAMs) have been overlooked and should be considered as promising materials for molecular engineering of spintronic devices. Surprisingly, up to now the first key step of SAM grafting protocols over LSMO surface thin films is still missing. We report the grafting of dodecyl (C12P) and octadecyl (C18P) phosphonic acids over the LSMO half-metallic oxide. Alkylphosphonic acids form ordered self-assembled monolayers, with the phosphonic group coordinated to the surface and alkyl chains tilted from the surface vertical by 43° (C12P) and 27° (C18P). We have electrically characterized these SAMs in nanodevices and found that they act as tunnel barriers, opening the door toward the integration of alkylphosphonic acid//LSMO SAMs into future molecular/organic spintronic devices such as spin OLEDs.

  4. Activation of the Kelch-like ECH-associated protein 1 (Keap1)/NF-E2-related factor 2 (Nrf2) pathway through covalent modification of the 2-alkenal group of aliphatic electrophiles in Coriandrum sativum L.

    PubMed

    Abiko, Yumi; Mizokawa, Mai; Kumagai, Yoshito

    2014-11-12

    Phytochemicals able to activate the transcription factor NF-E2-related factor 2 (Nrf2) were isolated from an extract of Coriandrum sativum L. (C. sativum) leaves by preparative octadecyl silica column chromatography. Ultraperformance liquid chromatography and liquid chromatography-tandem mass spectrometry analysis of the isolated components after derivatization with 2-diphenylacetyl-1,3-inandione-1-hydrazone and experiments with HepG2 cells revealed that (E)-2-alkenals with different carbon numbers play a role in Nrf2 activation in these cells. Such Nrf2 activation appears to be attributable to S-alkylation of Kelch-like ECH-associated protein 1 (Keap1), the negative regulator for Nrf2, as determined by a biotin-PEAC5-maleimide assay. Interestingly, (E)-2-butenal caused Keap1 modification and Nrf2 activation, whereas butanal did not. These results suggest that (E)-2-alkenals with an α,β-unsaturated aldehyde moiety, which is a common substituent in phytochemicals isolated from C. sativum leaves, activate the Keap1/Nrf2 pathway associated with cellular protection. PMID:25307732

  5. A polymeric fastener can easily functionalize liposome surfaces with gadolinium for enhanced magnetic resonance imaging.

    PubMed

    Smith, Cartney E; Shkumatov, Artem; Withers, Sarah G; Yang, Binxia; Glockner, James F; Misra, Sanjay; Roy, Edward J; Wong, Chun-Ho; Zimmerman, Steven C; Kong, Hyunjoon

    2013-11-26

    Common methods of loading magnetic resonance imaging (MRI) contrast agents into nanoparticles often suffer from challenges related to particle formation, complex chemical modification/purification steps, and reduced contrast efficiency. This study presents a simple, yet advanced process to address these issues by loading gadolinium, an MRI contrast agent, exclusively on a liposome surface using a polymeric fastener. The fastener, so named for its ability to physically link the two functional components together, consisted of chitosan substituted with diethylenetriaminepentaacetic acid (DTPA) to chelate gadolinium, as well as octadecyl chains to stabilize the modified chitosan on the liposome surface. The assembly strategy, mimicking the mechanisms by which viruses and proteins naturally anchor to a cell, provided greater T1 relaxivity than liposomes loaded with gadolinium in both the interior and outer leaflet. Gadolinium-coated liposomes were ultimately evaluated in vivo using murine ischemia models to highlight the diagnostic capability of the system. Taken together, this process decouples particle assembly and functionalization and, therefore, has considerable potential to enhance imaging quality while alleviating many of the difficulties associated with multifunctional particle fabrication.

  6. Effect of temperature on competitive adsorption of the solute and the organic solvent in reversed-phase liquid chromatography.

    PubMed

    Poplewska, Izabela; Piatkowski, Wojciech; Antos, Dorota

    2006-01-27

    In analysis of the temperature effect on chromatographic separations the influence of the adsorption of organic solvent on the retention properties of solute is generally not taken into account. In fact, adsorption behavior of solutes is strongly affected by competitive adsorption of organic solvents, which is temperature dependent. In this work changes of adsorption equilibrium of an organic solvent as well as a solute with temperature have been analyzed. Data of the excess adsorption of methanol from aqueous solutions on octadecyl-bonded silica have been acquired at different temperature. Experiments have been performed over a relatively narrow temperature range corresponding to typical chromatographic conditions, i.e., 10-50 degrees C. The competitive adsorption equilibria of model solutes (i.e., two homologous compounds: cyclopentanone and cyclohexanone) have been measured at different temperature and composition of the mobile phase. Temperature alterations to the retention properties were found to result from combined effects of changes in adsorption behavior of the organic solvent and of the solute. The influence of temperature on the separation selectivity has been considered.

  7. Phelligridins C-F: cytotoxic pyrano[4,3-c][2]benzopyran-1,6-dione and furo[3,2-c]pyran-4-one derivatives from the fungus Phellinus igniarius.

    PubMed

    Mo, Shunyan; Wang, Sujuan; Zhou, Guangxiong; Yang, Yongchun; Li, Yan; Chen, Xiaoguang; Shi, Jiangong

    2004-05-01

    Three unique pyrano[4,3-c][2]benzopyran-1,6-dione derivatives and a new furo[3,2-c]pyran-4-one, named phelligridins C-F (2-5), together with hispolon (8), (E)-4-(3,4-dihydroxyphenyl)but-3-en-2-one (9), 4-hydroxybenzaldehyde, protocatechualdehyde, syringic acid, protocatechuic acid, caffeic acid, isoergosterone, and octadecyl ferulate were isolated and identified from the ethanolic extract of Phellinus igniarius. Their structures were determined by spectroscopic methods including IR, MS, and 1D and 2D NMR experiments. The structures of the new compounds were characterized as 3-(4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (2), 3-(3,4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (3), 8,9-dihydroxy-3-[5',6'-dihydroxy-5' '-methyl-3' '-oxo-spiro[fural-2' '(3' 'H),1'-indene]-2'-yl]-1H,6H-pyrano[4,3-c][2]benzopyran-1,6-dione (4), and (3Z)-3-(3,4-dihydroxybenzylidene)-6-(3,4-dihydroxystyryl)-2,3-dihydro-2-methoxy-2-(2-oxo-propyl)furo[3,2-c]pyran-4-one (5), respectively. Some compounds including 2 and 3 showed in vitro selective cytotoxicity against a human lung cancer cell line (A549) and a liver cancer cell line (Bel7402). Possible biogenetic sequences to the formation of 1-9 are postulated.

  8. Second-harmonic generation from Z-type Langmuir-Blodgett films of a transparent dye and a comparison of the properties when the layers are interleaved with poly(t-butyl methacrylate)

    NASA Astrophysics Data System (ADS)

    Ashwell, Geoffrey J.; Ranjan, Rakesh

    1998-10-01

    The Langmuir-Blodgett (LB) film structure of E-4-[(N- octadecyl-6,7,8-trihydro-5-isoquinolylidene)methyl]-N,N- dibutylaniline octadecylsulfate is non-centrosymmetric when the dye is deposited on the up-stroke (Z-type) and when the layers are interleaved with poly(t-butyl methacrylate). The second-harmonic intensity increases as I(N)2(omega ) equals I(1)2(omega )N2, where N is the number of active layers, and the intensity is further enhanced when the dye is mixed in a 1 to 1 ratio with octadecanoic acid. The second-order susceptibility and repeat lattice spacing of the mixed LB films are as follows: (chi) zzz(2) equals 76 pm V-1 at 1.064 micrometers and l equals 3.15 nm layer-1 when Z-type; (chi) zzz(2) equals 52 pm V-1 and l equals 4.13 nm bilayer-1 when interleaved. The films are transparent at the fundamental wavelength and have a slight absorbance of ca. 5 X 10-4 per dye layer at 532 nm. The second-harmonic intensity is the strongest to date from such a weakly absorbing LB film and this is attributed to the close proximity of the charge-transfer band and to an optimized packing arrangement.

  9. Differential attractiveness of human foot odours to Anopheles gambiae Giles sensu stricto (Diptera: Culicidae) and variation in their chemical composition.

    PubMed

    Omolo, M O; Njiru, B; Ndiege, I O; Musau, R M; Hassanali, A

    2013-10-01

    Counter flow geometry (CFG) traps (American Biophysics) baited with foot odours (adsorbed overnight on a combination of a nylon and a cotton socks) from 4 groups of 4 male volunteers were initially used in a screen-house to compare and grade the attractiveness of Anopheles gambiae Giles sensu stricto to these odours. Ten individuals were then selected from the 4 groups for further grading in which mosquito attractiveness to odours adsorbed on socks worn by each of the individuals was compared against a control (clean, un-worn cotton and nylon socks). A gradation of attractiveness was found, with the most attractive foot odour catching 8-fold more mosquitoes than the least attractive one (t-test, p=0.001). For comparison of the chromatographic profiles of the foot odours and identification of their constituents, six adsorbents (tenax, chromsorb, porapak Q, activated charcoal, reverse phase octadecyl and octyl bonded silica) were evaluated for their suitability in trapping the volatiles in a static mode. Of these, porapak Q was found to be the most effective. Comparison of the gas-chromatographic (GC) and gas chromatography-linked mass spectrometry (GC-MS) profiles of blends collected from the most and least attractive feet on porapak Q adsorbent revealed both qualitative and quantitative differences. The implication of our finding on differential attraction of An. gambiae to their preferred feeding site of different human subjects is highlighted.

  10. Exploiting Fast Exciton Diffusion in Dye-Doped Polymer Nanoparticles to Engineer Efficient Photoswitching.

    PubMed

    Trofymchuk, Kateryna; Prodi, Luca; Reisch, Andreas; Mély, Yves; Altenhöner, Kai; Mattay, Jochen; Klymchenko, Andrey S

    2015-06-18

    Photoswitching of bright fluorescent nanoparticles opens new possibilities for bioimaging with superior temporal and spatial resolution. However, efficient photoswitching of nanoparticles is hard to achieve using Förster resonance energy transfer (FRET) to a photochromic dye, because the particle size is usually larger than the Förster radius. Here, we propose to exploit the exciton diffusion within the FRET donor dyes to boost photoswitching efficiency in dye-doped polymer nanoparticles. To this end, we utilized bulky hydrophobic counterions that prevent self-quenching and favor communication of octadecyl rhodamine B dyes inside a polymer matrix of poly(D,L-lactide-co-glycolide). Among tested counterions, only perfluorinated tetraphenylborate that favors the exciton diffusion enables high photoswitching efficiency (on/off ratio ∼20). The switching improves with donor dye loading and requires only 0.1-0.3 wt % of a diphenylethene photochromic dye. Our nanoparticles were validated both in solution and at the single-particle level. The proposed concept paves the way to new efficient photoswitchable nanomaterials.

  11. Gelation in a model 1-component system with adhesive hard-sphere interactions

    NASA Astrophysics Data System (ADS)

    Kim, Jung Min; Eberle, Aaron; Fang, Jun; Wagner, Norman

    2012-02-01

    Colloidal dispersions can undergo a dynamical arrest of the disperse phase leading to a system with solid-like properties when either the volume fraction or the interparticle potential is varied. Systems that contain low to moderate particulate concentrations form gels whereas higher concentrations lead to glassy states in which caging by nearest neighbors can be a significant contributor to the arrested long-time dynamics. Colloid polymer mixtures have been the prevalent model system for studying the effect of attraction, where attractions are entropically driven by depletion effects, in which gelation has been shown to be a result of phase separation [1]. Using the model 1-component octadecyl coated silica nanoparticle system, Eberle et al. [2] found the gel-line to intersect the spinodal to the left of the critical point, and at higher concentrations extended toward the mode coupling theory attractive driven glass line. . We continue this study by varying the particle diameter and find quantitative differences which we explain by gravity. 1. Lu, P.J., et al., Nature, 2008. 453(7194): p. 499-504.2. Eberle, A.P.R., N.J. Wagner, and R. Castaneda-Priego, Physical Review Letters, 2011. 106(10).

  12. Optically active microspheres constructed by helical substituted polyacetylene and used for adsorption of organic compounds in aqueous systems.

    PubMed

    Liang, Junya; Song, Ci; Deng, Jianping

    2014-11-12

    This article reports optically active microspheres consisting of chiral helical substituted polyacetylene and β-cyclodextrin-derivative (β-CD-A). The microspheres showed remarkable adsorption toward various organic compounds in water. To prepare the microspheres, an acetylenic-derived helical macro-monomer was synthesized and then underwent aqueous suspension copolymerization with octadecyl acrylate and butyl acrylate by using azobis(isobutyronitrile) as initiator and β-CD-A simultaneously as comonomer and cross-linking agent. The helical macro-monomer chains enabled the microspheres to exhibit desirable enantio-differentiating adsorption capacity toward chiral compounds respectively dissolved in organic solvent, dispersed in water, and dissolved in water. The saturated absorbency toward (R)-(+)- and (S)-(-)-1-phenylethylamine was 29 and 12 mg · g(-1), respectively. The microspheres also showed large oil absorbency (e.g., 22 g · g(-1) CCl4) and a large adsorption toward methyl red (as a model for organic dyes) dispersed in water. The presence of β-CD-A moieties improved the adsorption performance of the microspheres. The present optically active microspheres open a new approach for preparing adsorbents particularly chiral adsorbents with potentials for wastewater treatment. PMID:25290256

  13. β-Cyclodextrin-based oil-absorbent microspheres: preparation and high oil absorbency.

    PubMed

    Song, Ci; Ding, Lei; Yao, Fei; Deng, Jianping; Yang, Wantai

    2013-01-01

    This article reports the preparation and evaluation of polymeric microspheres as a new class of oil-absorbent (POAMs). Based on our earlier oil-absorbents, the present microspheres contained β-cyclodextrin (β-CD) moieties as both cross-linking agent and porogen agent, and showed exciting high oil absorbency, fast oil absorption speed and good reusability. Such microspheres were prepared via suspension polymerization with octadecyl acrylate and butyl acrylate as co-monomers, β-CD derivative as cross-linking agent, 2,2'-azoisobutyronitrile as initiator and polyvinylalcohol as stabilizer. Oil absorbency of the POAMs was, for CCl(4), 83.4; CHCl(3), 75.1; xylene, 48.7; toluene, 42.8; gasoline, 30.0; kerosene 27.1; and diesel, 18.2 g/g (oil/POAMs). Saturation oil absorption reached within 3h in CCl(4). The POAMs exhibited high oil retention percentage (>90%), and can be reused for at least 10 times while keeping oil absorbency almost unchanged. PMID:23044125

  14. Determination of hydrophobicity of non-homologous series of anticancer drugs by reversed-phase high-performance liquid chromatography.

    PubMed

    Forgács, E; Cserháti, T

    1995-02-01

    The hydrophobicity and specific hydrophobic surface area of 21 commercial anticancer drugs were determined by reversed-phase high-performance liquid chromatography on an octadecyl-silica column using methanol-water mixtures as eluents. Linear correlations were calculated between the log k' values and the methanol concentration of the eluent, the intercept and slope were considered as the best estimation of the hydrophobicity and specific hydrophobic surface area. The relationship between retention characteristics and physicochemical parameters of drugs was evaluated by multivariate mathematical statistical methods, such as principal component analysis followed by two-dimensional non-linear mapping, varimax rotation and by cluster analysis. Anticancer drugs can be well separated by reversed-phase HPLC. Various multivariate mathematical statistical calculations indicate that the retention of the investigated drugs is mainly governed by hydrophobic and steric parameters. The results suggest that the use of principal component analysis followed by two-dimensional non-linear mapping is superior to cluster analysis for the evaluation of large retention data matrices.

  15. A Facile Strategy for Catalyst Separation and Recycling Suitable for ATRP of Hydrophilic Monomers Using a Macroligand.

    PubMed

    Jiang, Xiaowu; Wu, Jian; Zhang, Lifen; Cheng, Zhenping; Zhu, Xiulin

    2016-01-01

    How to simply and efficiently separate and recycle catalyst has still been a constraint for the wide application of atom transfer radical polymerization (ATRP), especially for the polymerization systems with hydrophilic monomers because the polar functional groups may coordinate with transition metal salts, resulting in abundant catalyst residual in the resultant water-soluble polymers. In order to overcome this problem, a latent-biphasic system is developed, which can be successfully used for ATRP catalyst separation and recycling in situ for various kinds of hydrophilic monomers for the first time, such as poly(ethylene glycol) monomethyl ether methacrylate (PEGMA), 2-hydroxyethyl methacrylate (HEMA), 2-(dimethylamino)ethyl methacrylate (DMAEMA), N,N-dimethyl acrylamide (DMA), and N-isopropylacrylamide (NIPAM). Herein, random copolymer of octadecyl acrylate (OA), MA-Ln (2-(bis(pyridin-2-ylmethyl)amino)ethyl acrylate), and POA-ran-P(MA-Ln) is designed as the macroligand, and heptane/ethanol is selected as the biphasic solvent. Copper(II) bromide (CuBr2 ) is employed as the catalyst, PEG-bound 2-bromo-2-methylpropanoate (PEG350 -Br) as the water-soluble ATRP initiator and 2,2'-azobis(isobutyronitrile) (AIBN) as the azo-initiator to establish an ICAR (initiators for continuous activator regeneration) ATRP system. Importantly, well-defined water-soluble polymers are obtained even though the recyclable catalyst is used for sixth times.

  16. Solid-phase extraction-gas chromatography and solid-phase extraction-gas chromatography-mass spectrometry determination of corrosion inhibiting long-chain primary alkyl amines in chemical treatment of boiler water in water-steam systems of power plants.

    PubMed

    Kusch, Peter; Knupp, Gerd; Hergarten, Marcus; Kozupa, Marian; Majchrzak, Maria

    2006-04-28

    Gas chromatography with simultaneous flame-ionization detection (FID) and a nitrogen-phosphorus detection (NPD) as well as gas chromatography-mass spectrometry (GC/MS) has been used to characterize long-chain primary alkyl amines after derivatization with trifluoroacetic anhydride (TFAA). Electron impact ionization- (EI) and negative chemical ionization (NCI) mass spectra of trifluoroacetylated derivatives of the identified tert-octadecylamines are presented for the first time. The corrosion inhibiting alkyl amines were applied in a water-steam circuit of energy systems in the power industry. Solid-phase extraction (SPE) with octadecyl bonded silica (C18) sorbents followed by gas chromatography were used for quantification of the investigated tert-octadecylamines in boiler water, superheated steam and condensate samples from the power plant. The estimated values were: 89 microg l(-1)(n = 5, RSD = 7.8%), 45 microg l(-1) (n = 5, RSD = 5.4%) and 37 microg l(-1)(n = 5, RSD = 2.3%), respectively.

  17. Development and Validation of Reversed-Phase High Performance Liquid Chromatographic Method for Hydroxychloroquine Sulphate

    PubMed Central

    Singh, A.; Roopkishora; Singh, C. L.; Gupta, R.; Kumar, S.; Kumar, M.

    2015-01-01

    In the present work new, simple reversed-phase high performance liquid chromatographic method was developed and validated for the determination of hydroxychloroquine sulphate in blood plasma. Chloroquine sulphate was used as an internal standard. The chromatographic separation was achieved with octadecyl silane Hypersil C18 column (250×6 mm, 5 μm) using water and organic (acetonitrile:methanol: 50:50, v/v) mobile phase in 75:25 v/v ratio, with sodium 1-pentanesulfonate and phosphoric acid. This organic phase was maintained at pH 3.0 by orthophosphoric acid. The flow rate of 2.0 ml/min. with detection at 343 nm was used in the analysis. The calibration curve of standard hydroxychloroquine sulphate was linear in range 0.1-20.0 μg/ml. The method was validated with respected to linearity, range, precision, accuracy, specificity and robustness studies according to ICH guidelines. The method was found to be accurate and robust to analyze the hydroxychloroquine sulphate in plasma samples. PMID:26798174

  18. Development and Validation of Reversed-Phase High Performance Liquid Chromatographic Method for Hydroxychloroquine Sulphate.

    PubMed

    Singh, A; Roopkishora; Singh, C L; Gupta, R; Kumar, S; Kumar, M

    2015-01-01

    In the present work new, simple reversed-phase high performance liquid chromatographic method was developed and validated for the determination of hydroxychloroquine sulphate in blood plasma. Chloroquine sulphate was used as an internal standard. The chromatographic separation was achieved with octadecyl silane Hypersil C18 column (250×6 mm, 5 μm) using water and organic (acetonitrile:methanol: 50:50, v/v) mobile phase in 75:25 v/v ratio, with sodium 1-pentanesulfonate and phosphoric acid. This organic phase was maintained at pH 3.0 by orthophosphoric acid. The flow rate of 2.0 ml/min(.) with detection at 343 nm was used in the analysis. The calibration curve of standard hydroxychloroquine sulphate was linear in range 0.1-20.0 μg/ml. The method was validated with respected to linearity, range, precision, accuracy, specificity and robustness studies according to ICH guidelines. The method was found to be accurate and robust to analyze the hydroxychloroquine sulphate in plasma samples. PMID:26798174

  19. Microwave synthesis, characterization, and bio-efficacy of novel halogenated Schiff bases.

    PubMed

    Singh, Braj B; Shakil, Najam A; Kumar, Jitendra; Rana, Virendra S; Mishra, Anuradha

    2016-08-01

    A new series of halogenated Schiff bases was synthesized by the condensation of 5-fluoro-2-hydroxy acetophenone and 3,5-dichloro-2-hydroxy acetophenone with different alkyl amines, namely propyl, pentyl, hexyl, heptyl, octyl, nonyl, dodecyl, tetradecyl, hexadecyl, and octadecyl amines, under microwave irradiation. Newly formed molecules were characterized by Infrared and nuclear magnetic resonance ((1)H NMR and (13)C NMR) spectroscopic techniques. Further, the Schiff bases were screened for antifungal bioassay, and the results showed potential fungicidal activity against two very important plant infecting fungi, viz. Rhizoctonia solani and Sclerotium rolfsii. Among the screened compounds, 2,4-dichloro-2-[1-(propylimino)ethyl]phenol was found to be the most active compound against both R. solani (ED50 8.02 mg L(-1)) and S. rolfsii (ED50 21.51 mg L(-1)) followed by 2,4-dichloro-2-[1-(pentylimino) ethyl]phenol (ED50 13.02 and 29.57 mg L(-1), respectively). The synthesized compounds were also screened for antioxidant activity by 2,2-diphenyl-1-picrylhydrazyl (DPPH)-free radical scavenging technique. All the compounds showed very low to moderate activity as compared with Gallic acid. PMID:27167104

  20. Pressurized CEC with amperometric detection using mixed-mode monolithic column for rapid analysis of chlorophenols and phenol.

    PubMed

    Lu, Lanxiang; Chen, Yankai; Yu, Xiaowei; Wu, Xiangzong; Tang, Fengxiang; Wu, Xiaoping

    2013-07-01

    A simple analysis of chlorophenols (2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, and pentachlorophenol) and phenol was accomplished by coupling a pressurized CEC with amperometric detection (AD). Efficient and reproducible separation of these compounds was achieved within 9 min on a capillary monolithic stationary phase bonded with octadecyl ligands and sulfonate groups, where the selectivity and the retention of analytes can be functionally controlled by optimizing experimental variables, including organic modifier content, mobile phase pH, ionic strength, working electrode potential, separation voltage, and supplementary pressure. A mixed-mode retention mechanism consisting of reverse-phase chromatographic partition, electrostatic repulsion, and electrophoresis is considered to play roles in the separation. The use of ACN-based media seems effectual in preventing the unfavorable irreversible adsorption on both wall and electrode, and offer higher sensitivity and less electrode fouling in AD of phenols. The LODs were in the range from 0.02 to 0.2 μg/mL with a wide linear dynamic range of 5000-fold, while the peak area precision ranged from 3.2 to 7.5%. The feasibility of using this method in real analysis was evaluated by recovery estimates and comparative experiment on spiked tap water samples. Good recoveries of 80-110% were achieved. Additionally, a paired t-test was used to correlate the two methods.

  1. Control of Pre-Tilt Angles of Liquid Crystal Molecules Using a Chemically Adsorbed Monomolecular Layer as an Alignment Film in Liquid Crystal Cells

    NASA Astrophysics Data System (ADS)

    Ogawa, Kazufumi; Ohtake, Tadashi; Nomura, Takaiki

    2002-11-01

    Photoaligned monomolecular layers containing two materials were formed to control pre-tilt angles (θp) of liquid crystal molecules for twisted nematic (TN) type liquid crystal displays (LCDs) by a chemical adsorption (CA) technique and a photoalignment technique. One was a new chlorosilane type surfactant, 4‧-(6-trichlorosilyloxyhexyloxy) chalcone (CO), having photopolymerizablity, and the other was a surfactant having a straight carbon chain (SC). Although we tried screening six different surfectants as an additive to CO, a surfactant having a long straight hydrocarbon chain (octadecyl-trichlorosilane: C18) was the most suitable for the TN type LCDs. By changing the molecular ratio of CO and C18, pre-tilt angles of liquid crystal molecules in a test liquid crystal (LC) cell could be controlled from 0 to 8° with perfect mono-domain alignment. When surfactants having short hydrocarbon chains and those having fluorocarbon chains were used, the quality of the TN type LC cells obtained was not good.

  2. Propylammonium nitrate as a solvent for amphiphile self-assembly into micelles, lyotropic liquid crystals, and microemulsions.

    PubMed

    Atkin, Rob; Bobillier, Sophie M C; Warr, Gregory G

    2010-01-28

    The phase behavior and self-assembled microstructures of a range of oligo(oxyethylene)-n-alkyl ether (C(i)E(j)) surfactants has been investigated in propylammonium nitrate (PAN), a room temperature ionic liquid. Micelles and single-phase microemulsions were all found to form at alkyl chain lengths from dodecyl to octadecyl, and lyotropic liquid crystals formed with hexadecyl chains or longer. Small-angle neutron scattering (SANS) shows that self-assembly occurs by solvophobic interactions driving the aggregation of the alkyl chains, but several results indicate that these are weaker in PAN than in water or ethylammonium nitrate, due chiefly to the hydrophobicity of PAN. Longer alkyl chains are needed for lyotropic liquid crystals to form, and higher surfactant concentrations are needed to form a single phase microemulsion. Conductivity shows these microemulsions to be weakly structured, and relatively insensitive to oil or surfactant molecular structure, unlike water-based systems. However, SANS contrast variation reveals a nanosegregation of oil from the alkyl tails of surfactants within the microemulsion, and may suggest a cosurfactant-like role for the propylammonium cation. Molecular areas within microemulsions and lamellar phases are larger than corresponding water- or ethylammonium nitrate-based systems due to the large molecular volume of the solvating PANs. PMID:20039680

  3. A Facile Strategy for Catalyst Separation and Recycling Suitable for ATRP of Hydrophilic Monomers Using a Macroligand.

    PubMed

    Jiang, Xiaowu; Wu, Jian; Zhang, Lifen; Cheng, Zhenping; Zhu, Xiulin

    2016-01-01

    How to simply and efficiently separate and recycle catalyst has still been a constraint for the wide application of atom transfer radical polymerization (ATRP), especially for the polymerization systems with hydrophilic monomers because the polar functional groups may coordinate with transition metal salts, resulting in abundant catalyst residual in the resultant water-soluble polymers. In order to overcome this problem, a latent-biphasic system is developed, which can be successfully used for ATRP catalyst separation and recycling in situ for various kinds of hydrophilic monomers for the first time, such as poly(ethylene glycol) monomethyl ether methacrylate (PEGMA), 2-hydroxyethyl methacrylate (HEMA), 2-(dimethylamino)ethyl methacrylate (DMAEMA), N,N-dimethyl acrylamide (DMA), and N-isopropylacrylamide (NIPAM). Herein, random copolymer of octadecyl acrylate (OA), MA-Ln (2-(bis(pyridin-2-ylmethyl)amino)ethyl acrylate), and POA-ran-P(MA-Ln) is designed as the macroligand, and heptane/ethanol is selected as the biphasic solvent. Copper(II) bromide (CuBr2 ) is employed as the catalyst, PEG-bound 2-bromo-2-methylpropanoate (PEG350 -Br) as the water-soluble ATRP initiator and 2,2'-azobis(isobutyronitrile) (AIBN) as the azo-initiator to establish an ICAR (initiators for continuous activator regeneration) ATRP system. Importantly, well-defined water-soluble polymers are obtained even though the recyclable catalyst is used for sixth times. PMID:26506506

  4. Simple method for the analysis of food dyes on reversed-phase thin-layer plates.

    PubMed

    Oka, H; Ikai, Y; Kawamura, N; Yamada, M; Inoue, H; Ohno, T; Inagaki, K; Kuno, A; Yamamoto, N

    1987-12-18

    A technique for the determination of food dyes using reversed-phase thin-layer chromatography on octadecyl-modified silica is described. A solvent system containing 5.0% aqueous sodium sulphate solution enables good separation of the food dyes. Their separation is dependent on the pH of the solvent system, good separation among all dyes being obtained between pH 6.0 and 7.0. The determination of thirteen dyes can be achieved by a combination of methanol-acetonitrile-5.0% aqueous sodium sulphate solution (3:3:10) (solvent system A) and methanol-methyl ethyl ketone-5.0% aqueous sodium sulphate solution (1:1:1) (solvent system B). Solvent system A was used for the determination of Tartrazine, Amaranth, Indigo Carmine, New Coccine, Sunset Yellow FCF, Allura Red AC, Fast Green FCF and Brilliant Blue FCF and for the screening of Acid Red (R-106), Eosin (R-103), Erythrosin (R-3), Rose Bengale (R-105) and Phloxine (R-104). When the spots of R-3, R-103, R-104, R-105 and R-106 appear on the plate, their determination can be achieved by using solvent system B. Each calibration graph was linear between 0.2 and 1.0 micrograms.

  5. 1 -O-alkyl-2-(omega-oxo)acyl-sn-glycerols from shark oil and human milk fat are potential precursors of PAF mimics and GHB.

    PubMed

    Hartvigsen, Karsten; Ravandi, Amir; Harkewicz, Richard; Kamido, Hiroshi; Bukhave, Klaus; Hølmera, Gunhild; Kuksis, Arnis

    2006-07-01

    This study examines the feasibility that peroxidation and lipolysis of 1-O-alkyl-2,3-diacyl-sn-glycerols (DAGE) found in shark liver oil and human milk fat constitutes a potential source of dietary precursors of platelet activating factor (PAF) mimics and of gamma-hydroxybutyrate (GHB). Purified DAGE were converted into 1-O-alkyl-2-acyl-sn-glycerols by pancreatic lipase, without isomerization, and transformed into 1-O-alkyl-2-oxoacyl-sn-glycerols by mild autooxidation. The various core aldehydes without derivatization, as well as the corresponding dinitrophenylhydrazones, were characterized by chromatographic retention time and diagnostic ions by online electrospray mass spectrometry. Core aldehydes of oxidized shark liver oil yielded 23 molecular species of 1-O-alkyl-sn-glycerols with short-chain sn-2 oxoacyl groups, ranging from 4 to 13 carbons, some unsaturated. Autooxidation of human milk fat yielded 1-O-octadecyl-2-(9-oxo)nonanoyl-sn-glycerol, as the major core aldehyde. Because diradylglycerols with short fatty chains are absorbed in the intestine and react with cytidine diphosphate-choline in the enterocytes, it is concluded that formation of such PAF mimics as 1-O-alkyl-2-(omega-oxo)acyl-sn-glycerophosphocholine from unsaturated dietary DAGE is a realistic possibility. Likewise, a C4 core alcohol produced by aldol-keto reduction of a C4 core aldehyde constitutes a dietary precursor of the neuromodulator and recreational drug GHB, which has not been previously pointed out.

  6. Isolation and sequence determination of trichorzianines A antifungal peptides from Trichoderma harzianum.

    PubMed

    el Hajji, M; Rebuffat, S; Lecommandeur, D; Bodo, B

    1987-02-01

    Trichorzianines A, membrane active peptides of the peptaibol class, were isolated from cultures of the mould Trichoderma harzianum. Trichorzianines A were separated into pure components by HPLC on octadecyl bonded and SiO2 phases successively. Nine trichorzianines A (IIa, IIIa, IIIb, IIIc, IVb, Vb, VIa, VIb and VII) were isolated from the complex microheterogeneous mixture. Their N-terminal amino acid is acetylated, the C-terminal amino alcohol is either tryptophanol or phenylalaninol, 7 to 8 of the 19 residues are alpha-aminoisobutyric acid. Gas chromatography on a chiral phase showed isovaline to have the D-configuration and all the other optically active amino acids and amino alcohols to have the L-configuration. The amino acid sequences were determined from their positive ion FAB mass spectra which exhibited the preferential cleavage of the Aib 12-Pro 13 amide bond as a main fragmentation. The resulting fragments subsequently underwent amide bond ruptures that generated two series of abundant acylium ions which enabled direct determination of the 1-19 sequence. The relative position of the isomeric amino acids in the sequence of trichorzianine AVII was assigned from analysis of the N- and C-terminal oligopeptides yielded by its selective acidic hydrolysis. The microheterogeneity of trichorzianines A results mainly from single or multiple substitution of amino acids at the specific positions 5, 14, 16 and 19. PMID:3570662

  7. The antiproliferative effect of hexadecylphosphocholine toward HL60 cells is prevented by exogenous lysophosphatidylcholine.

    PubMed

    Boggs, K; Rock, C O; Jackowski, S

    1998-01-01

    The mechanisms that account for the anti-proliferative properties of the biologically active lysophospholipid analog hexadecylphosphocholine (HexPC) were investigated in HL60 cells. HexPC inhibited the incorporation of choline into phosphatidylcholine and the pattern of accumulation of soluble choline-derived metabolites pinpointed CTP:phosphocholine cytidylyltransferase (CT) as the inhibited step in vivo. HexPC also inhibited recombinant CT in vitro. HexPC treatment led to accumulation of cells in G2/M phase, triggered DNA fragmentation and caused morphological changes associated with apoptosis. The supplementation of HexPC-treated cells with exogenous lysophosphatidylcholine (LPC) completely reversed the cytotoxic effects of HexPC and restored HL60 cell proliferation in the presence of the drug. LPC provided an alternate pathway for phosphatidylcholine synthesis via the acylation of exogenous LPC. This result contrasted with the response of HL60 cells to 1-O-octadecyl-2-O-methyl-rac-glycero-3-phosphocholine (ET-18-OCH3) where LPC overcame the cytotoxic effects but did not support continued cell proliferation. Morphological integrity, DNA stability and cell viability were maintained in cells treated with LPC plus either antineoplastic agent. Thus the inhibition of phosphatidylcholine biosynthesis at the CT step accounts for the cytotoxicity of both HexPC and ET-18-OCH3 which is overridden by providing an alternate pathway for phosphatidylcholine synthesis via the acylation of exogenous LPC.

  8. Comparison of extraction methods and detection systems in the gas chromatographic analysis of volatile carbonyl compounds.

    PubMed

    Stashenko, E E; Ferreira, M C; Sequeda, L G; Martínez, J R; Wong, J W

    1997-08-29

    High-resolution gas chromatography (HRGC) with electron-capture detection (ECD), nitrogen-phosphorus detection (NPD), flame ionization detection (FID) or with mass spectrometry-selected ion monitoring (MS-SIM) was used in the analysis of volatile carbonyl compounds. Eighteen carbonyl compounds that are typically produced during lipid peroxidation were derivatized quantitatively with pentafluorophenylhydrazine (PFPH) at room temperature, to afford their corresponding water-insoluble hydrazones. These derivatives were extracted into non-polar phases by means of either liquid-liquid extraction (LLE) (hexane) or solid-phase extraction (SPE) on 3 ml C18 octadecyl-bonded phase cartridges. Detection limits of 10(-14) and 10(-12) mol/ml per aldehyde were achieved with the ECD and MS-SIM systems, respectively. The effects of extraction conditions on sensitivity and recovery were determined by performing parallel HRGC-ECD and HRGC-MS-SIM analyses of pentafluorophenylhydrazones of the eighteen compounds under study. Recoveries of 51.4-78.9 +/- 1.2-4.5 and 80.9-98.3 +/- 1.0-3.5% were obtained with LLE and SPE, respectively. The method was applied to the analysis of the volatile carbonyl compounds in various heated vegetable oils (corn, palm or sunflower) and to the analysis of volatile aldehydes in human urine. PMID:9335127

  9. Rapid and simultaneous measurement of estrone, estradiol, estriol and estetrol in serum by high performance liquid chromatography with electrochemical detection.

    PubMed

    Hayashi, N; Hayata, K; Sekiba, K

    1985-04-01

    A high performance liquid chromatographic (HPLC) method with electrochemical detection (ECD) was developed for the simultaneous measurement of estrone, estradiol, estriol and estetrol in serum. These hormones were extracted with diethylether, chromatographed on an silica-octadecyl silane (ODS) column with an eluent of phosphate buffer solution-acetonitrile-methanol (volume ratio 152:85:40), and detected by ECD at +1.0V vs. Ag/AgCl. In comparisons between the values measured by this method and radioimmunoassay, significant correlations were noted for estrone (r = 0.759, p less than 0.01), estradiol (r = 0.816, p less than 0.001) and estriol (r = 0.830, p less than 0.001). In clinical applications of this method, differences between cases of the normal and the anencephalic pregnancy in the thirty-eighth week of gestation were distinct not only in the individual estrogen, but also in the profile analysis of estrogens. With this method, all 4 serum estrogens above approximately 500 pg/ml could be measured within 2 h, and the method seemed to be clinically applicable. PMID:4003113

  10. Solid-phase extraction-gas chromatography and solid-phase extraction-gas chromatography-mass spectrometry determination of corrosion inhibiting long-chain primary alkyl amines in chemical treatment of boiler water in water-steam systems of power plants.

    PubMed

    Kusch, Peter; Knupp, Gerd; Hergarten, Marcus; Kozupa, Marian; Majchrzak, Maria

    2006-04-28

    Gas chromatography with simultaneous flame-ionization detection (FID) and a nitrogen-phosphorus detection (NPD) as well as gas chromatography-mass spectrometry (GC/MS) has been used to characterize long-chain primary alkyl amines after derivatization with trifluoroacetic anhydride (TFAA). Electron impact ionization- (EI) and negative chemical ionization (NCI) mass spectra of trifluoroacetylated derivatives of the identified tert-octadecylamines are presented for the first time. The corrosion inhibiting alkyl amines were applied in a water-steam circuit of energy systems in the power industry. Solid-phase extraction (SPE) with octadecyl bonded silica (C18) sorbents followed by gas chromatography were used for quantification of the investigated tert-octadecylamines in boiler water, superheated steam and condensate samples from the power plant. The estimated values were: 89 microg l(-1)(n = 5, RSD = 7.8%), 45 microg l(-1) (n = 5, RSD = 5.4%) and 37 microg l(-1)(n = 5, RSD = 2.3%), respectively. PMID:16483586

  11. Multifunctional electroactive electrospun nanofiber structures from water solution blends of PVA/ODA-MMT and poly(maleic acid-alt-acrylic acid): effects of Ag, organoclay, structural rearrangement and NaOH doping factors

    NASA Astrophysics Data System (ADS)

    Şimşek, Murat; Rzayev, Zakir M. O.; Bunyatova, Ulviya

    2016-06-01

    Novel multifunctional colloidal polymer nanofiber electrolytes were fabricated by green reactive electrospinning nanotechnology from various water solution/dispersed blends of poly (vinyl alcohol-co-vinyl acetate) (PVA)/octadecyl amine-montmorillonite (ODA-MMT) as matrix polymer nanocomposite and poly(maleic acid-alt-acrylic acid) (poly(MAc-alt-AA) and/or its Ag-carrying complex as partner copolymers. Polymer nanofiber electrolytes were characterized using FTIR, XRD, thermal (DSC, TGA-DTG), SEM, and electrical analysis methods. Effects of partner copolymers, organoclay, in situ generated silver nanoparticles (AgNPs), and annealing procedure on physical and chemical properties of polymer composite nanofibers were investigated. The electrical properties (resistance, conductivity, activation energy) of nanofibers with/without NaOH doping agent were also evaluated. This work presented a structural rearrangement of nanofiber mats by annealing via decarboxylation of anhydride units with the formation of new conjugated double bond sites onto partner copolymer main chains. It was also found that the semiconductor behaviors of nanofiber structures were essentially improved with increasing temperature and fraction of partner copolymers as well as presence of organoclay and AgNPs in nanofiber composite.

  12. Quantification of glycated N-terminal peptide of hemoglobin using derivatization for multiple functional groups of amino acids followed by liquid chromatography/tandem mass spectrometry.

    PubMed

    Sakaguchi, Yohei; Kinumi, Tomoya; Yamazaki, Taichi; Takatsu, Akiko

    2016-02-01

    A novel method of amino acid analysis using derivatization of multiple functional groups (amino, carboxyl, and phenolic hydroxyl groups) was applied to measure glycated amino acids in order to quantify glycated peptides and evaluate the degree of glycation of peptide. Amino and carboxyl groups of amino acids were derivatized with 1-bromobutane so that the hydrophobicities and basicities of the amino acids, including glycated amino acids, were improved. These derivatized amino acids could be detected with high sensitivity using LC-MS/MS. In this study, 1-deoxyfructosyl-VHLTPE and VHLTPE, which are N-terminal peptides of the β-chains of hemoglobin, were selected as target compounds. After reducing the peptide sample solution with sodium borohydride, the obtained peptides were hydrolyzed with hydrochloric acid. The released amino acids were then derivatized with 1-bromobutane and analyzed with LC-MS/MS. The derivatized amino acids, including glycated amino acids, could be separated using an octadecyl silylated silica column and good sharp peaks were detected. We show a confirmatory experiment that the proposed method can be applied to evaluate the degree of glycation of peptides, using mixtures of glycated and non-glycated peptide.

  13. Determination of anionic and nonionic surfactants, their degradation products, and endocrine-disrupting compounds in sewage sludge by liquid chromatography/mass spectrometry.

    PubMed

    Petrović, M; Barceló, D

    2000-10-01

    A comprehensive analytical method based on reversed-phase liquid chromatography and mass spectrometry using both atmospheric pressure chemical ionization and electrospray ionization has been developed for the simultaneous determination of anionic and nonionic surfactants, their polar degradation products, and endocrine-disrupting compounds (EDCs) in sewage sludge. Extraction of target compounds, with recovery rates from 86% to nearly 100% for polyethoxylates and from 84 to 94% for polar degradation products, was achieved applying ultrasonic solvent extraction with a mixture of methanol/ dichloromethane (7:3, v/v). Cleanup of sample extracts was performed on octadecyl solid-phase extraction cartridges. Determination of less polar compounds: alcohol ethoxylates (AEOs), nonylphenol ethoxylates (NPEOs), coconut diethanol amides, poly(ethylene glycol)s, and phthalate esters was accomplished by reversed-phase LC-APCI-MS in positive ionization mode, while more polar compounds: nonylphenolcarboxylates, nonylphenol (NP), octylphenol, and bisphenol Awere analyzed by ion-pair LC-ESI-MS under negative ionization conditions. This protocol was successfully applied to the trace determination of anionic and nonionic surfactants, polar degradation products, and EDCs in sewage sludge collected from different sewage treatment plants. The analysis revealed the presence of NP at high concentration levels ranging from 25 to 600 mg/kg. Polyethoxylates (AEOs and NPEOs) were also found in all samples at parts-per-million levels (10-190 mg/kg AEOs and 2-135 mg/kg NPEOs, respectively). PMID:11028611

  14. Detergent induction of HEK 293A cell membrane permeability measured under quiescent and superfusion conditions using whole cell patch clamp.

    PubMed

    Vaidyanathan, Sriram; Orr, Bradford G; Banaszak Holl, Mark M

    2014-02-27

    Detergents have several biological applications but present cytotoxicity concerns, since they can solubilize cell membranes. Using the IonFlux 16, an ensemble whole cell planar patch clamp, we observed that anionic sodium dodecyl sulfate (SDS), cationic cetyltrimethylammonium bromide (CTAB), and cationic, fluorescent octadecyl rhodamine B (ORB) increased the membrane permeability of cells substantially within a second of exposure, under superfusion conditions. Increased permeability was irreversible for 15 min. At subsolubilizing detergent concentrations, patched cells showed increased membrane currents that reached a steady state and were intact when imaged using fluorescence microscopy. SDS solubilized cells at concentrations of 2 mM (2× CMC), while CTAB did not solubilize cells even at concentrations of 10 mM (1000× CMC). The relative activity for plasma membrane current induction was 1:20:14 for SDS, CTAB, and ORB, respectively. Under quiescent conditions, the relative ratio of lipid to detergent in cell membranes at the onset of membrane permeability was 1:7:5 for SDS, CTAB, and ORB, respectively. The partition constants (K) for SDS, CTAB, and ORB were 23000, 55000, and 39000 M(-1), respectively. Combining the whole cell patch clamp data and XTT viability data, SDS ≤ 0.2 mM and CTAB and ORB ≤ 1 mM induced cell membrane permeability without causing acute toxicity.

  15. Time- and temperature-dependent migration studies of Irganox 1076 from plastics into foods and food simulants.

    PubMed

    Beldì, G; Pastorelli, S; Franchini, F; Simoneau, C

    2012-01-01

    The study provides an exhaustive set of migration data for octadecyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate (Irganox 1076) from low-density polyethylene (LDPE) in several food matrices. Irganox 1076 was used as a model migrant because it represents one of the typical substances used as an antioxidant in food packaging polymers. Kinetic (time-dependent) migration studies of Irganox 1076 were performed for selected foodstuffs chosen with different physical-chemical properties and in relation to the actual European food consumption market. The effect of fat content and of the temperature of storage on the migration from plastic packaging was evaluated. The results show that migration increased with fat content and storage temperature. All data obtained from real foods were also compared with data obtained from simulants tested in the same conditions. In all studied cases, the kinetics in simulants were higher than those in foodstuffs. The work provides data valuable for the extension of the validation of migration model developed on simulants to foodstuffs themselves. PMID:22313384

  16. Ultra-high ordered, centimeter scale preparation of microsphere Langmuir films.

    PubMed

    Kallepalli, L N Deepak; Constantinescu, C; Delaporte, P; Utéza, O; Grojo, D

    2015-05-15

    Controlling the preparation of nano/microsphere monolayers on large areas remains a difficult task but is crucial for several fabrication methods of highly-ordered periodic nanostructures. We demonstrate the preparation of ordered monolayers of few square centimeters with an extremely high coverage ratio (>98%) by implementing a modified protocol (MP) Langmuir Blodgett (LB) technique. We use octadecyl type hydrocarbon (C18) functionalized spherical particles (polystyrene and silica) with diameters in the range 1-5 μm, and a selected mixture of solvents for accurate control of the surface tension and particles' mobility at the water surface. This leads to a delicate growth of crystal-like monolayers which are subsequently transferred to glass or silicon substrates. While operating the Langmuir-Blodgett trough, a key enabling the quality enhancement resides not only on surface tension measurements but also on simple visual inspections of the water surface supporting the monolayer. The protocol yields a strong reduction of sensitivity to thermodynamical and mechanical disturbances leading to a robust method that could be automated by adding a feedback on the operated system based real-time image processing. A simple analytical approach is used to explain why this MP-LB technique is more appropriate in growing micrometric-sized objects in comparison to standard protocols optimized for the preparation of molecular films.

  17. Effect of EMA and antioxidants on properties of thermoplastic starch blown films

    NASA Astrophysics Data System (ADS)

    Threepopnatkul, P.; Kulsetthanchalee, C.; Sittattrakul, A.; Kaewjinda, E.

    2015-07-01

    The objectives of this study were to investigate the effect of poly(ethylene-co-methyl acrylate) (EMA) at 10, 30 and 50 wt% on the morphological properties, moisture sorption, water vapor permeability and biodegradability of thermoplastic starch (TPS). Urea and formamide were used as a mixed plasticizer. In addition, the effect of antioxidants namely, 3,5-di-tert-butyl-4-hydroxyhydrocinnamate (DTBH), butylated hydroxytoluene (BHT) and bis(octadecyl)hydroxylamine (BOH) at 1 wt% on the properties of TPS/EMA film was investigated. TPS/EMA films were produced by a blown film molding machine and characterized by scanning electron microscropy, moisture sorption, water vapor permeability and biodegradability measurement. Results found that the increment of EMA content in the TPS matrix could improve the water sorption, water vapor permeability and biodegradability properties of TPS/EMA films. For biodegradation, the weight loss of the blended films was directly proportional to TPS content. Regarding the antioxidants effect, the water vapor permeability of TPS/EMA films containing DTBH was higher than the one with BOH and BHT. However, the antioxidants contributed little to the biodegradability of TPS/EMA films and had no effect on the moisture sorption of TPS/EMA films.

  18. Synthesis and evaluation of an aromatic polymer-coated zirconia for reversed-phase liquid chromatography.

    PubMed

    Zhao, J; Carr, P W

    1999-11-15

    We synthesized a novel aromatic polymer-coated zirconia-based RPLC stationary phase by chemical adsorption of a copolymer of chloromethylstyrene and diethoxymethylvinylsilane onto zirconia (CMS/VMS-ZrO2). Characterization of the pore structure of the support by nitrogen porosimetry and inverse size-exclusion chromatography indicates that CMS/VMS-ZrO2 maintains the well-defined pore structure of the base material. Flow studies show that CMS/VMS-ZrO2 has good mass transfer characteristics. The reversed-phase retention characteristics of the new support are comparable to those of conventional silica-bonded phases. We have also evaluated the mechanical, thermal, and pH stability of CMS/VMS-ZrO2. The results show that CMS/VMS-ZrO2 is stable over a very wide range of pH (pH = 1-13) and at temperatures as high as 160 degrees C. Chromatographic separations of some low molecular weight aromatic analytes on CMS/VMS-ZrO2 and octadecyl-bonded silica phases indicate that there are some subtle but significant differences in the chromatographic selectivity of these two types of phases. PMID:10575967

  19. Mixed-mode sorption of hydroxylated atrazine degradation products to sell: A mechanism for bound residue

    USGS Publications Warehouse

    Lerch, R.N.; Thurman, E.M.; Kruger, E.L.

    1997-01-01

    This study tested the hypothesis that sorption of hydroxylated atrazine degradation products (HADPs: hydroxyatrazine, HA; deethylhydroxyatrazine, DEHA; and deisopropylhydroxyatrazine, DIHA) to soils occurs by mixed-mode binding resulting from two simultaneous mechanisms: (1) cation exchange and (2) hydrophobic interaction. The objective was to use liquid chromatography and soil extraction experiments to show that mixed-mode binding is the mechanism controlling HADP sorption to soils and is also a mechanism for bound residue. Overall, HADP binding to solid-phase extraction (SPE) sorbents occurred in the order: cation exchange >> octadecyl (C18) >> cyanopropyl. Binding to cation exchange SPE and to a high-performance liquid chromatograph octyl (C8) column showed evidence for mixed-mode binding. Comparison of soil extracted by 0.5 M KH2P04, pH 7.5, or 25% aqueous CH3CN showed that, for HA and DIHA, cation exchange was a more important binding mechanism to soils than hydrophobic interaction. Based on differences between several extractants, the extent of HADP mixed-mode binding to soil occurred in the following order: HA > DIHA > DEHA. Mixed-mode extraction recovered 42.8% of bound atrazine residues from aged soil, and 88% of this fraction was identified as HADPs. Thus, a significant portion of bound atrazine residues in soils is sorbed by the mixed-mode binding mechanisms.

  20. Studies on the compressibility of wax matrix granules of acetaminophen and their admixtures with various tableting bases.

    PubMed

    Uhumwangho, M U; Okor, R S

    2006-04-01

    Matrix granules of acetaminophen have been formed by a melt granulation process whereby the acetaminophen powder was triturated with the melted wax--goat wax, glyceryl monostearate or carnuba wax. The compressibility of the matrix granules and their admixture, with diluent granules (lactose, alpha-cellulose or microcrystalline cellulose) was investigated. The granules were compressed to tablets at a constant load (30 arbitrary units on the load scale) of a manesty single punch machine. Resulting tablets were evaluated for tensile strength (T) and disintegration times (DT). Granule flow was determined by measuring their angle of repose when allowed to fall freely on a level surface. Matrix granules prepared by melt granulation with goat wax or glyceryl monostearate were too sticky and therefore did not flow at all. They were also poorly compressible (T values = 0.20MN/m2). Inclusion of the diluent remarkably improved granule flow property and compressibility. The T values of the tablets (measure of compressibility) increased from about 0.24 to 0.65 MN/m2 during increase in diluent (lactose) content from 20 to 80 %w/w. Microcrystalline cellulose and alpha-cellulose were more effective than lactose in promoting compressibility of the granules. By contrast the matrix granules formed with carnuba wax were free flowing (angle of repose, 18.60). Addition of the diluent further improved flowability slightly. The matrix granules (without a diluent) were readily compressible (T value, 1.79MN/m2). Addition of the diluent (80%w/w) reduced T values (MN/m2) slightly to 1.32 (lactose), 1.48 (alpha-cellulose) and 1.74 (microcrystalline cellulose). Tablets of the matrix granules only, disintegrated rapidly within 3 minutes. DT was further reduced to <30 s by addition of any of the diluents. The indication is that the inclusion of the diluents studied can be used to improve the compressibility of the otherwise poorly compressible matrix granules. Based on the flowability

  1. Archaea mediate anaerobic oxidation of methane in deep euxinic waters of the Black Sea

    NASA Astrophysics Data System (ADS)

    Wakeham, Stuart G.; Lewis, Cynthia M.; Hopmans, Ellen C.; Schouten, Stefan; Sinninghe Damsté, Jaap S.

    2003-04-01

    We evaluate anaerobic oxidation of methane (AOM) in the Black Sea water column by determining distributions of archaea-specific glyceryl dialkyl glyceryl tetraethers (GDGTs) and 13C isotopic compositions of their constituent biphytanes in suspended particulate matter (SPM), sinking particulate matter collected in sediment traps, and surface sediments. We also determined isotopic compositions of fatty acids specific to sulfate-reducing bacteria to test for biomarker and isotopic evidence of a syntrophic relationship between archaea and sulfate-reducing bacteria in carrying out AOM. Bicyclic and tricyclic GDGTs and their constituent 13C-depleted monocyclic and bicyclic biphytanes (down to -67‰) indicative of archaea involved in AOM were present in SPM in the anoxic zone below 700 m depth. In contrast, GDGT-0 and crenarchaeol derived from planktonic crenarchaeota dominated the GDGT distributions in the oxic surface and shallow anoxic waters. Fatty acids indicative of sulfate-reducing bacteria (i.e., iso- and anteiso-C 15) were not strongly isotopically depleted (e.g., -32 to -25‰), although anteiso-C 15 was 5‰ more depleted in 13C than iso-C 15. Our results suggest that either AOM is carried out by archaea independent of sulfate-reducing bacteria or those sulfate-reducing bacteria involved in a syntrophy with methane-oxidizing archaea constitute a small enough fraction of the total sulfate-reducing bacterial community that an isotope depletion in their fatty acids is not readily detected. Sinking particulate material collected in sediment traps and the underlying sediments in the anoxic zone contained the biomarker and isotope signature of upper-water column archaea. AOM-specific GDGTs and 13C-depleted biphytanes characteristic of the SPM in the deep anoxic zone are not incorporated into sinking particles and are not efficiently transported to the sediments. This observation suggests that sediments may not always record AOM in overlying euxinic water columns and

  2. Studies on the compressibility of wax matrix granules of acetaminophen and their admixtures with various tableting bases.

    PubMed

    Uhumwangho, M U; Okor, R S

    2006-04-01

    Matrix granules of acetaminophen have been formed by a melt granulation process whereby the acetaminophen powder was triturated with the melted wax--goat wax, glyceryl monostearate or carnuba wax. The compressibility of the matrix granules and their admixture, with diluent granules (lactose, alpha-cellulose or microcrystalline cellulose) was investigated. The granules were compressed to tablets at a constant load (30 arbitrary units on the load scale) of a manesty single punch machine. Resulting tablets were evaluated for tensile strength (T) and disintegration times (DT). Granule flow was determined by measuring their angle of repose when allowed to fall freely on a level surface. Matrix granules prepared by melt granulation with goat wax or glyceryl monostearate were too sticky and therefore did not flow at all. They were also poorly compressible (T values = 0.20MN/m2). Inclusion of the diluent remarkably improved granule flow property and compressibility. The T values of the tablets (measure of compressibility) increased from about 0.24 to 0.65 MN/m2 during increase in diluent (lactose) content from 20 to 80 %w/w. Microcrystalline cellulose and alpha-cellulose were more effective than lactose in promoting compressibility of the granules. By contrast the matrix granules formed with carnuba wax were free flowing (angle of repose, 18.60). Addition of the diluent further improved flowability slightly. The matrix granules (without a diluent) were readily compressible (T value, 1.79MN/m2). Addition of the diluent (80%w/w) reduced T values (MN/m2) slightly to 1.32 (lactose), 1.48 (alpha-cellulose) and 1.74 (microcrystalline cellulose). Tablets of the matrix granules only, disintegrated rapidly within 3 minutes. DT was further reduced to <30 s by addition of any of the diluents. The indication is that the inclusion of the diluents studied can be used to improve the compressibility of the otherwise poorly compressible matrix granules. Based on the flowability

  3. Multi-proxy geochemical analyses of Indus Submarine Fan sediments sampled by IODP Expedition 355: implications for sediment provenance and palaeoclimate reconstructions

    NASA Astrophysics Data System (ADS)

    Bratenkov, Sophia; George, Simon C.; Bendle, James; Liddy, Hannah; Clift, Peter D.; Pandey, Dhananjai K.; Kulhanek, Denise K.; Andò, Sergio; Tiwari, Manish; Khim, Boo-Keun; Griffith, Elizabeth; Steinke, Stephan; Suzuki, Kenta; Lee, Jongmin; Newton, Kate; Tripathi, Shubham; Expedition 355 Scientific Party

    2016-04-01

    petrography and heavy mineral analysis, geochemical data, isotope composition, and biomarker analysis. Preliminary organic geochemistry data suggest an increase of terrigenous organic matter input into sediment starting around 10.5 Ma, with a strong decrease in the last 1 Ma. Moreover, the detailed analyses of the glyceryl dialkyl glyceryl tetraether (GDGT) and alkenone lipids provide the first sea surface temperature (SST) reconstructions in the region. These data indicate decreasing SST from the Middle Miocene Climatic Optimum until today. This research provides an exceptional opportunity to apply a multiproxy approach to understand sediment provenance, erosional processes, and palaeoclimate evolution in the eastern Arabian Sea.

  4. Preparation and evaluation of a self-nanoemulsifying drug delivery system loaded with Akebia saponin D–phospholipid complex

    PubMed Central

    Shen, Jinyang; Bi, Jianping; Tian, Hongli; Jin, Ye; Wang, Yuan; Yang, Xiaolin; Yang, Zhonglin; Kou, Junping; Li, Fei

    2016-01-01

    Background Akebia saponin D (ASD) exerts various pharmacological activities but with poor oral bioavailability. In this study, a self-nanoemulsifying drug delivery system (SNEDDS) based on the drug–phospholipid complex technique was developed to improve the oral absorption of ASD. Methods ASD–phospholipid complex (APC) was prepared using a solvent-evaporation method and characterized by infrared spectroscopy, differential scanning calorimetry, morphology observation, and solubility test. Oil and cosurfactant were selected according to their ability to dissolve APC, while surfactant was chosen based on its emulsification efficiency in SNEDDS. Pseudoternary phase diagrams were constructed to determine the optimized APC-SNEDDS formulation, which was characterized by droplet size determination, zeta potential determination, and morphology observation. Robustness to dilution and thermodynamic stability of optimized formulation were also evaluated. Subsequently, pharmacokinetic parameters and oral bioavailability of ASD, APC, and APC-SNEDDS were investigated in rats. Results The liposolubility significantly increased 11.4-fold after formation of APC, which was verified by the solubility test in n-octanol. Peceol (Glyceryl monooleate [type 40]), Cremophor® EL (Polyoxyl 35 castor oil), and Transcutol HP (Diethylene glycol monoethyl ether) were selected as oil, surfactant, and cosurfactant, respectively. The optimal formulation was composed of Glyceryl monooleate (type 40), Polyoxyl 35 castor oil, Diethylene glycol monoethyl ether, and APC (1:4.5:4.5:1.74, w/w/w/w), which showed a particle size of 148.0±2.7 nm and a zeta potential of −13.7±0.92 mV after dilution with distilled water at a ratio of 1:100 (w/w) and good colloidal stability. Pharmacokinetic studies showed that APC-SNEDDS exhibited a significantly greater Cmax1 (733.4±203.8 ng/mL) than ASD (437.2±174.2 ng/mL), and a greater Cmax2 (985.8±366.6 ng/mL) than ASD (180.5±75.1 ng/mL) and APC (549.7±113

  5. Formulation and in vitro release evaluation of newly synthesized palm kernel oil esters-based nanoemulsion delivery system for 30% ethanolic dried extract derived from local Phyllanthus urinaria for skin antiaging

    PubMed Central

    Mahdi, Elrashid Saleh; Noor, Azmin Mohd; Sakeena, Mohamed Hameem; Abdullah, Ghassan Z; Abdulkarim, Muthanna F; Sattar, Munavvar Abdul

    2011-01-01

    Background Recently there has been a remarkable surge of interest about natural products and their applications in the cosmetic industry. Topical delivery of antioxidants from natural sources is one of the approaches used to reverse signs of skin aging. The aim of this research was to develop a nanoemulsion cream for topical delivery of 30% ethanolic extract derived from local Phyllanthus urinaria (P. urinaria) for skin antiaging. Methods Palm kernel oil esters (PKOEs)-based nanoemulsions were loaded with P. urinaria extract using a spontaneous method and characterized with respect to particle size, zeta potential, and rheological properties. The release profile of the extract was evaluated using in vitro Franz diffusion cells from an artificial membrane and the antioxidant activity of the extract released was evaluated using the 2, 2-diphenyl-1-picrylhydrazyl (DPPH) method. Results Formulation F12 consisted of wt/wt, 0.05% P. urinaria extract, 1% cetyl alcohol, 0.5% glyceryl monostearate, 12% PKOEs, and 27% Tween® 80/Span® 80 (9/1) with a hydrophilic lipophilic balance of 13.9, and a 59.5% phosphate buffer system at pH 7.4. Formulation F36 was comprised of 0.05% P. urinaria extract, 1% cetyl alcohol, 1% glyceryl monostearate, 14% PKOEs, 28% Tween® 80/Span® 80 (9/1) with a hydrophilic lipophilic balance of 13.9, and 56% phosphate buffer system at pH 7.4 with shear thinning and thixotropy. The droplet size of F12 and F36 was 30.74 nm and 35.71 nm, respectively, and their nanosizes were confirmed by transmission electron microscopy images. Thereafter, 51.30% and 51.02% of the loaded extract was released from F12 and F36 through an artificial cellulose membrane, scavenging 29.89% and 30.05% of DPPH radical activity, respectively. Conclusion The P. urinaria extract was successfully incorporated into a PKOEs-based nanoemulsion delivery system. In vitro release of the extract from the formulations showed DPPH radical scavenging activity. These formulations can

  6. Lipids and the malarial parasite*

    PubMed Central

    Holz, George G.

    1977-01-01

    Merozoite endocytosis initiates Plasmodium development in a vacuole bounded by an erythrocyte-derived membrane, whose asymmetrical distribution of lipids and proteins is reversed in its orientation with respect to the parasite plasma membrane. Reorientation may accompany the proliferation of the membrane associated with the parasite's growth and phagocytic and pinocytic feeding. Increases in the membrane surface area of the parasite, and in some cases of the erythrocyte, parallel parasite growth and segmentation. Augmentation of all the membrane systems of the infected erythrocyte causes the lipid content to rise rapidly, but the parasite lipid composition differs from that of the erythrocyte in many respects: it is higher in diacyl phosphatidylethanolamine, phosphatidylinositol, polyglycerol phosphatides, diacylglycerols, unesterified fatty acids, triacylglycerols, and hexadecanoic and octadecenoic fatty acids and lower in sphingomyelin, phosphatidylserine, alkoxy phosphatidylethanolamine, cholesterol, and polyunsaturated fatty acids. Active lipid metabolism accompanies the membrane proliferation associated with feeding, growth, and reproduction. Plasmodium is incapable of de novo biosynthesis of fatty acids and cholesterol; however, it can fabricate its glycerides and phosphoglycerides with host-supplied fatty acids, nitrogenous bases, alcohols, ATP, and coenzyme A, and can generate the glyceryl moiety during glycolysis. Cholesterol is obtained from the host but nothing is known of sphingolipid origins. Lipid metabolism of the parasite may be associated with alterations in the amounts of octadecenoic fatty acids and cholesterol in the erythrocyte plasma membrane, which in turn are responsible for changes in permeability and fragility. PMID:412602

  7. Development of cationic solid lipid nanoparticles with factorial design-based studies for topical administration of doxorubicin.

    PubMed

    Taveira, Stephânia F; Araújo, Luciana M P de Campos; de Santana, Danielle C A S; Nomizo, Auro; de Freitas, Luiz Alexandre P; Lopez, Renata F V

    2012-04-01

    Topical chemotherapy using doxorubicin, a powerful anticancer drug, can be used as an alternative with reduced systemic toxicity when treating skin cancer. The aim of the present work was to use factorial design-based studies to develop cationic solid lipid nanoparticles containing doxorubicin; further investigations into the influence of these particles on the drug's cytotoxicity and cellular uptake in B16F10 murine melanoma cells were performed. A 32 full factorial design was applied for two different lipid phases; one phase used stearic acid and the other used a 1:2 mixture of stearic acid and glyceryl behenate. The two factors investigated included the ratio between the lipid and the water phase and the ratio between the surfactant (poloxamer) and the co-surfactant (cetylpyridinium chloride). It was observed that the studied factors did not affect the mean diameter or the polydispersity of the obtained nanoparticles; however, they did significantly affect the zeta potential values. Optimised formulations with particle sizes ranging from 251 to 306 nm and positive zeta potentials were selected for doxorubicin incorporation. High entrapment efficiencies were achieved (97%) in formulations with higher amounts of stearic acid, suggesting that cationic charges on doxorubicin molecules may interact with the negative charges in stearic acid. Melanoma culture cell experiments showed that cationic solid lipid nanoparticles without drug were not cytotoxic to melanoma cells. The encapsulation of doxorubicin significantly increased cytotoxicity, indicating the potential of these nanoparticles for the treatment of skin cancer.

  8. Unexpected skin barrier influence from nonionic emulsifiers.

    PubMed

    Bárány, E; Lindberg, M; Lodén, M

    2000-02-15

    Skin disorders are often treated with creams containing various active substances. The creams also contain emulsifiers, which are surface-active ingredients used to stabilize the emulsion. Emulsifiers are potential irritants and in the present study the influence of stearic acid, glyceryl stearate, PEG-2, -9, -40, and -100 stearate, steareth-2, -10 and -21 on normal as well as on irritated skin have been evaluated with non-invasive measurements. Test emulsions were created by incorporating 5% emulsifiers in a water/mineral oil mixture (50:50). The emulsions and their vehicle were then applied to normal skin for 48 h and to sodium lauryl sulfate (SLS) damaged skin for 17 h in aluminum chambers. Twenty-four hours after removal of the chambers the test sites were evaluated for degree of irritation. In normal skin, the emulsifiers induced significant differences in TEWL but not in skin blood flow. Five of the emulsifiers increased TEWL. In SLS-damaged skin an aggravation of the irritation was expected. However, no differences regarding skin blood flow was noted from the emulsifiers. Furthermore, three emulsifiers unexpectedly decreased TEWL. These results highlight the possibility of absorption of these emulsifiers into the lipid bilayer, which increase TEWL in normal skin and decrease TEWL in damaged skin.

  9. Defensive Armor of Potato Tubers: Nonpolar Metabolite Profiling, Antioxidant Assessment, and Solid-State NMR Compositional Analysis of Suberin-Enriched Wound-Healing Tissues.

    PubMed

    Dastmalchi, Keyvan; Kallash, Linda; Wang, Isabel; Phan, Van C; Huang, Wenlin; Serra, Olga; Stark, Ruth E

    2015-08-01

    The cultivation, storage, and distribution of potato tubers are compromised by mechanical damage and suboptimal healing. To investigate wound-healing progress in cultivars with contrasting russeting patterns, metabolite profiles reported previously for polar tissue extracts were complemented by GC/MS measurements for nonpolar extracts and quantitative (13)C NMR of interfacial solid suspensions. Potential marker compounds that distinguish cultivar type and wound-healing time point included fatty acids, fatty alcohols, alkanes, glyceryl esters, α,ω-fatty diacids, and hydroxyfatty acids. The abundant long-chain fatty acids in nonpolar extracts and solids from the smooth-skinned Yukon Gold cultivar suggested extensive suberin biopolymer formation; this hypothesis was supported by high proportions of arenes, alkenes, and carbonyl groups in the solid and among the polar markers. The absence of many potential marker classes in nonpolar Atlantic extracts and interfacial solids suggested a limited extent of suberization. Modest scavenging activities of all nonpolar extracts indicate that the majority of antioxidants produced in response to wounding are polar.

  10. Lipid nanoparticles based on butyl-methoxydibenzoylmethane: in vitro UVA blocking effect.

    PubMed

    Niculae, G; Lacatusu, I; Badea, N; Meghea, A

    2012-08-10

    The aim of the present study was to obtain efficient lipid nanoparticles loaded with butyl-methoxydibenzoylmethane (BMDBM) in order to develop cosmetic formulations with enhanced UVA blocking effect. For this purpose, two adequate liquid lipids (medium chain triglycerides and squalene) have been used in combination with two solid lipids (cetyl palmitate and glyceryl stearate) in order to create appropriate nanostructured carriers with a disordered lipid network able to accommodate up to 1.5% BMDBM. The lipid nanoparticles (LNs) were characterized in terms of particle size, zeta potential, entrapment efficiency, loading capacity and in vitro UVA blocking effect. The efficiency of lipid nanoparticles in developing some cosmetic formulations has been evaluated by determining the in vitro erythemal UVA protection factor. In order to quantify the photoprotective effect, some selected cream formulations based on BMDBM-LNs and a conventional emulsion were exposed to photochemical UV irradiation at a low energy to simulate the solar energy during the midday. The results obtained demonstrated the high ability of cream formulations based on BMDBM-LNs to absorb more than 96% of UVA radiation. Moreover, the developed cosmetic formulations manifest an enhanced UVA blocking effect, the erythemal UVA protection factor being four times higher than those specific to conventional emulsions.

  11. A monolithic lipase reactor for biodiesel production by transesterification of triacylglycerides into fatty acid methyl esters

    PubMed Central

    Urban, Jiri; Svec, Frantisek; Fréchet, Jean M.J.

    2011-01-01

    An enzymatic reactor with lipase immobilized on a monolithic polymer support has been prepared and used to catalyze the transesterification of triacylglycerides into the fatty acid methyl esters commonly used for biodiesel. A design of experiments procedure was used to optimize the monolithic reactor with variables including control of the surface polarity of the monolith via variations in the length of the hydrocarbon chain in alkyl methacrylate monomer, time of grafting of 1-vinyl-4,4-dimethylazlactone used to activate the monolith, and time used for the immobilization of porcine lipase. Optimal conditions involved the use of a poly(stearyl methacrylate-co-ethylene dimethacrylate) monolith, grafted first with vinylazlactone, then treated with lipase for 2 h to carry out the immobilization of the enzyme. Best conditions for the transesterification of glyceryl tributyrate included a temperature of 37°C and a 10 min residence time of the substrate in the bioreactor. The reactor did not lose its activity even after pumping through it a solution of substrate equaling 1,000 reactor volumes. This enzymatic reactor was also used for the transesterification of triacylglycerides from soybean oil to fatty acid methyl esters thus demonstrating the ability of the reactor to produce biodiesel. PMID:21915852

  12. Vascular system: role of nitric oxide in cardiovascular diseases.

    PubMed

    Bian, Ka; Doursout, Marie-Françoise; Murad, Ferid

    2008-04-01

    In contrast with the short research history of the enzymatic synthesis of nitric oxide (NO), the introduction of nitrate-containing compounds for medicinal purposes marked its 150th anniversary in 1997. Glyceryl trinitrate (nitroglycerin) is the first compound of this category. On October 12, 1998, the Nobel Assembly awarded the Nobel Prize in Medicine or Physiology to scientists Robert Furchgott, Louis Ignarro, and Ferid Murad for their discoveries concerning NO as a signaling molecule in the cardiovascular system. NO-mediated signaling is a recognized component in various physiologic processes (eg, smooth muscle relaxation, inhibition of platelet and leukocyte aggregation, attenuation of vascular smooth muscle cell proliferation, neurotransmission, and immune defense), to name only a few. NO has also been implicated in the pathology of many inflammatory diseases, including arthritis, myocarditis, colitis, and nephritis and a large number of pathologic conditions such as amyotrophic lateral sclerosis, cancer, diabetes, and neurodegenerative diseases. Some of these processes (eg, smooth muscle relaxation, platelet aggregation, and neurotransmission) require only a brief production of NO at low nanomolar concentrations and are dependent on the recruitment of cyclic guanosine monophosphate (cGMP)-dependent signaling. Other processes are associated with direct interaction of NO or reactive nitrogen species derived from it with target proteins and requires a more sustained production of NO at higher concentrations but do not involve the cGMP pathway.

  13. Nitric oxide (NO)--biogeneration, regulation, and relevance to human diseases.

    PubMed

    Bian, Ka; Murad, Ferid

    2003-01-01

    On October 12, 1998, the Nobel Assembly awarded the Nobel Prize in Medicine and Physiology to scientists Robert Furchgott, Louis Ignarro, and Ferid Murad for their discoveries concerning nitric oxide as a signalling molecule in the cardiovascular system. In contrast with the short research history of the enzymatic synthesis of NO, the introduction of nitrate-containing compounds for medicinal purposes marked its 150th anniversary in 1997. Glyceryl trinitrate (nitroglycerin; GTN) is the first compound of this category. Alfred Nobel (the founder of Nobel Prize) himself had suffered from angina pectoris and was prescribed nitroglycerin for his chest pain. Almost a century later, research in the NO field has dramatically extended and the role of NO in physiology and pathology has been extensively studied. The steady-state concentration and the biological effects of NO are critically determined not only by its rate of formation, but also by its rate of decomposition. Biotransformation of NO and its related N-oxides occurs via different metabolic routes within the body and presents another attractive field for our research as well as for the venture of drug discovery.

  14. Patellar Tendinopathy

    PubMed Central

    Schwartz, Aaron; Watson, Jonathan N.; Hutchinson, Mark R.

    2015-01-01

    Context: Patellar tendinopathy is a common condition. There are a wide variety of treatment options available, the majority of which are nonoperative. No consensus exists on the optimal method of treatment. Evidence Acquisition: PubMed spanning 1962-2014. Study Design: Clinical review. Level of Evidence: Level 4. Results: The majority of cases resolve with nonoperative therapy: rest, physical therapy with eccentric exercises, cryotherapy, anti-inflammatories, corticosteroid injections, extracorporeal shockwave therapy, glyceryl trinitrate, platelet-rich plasma injections, and ultrasound-guided sclerosis. Refractory cases may require either open or arthroscopic debridement of the patellar tendon. Corticosteroid injections provide short-term pain relief but increase risk of tendon rupture. Anti-inflammatories and injectable agents have shown mixed results. Surgical treatment is effective in many refractory cases unresponsive to nonoperative modalities. Conclusion: Physical therapy with an eccentric exercise program is the mainstay of treatment for patellar tendinopathy. Platelet-rich plasma has demonstrated mixed results; evidence-based recommendations on its efficacy cannot be made. In the event that nonoperative treatment fails, surgical intervention has produced good to excellent outcomes in the majority of patients. PMID:26502416

  15. Intraoral film containing insulin-phospholipid microemulsion: formulation and in vivo hypoglycemic activity study.

    PubMed

    Rachmawati, Heni; Haryadi, Bernard Manuel; Anggadiredja, Kusnandar; Suendo, Veinardi

    2015-06-01

    Non-invasive administration of insulin is expected for better diabetes mellitus therapy. In this report, we developed intraoral preparation for insulin. Insulin was encapsulated into nanocarrier using self-assembly emulsification process. To increase lipophilicity of insulin, it was dispersed in phospholipid resulted in insulin-phospholipid solid dispersion. The microemulsion formula was established from our previous work which contained glyceryl monooleate (GMO), Tween 20, and polyethylene glycol (PEG 400) in a ratio of 1:8:1. To confirm the formation of insulin-phospholipid solid dispersion, PXRD, FTIR spectroscopy, and Raman spectroscopy were performed. Then, the microemulsion was evaluated for droplet size and distribution, zeta potential, entrapment efficiency, physical stability, and Raman spectroscopy. In addition, microemulsion with expected characteristic was evaluated for in vitro release, in vitro permeation, and in vivo activity. The droplets size of ∼100 nm with narrow distribution and positive charge of +0.56 mV were formed. The insulin encapsulated in the oil droplet was accounted of >90%. Water-soluble chitosan seems to be a promising film matrix polymer which also functioned as insulin release controller. Oral administration of insulin microemulsion to healthy Swiss-Webster mice showed hypoglycemic effect indicating the success of this protein against a harsh environment of the gastrointestinal tract. This effectiveness significantly increased by fourfold as compared to free insulin. Taken together, microemulsion seems to be a promising carrier for oral delivery of insulin.

  16. Paclitaxel loaded PEGylated gleceryl monooleate based nanoparticulate carriers in chemotherapy.

    PubMed

    Jain, Vikas; Swarnakar, Nitin K; Mishra, Prabhat R; Verma, Ashwni; Kaul, Ankur; Mishra, Anil K; Jain, Narendra K

    2012-10-01

    A PEGylated drug delivery system of paclitaxel (PTX), based on glyceryl monooleate (GMO) was prepared by optimizing various parameters to explore its potential in anticancer therapy. The prepared system was characterized through polarized light microscopy, TEM, AFM and SAXS to reveal its liquid crystalline nature. As GMO based LCNPs exhibit high hemolytic toxicity and faster release of entrapped drug (66.2 ± 2.5% in 24 h), PEGylation strategy was utilized to increase the hemocompatibility (reduction in hemolysis from 60.3 ± 10.2 to 4.4 ± 1.3%) and control the release of PTX (43.6 ± 3.2% released in 24 h). The cytotoxic potential and cellular uptake was assessed in MCF-7 cell lines. Further, biodistribution studies were carried out in EAT (Ehrlich Ascites tumor) bearing mice using (99m)Tc-(Technetium radionuclide) labeled formulations and an enhanced circulation time and tumor accumulation (14 and 8 times, respectively) were observed with PEGylated carriers over plain ones, at 24 h. Finally, tumor growth inhibition experiment was performed and after 15 days, control group exhibited 15 times enhancement in tumor volume, while plain and PEGylated systems exhibited only 8 and 4 times enhancement, respectively, as compared to initial tumor volume. The results suggest that PEGylation enhances the hemocompatibility and efficacy of GMO based system that may serve as an efficient i.v. delivery vehicle for paclitaxel.

  17. A novel in situ gel for sustained drug delivery and targeting.

    PubMed

    Ganguly, Sudipta; Dash, Alekha K

    2004-05-19

    The objective of this study was to develop a novel chitosan-glyceryl monooleate (GMO) in situ gel system for sustained drug delivery and targeting. The delivery system consisted of 3% (w/v) chitosan and 3% (w/v) GMO in 0.33M citric acid. In situ gel was formed at a biological pH. In vitro release studies were conducted in Sorensen's phosphate buffer (pH 7.4) and drugs were analyzed either by HPLC or spectrophotometry. Characterization of the gel included the effect of cross-linker, determination of diffusion coefficient and water uptake by thermogravimetric analysis (TGA). Mucoadhesive property of the gel was evaluated in vitro using an EZ-Tester. Incorporation of a cross-linker (glutaraldehyde) retarded the rate and extent of drug release. The in vitro release can further be sustained by replacing the free drug with drug-encapsulated microspheres. Drug release from the gel followed a matrix diffusion controlled mechanism. Inclusion of GMO enhanced the mucoadhesive property of chitosan by three- to sevenfold. This novel in situ gel system can be useful in the sustained delivery of drugs via oral as well as parenteral routes.

  18. A potential carrier based on liquid crystal nanoparticles for ophthalmic delivery of pilocarpine nitrate.

    PubMed

    Li, Jing; Wu, Lin; Wu, Weijun; Wang, Baoyan; Wang, Zhongyuan; Xin, Hongliang; Xu, Qunwei

    2013-10-15

    Poor corneal penetration and short preocular retention of a clinical hydrophilic drug, pilocarpine nitrate (PN), for the treatment of open-angle glaucoma and acute angle-closure glaucoma, limit its ocular application. The purpose of this study was to investigate the potential of liquid crystal nanoparticles (LCNPs) for ocular delivery of PN. LCNPs were developed by a top-down method using glyceryl monoolein (GMO) and water in the presence of stabilizer Poloxamer 407. They were characterized by transmission electron microscopy (TEM) and small angle X-ray diffraction (SAXS). The size of LCNP is 202.28±19.32 nm and the encapsulation efficiency reached 61.03%. The in vitro release profiles indicated that PN could keep sustained release from PN-loaded LCNPs for 8h. An ex vivo corneal permeation study revealed that the apparent permeability coefficient of PN-loaded LCNPs was 2.05-fold higher than that of commercial eye drops. In addition, the topical administration test showed that PN-loaded LCNPs had a prolonged effect on decreasing intraocular pressure (IOP) of rabbits compared with commercial drug and physiological saline. In conclusion, LCNPs had been demonstrated to be potential for controlled-release ocular drug delivery.

  19. Adsorption of nonlamellar nanostructured liquid-crystalline particles to biorelevant surfaces for improved delivery of bioactive compounds.

    PubMed

    Dong, Yao-Da; Larson, Ian; Barnes, Timothy J; Prestidge, Clive A; Boyd, Ben J

    2011-05-01

    The adsorption of nanostructured lyotropic liquid-crystal particles, cubosomes and hexosomes, at surfaces was investigated for potential use in surface-specific agrochemical delivery. Adsorption of phytantriol (PHYT) and glyceryl monooleate (GMO)-based cubosomes and hexosomes, stabilized using Pluronic F127, at tristearin-coated (model leaf surface) and uncoated zinc selenide surfaces was studied using attenuated total reflectance Fourier transform IR (ATR-FTIR) spectroscopy, by quantifying the IR absorbance due to the lipid components of the particles over time. The delivery of an encapsulated hydrophobic model herbicide [dichlorodiphenyldichloroethylene (DDE)] was also examined on the model and real leaf surfaces. The adsorption behavior of the particles by ATR-FTIR was dependent on the internal nanostructure and lipid composition, with PHYT cubosomes adsorbing more avidly at tristearin surfaces than GMO-based cubosomes or hexosomes. There was a direct correlation between DDE associated with the surfaces and the particle adsorption observed in the ATR-FTIR study, strongly implicating particle adsorption with the delivery efficiency. Differences between the mode of interaction of the Pluronic stabilizer with the different lipids and particle nanostructures were proposed to lead to differences in the particle adsorption behavior.

  20. Transdermal baicalin delivery using diethylene glycol monoethyl ether-mediated cubic phase gel.

    PubMed

    Zhang, Yongtai; Zhang, Kai; Guo, Teng; Li, Yuan; Zhu, Chunyun; Feng, Nianping

    2015-02-01

    This study investigated the transdermal permeability of baicalin, a hydrophobic and readily hydrolyzed drug, delivered by glyceryl monooleate (GMO)-based cubic phase gel (CPG) mediated with Transcotol(®) P (TP, diethylene glycol monoethyl ether). A range of CPGs was produced by varying GMO, water, and TP levels. Examination of their physicochemical properties revealed that the optically isotropic CPG showed higher viscosity than lamellar phase gels (LPG), and the baicalin cargo increased CPG viscosity. The GMO:TP ratio and water content also altered viscosity. CPG-mediated delivery increased baicalin's skin permeation, with 76.65- to 200.24-fold higher (p<0.05) transdermal flux than that of a Carbopol(®)-based hydrogel (HDG), and 6.72- to 17.55-fold (p<0.05) higher than that of LPG, with the same water content. Rat in vivo microdialysis showed that CPG produced sustained baicalin release, with superior pharmacokinetic parameters to those of HDG. Furthermore, cutaneous drug absorption was more efficient on rat abdominal skin, compared to that in the chest or scapular region. Effective fusion between the CPG lipid matrix and the stratum corneum may explain this enhancement of transdermal permeation. CPG containing TP therefore, achieved excellent transdermal drug delivery and good baicalin stability, indicating that this system represents a promising transdermal delivery vehicle.

  1. A rheological and microstructural characterisation of bigels for cosmetic and pharmaceutical uses.

    PubMed

    Lupi, Francesca R; Shakeel, Ahmad; Greco, Valeria; Oliviero Rossi, Cesare; Baldino, Noemi; Gabriele, Domenico

    2016-12-01

    Bigels are biphasic systems formed by water-based hydrogels and oil-based organogels, mainly studied, in the last few years, for pharmaceutical and cosmetic application focused on the controlled delivery of both lipophilic and hydrophilic active agents. The rheological properties of bigels depend on both the amount and the rheological characteristics of single structured phases. Moreover, it can be expected that, at large fractions of one of the starting gels, systems more complex than oil-in-water or water-in-oil can be obtained, yielding bicontinuous or matrix-in-matrix arrangement. Model bigels were investigated from a microstructural (i.e. microscopy and electrical conductivity tests) and rheological point of view. The hydrogel was prepared by using a low-methoxyl pectin whereas the organogel was prepared by using olive oil and, as gelator, a mixture of glyceryl stearate and policosanol. Model bigels were obtained by increasing the amount of organogel mixed with the hydrogel, and microstructural characterisation evidenced an organogel-in-hydrogel behaviour for all investigated samples, even though at the highest organogel content a more complex structure seems to arise. A semi-empirical model, based on theoretical equations developed for suspensions of elastic spheres in elastic media, was proposed to relate bigel rheological properties to single phase properties and fractions. PMID:27612723

  2. EPR investigation of gamma irradiated single crystal guaifenesin: A combined experimental and computational study

    NASA Astrophysics Data System (ADS)

    Tasdemir, Halil Ugur; Sayin, Ulku; Türkkan, Ercan; Ozmen, Ayhan

    2016-04-01

    Gamma irradiated single crystal of Guaifenesin (Glyceryl Guaiacolate), an important expectorant drug, were investigated with Electron Paramagnetic Resonance (EPR) spectroscopy between 123 and 333 K temperature at different orientations in the magnetic field. Considering the chemical structure and the experimental spectra of the gamma irradiated single crystal of guaifenesin sample, we assumed that alkoxy or alkyl-type paramagnetic species may be produced by irradiation. Depending on this assumption, eight possible alkoxy and alkyl-type radicals were modeled and EPR parameters of these modeled radicals were calculated using the B3LYP/6-311++G(d,p)-level of density functional theory (DFT). Theoretically calculated values of alkyl-type modeled radical(R3) are in good agreement with experimentally determined EPR parameters of single crystal. Furthermore, simulation spectra which are obtained by using the theoretical initial values are well matched with the experimental spectra. It was determined that a stable Cα •H2αCβHβCγH2γ (R3) alkyl radical was produced in the host crystal as a result of gamma irradiation.

  3. Integration of chemical catalysis with extractive fermentation to produce fuels.

    PubMed

    Anbarasan, Pazhamalai; Baer, Zachary C; Sreekumar, Sanil; Gross, Elad; Binder, Joseph B; Blanch, Harvey W; Clark, Douglas S; Toste, F Dean

    2012-11-01

    Nearly one hundred years ago, the fermentative production of acetone by Clostridium acetobutylicum provided a crucial alternative source of this solvent for manufacture of the explosive cordite. Today there is a resurgence of interest in solventogenic Clostridium species to produce n-butanol and ethanol for use as renewable alternative transportation fuels. Acetone, a product of acetone-n-butanol-ethanol (ABE) fermentation, harbours a nucleophilic α-carbon, which is amenable to C-C bond formation with the electrophilic alcohols produced in ABE fermentation. This functionality can be used to form higher-molecular-mass hydrocarbons similar to those found in current jet and diesel fuels. Here we describe the integration of biological and chemocatalytic routes to convert ABE fermentation products efficiently into ketones by a palladium-catalysed alkylation. Tuning of the reaction conditions permits the production of either petrol or jet and diesel precursors. Glyceryl tributyrate was used for the in situ selective extraction of both acetone and alcohols to enable the simple integration of ABE fermentation and chemical catalysis, while reducing the energy demand of the overall process. This process provides a means to selectively produce petrol, jet and diesel blend stocks from lignocellulosic and cane sugars at yields near their theoretical maxima.

  4. Organic composition of aerosol particulate matter during a haze episode in Kuala Lumpur, Malaysia

    NASA Astrophysics Data System (ADS)

    Radzi Bin Abas, M.; Rahman, Noorsaadah A.; Omar, Nasr Yousef M. J.; Maah, M. Jamil; Abu Samah, Azizan; Oros, Daniel R.; Otto, Angelika; Simoneit, Bernd R. T.

    The solvent-extractable compounds of urban airborne particulate matter were analyzed to determine the distributions of homologous and biomarker tracers. Samples were collected by high-volume air filtration during the haze episode of 1997 around the University of Malaya campus near Petaling Jaya, a suburb of Kuala Lumpur, Malaysia. These results show that the samples contain n-alkanes, n-alkan-2-ones, n-alkanols, methyl n-alkanoates, n-alkyl nitriles, n-alkanals, n-alkanoic acids, levoglucosan, PAHs, and UCM as the dominant components, with minor amounts of terpenoids, glyceryl esters and sterols, all derived from natural biogenic sources (vascular plant wax), from burning of biomass, and from anthropogenic utilization of fossil fuel products (lubricating oil, vehicle emissions, etc.). Some compositional differences are observed in the samples and greater atmospheric concentrations were found for almost all organic components in the samples collected near a roadway. The results interpreted in terms of major sources are due to local build-up of organic contaminants from vehicular emissions, smoke from biomass burning, and natural background as a result of the atmospheric stability during the haze episodes. The organic components transported in from areas outside the region, assuming all smoke components are external to the city, amount to about 30% of the total organic particle burden.

  5. Long-term sustained-released in situ gels of a water-insoluble drug amphotericin B for mycotic arthritis intra-articular administration: preparation, in vitro and in vivo evaluation.

    PubMed

    Shan-Bin, Guo; Yue, Tian; Ling-Yan, Jian

    2015-04-01

    Amphotericin B (AMB) was often used in intra-articular injection administration for fungal arthritis, because it could often bring a satisfactory therapeutic efficacy and a minimum systemic toxic side effect. However, because of the multiple operations and the frequent injections, the compliance of the patients was bad. Therefore, to develop a long-term sustained-released preparation of AMB for mycotic arthritis intra-articular administration is of great significance. The purpose of present study was to develop a long-term sustained-released in situ gel of a water-insoluble drug AMB for mycotic arthritis intra-articular administration. Based on the evaluations of the in vitro properties of the formulations, the formulation containing 10% (w/w) ethanol, 15% (w/w) PG, 0.75% (w/w) HA, 5% (w/w) purified soybean oil, 0.03% (w/w) α-tocopherol, 15% (w/w) water and 55% (w/w) glyceryl monooleate was selected as a suitable intra-articular injectable in situ gel drug delivery system for water-insoluble drug AMB. Furthermore, the results of the in vivo study on rabbits showed that the selected formulation was a safe and effective long-term sustained-released intra-articular injectable AMB preparation. Therefore, the presented in situ AMB gel could reduce the frequency of the administration in the AMB treatment of fungal arthritis, and then would get a good patient compliance. PMID:24502270

  6. Improvement of enalapril maleate chemical stability by high shear melting granulation.

    PubMed

    de Oliveira, Ana Paula Montandon; Cunha, Talita Amorim; Serpa, Raphael Caixeta; Taveira, Stephânia Fleury; Lima, Eliana Martins; Almeida Diniz, Danielle Guimarães; de Freitas, Luis Alexandre Pedro; Marreto, Ricardo Neves

    2014-09-18

    Abstract Enalapril maleate is a widely used drug, which is chemically unstable when mixed with excipients resulting in enalaprilat and diketopiperazine as the main degradation products. The preparation of enalapril sodium salt has been used to improve drug stability in solid dosage forms; however, product rejection is observed when the chemical reaction for obtaining the sodium salt is not completely finished before packaging. In this study, granules were prepared by melting granulation using stearic acid or glyceryl monostearate, with a view to developing more stable enalapril maleate solid dosage forms. The granules were prepared in a laboratory-scale high shear mixer and compressed in a rotary machine. Size distribution, flow properties, in vitro drug release and enalapril maleate chemical stability were evaluated and compared with data obtained from tablets prepared without hydrophobic binders. All formulations showed good physical properties and immediate drug release. The greatest improvement in the enalapril maleate stability was observed in formulations containing stearic acid. This study showed that hot melting granulation could be successfully used to prepare enalapril maleate granules which could substitute the in situ formation of enalapril sodium salt, since they provided better enalapril stability in solid dosage forms. PMID:25231642

  7. Curcuminoids-loaded lipid nanoparticles: novel approach towards malaria treatment.

    PubMed

    Nayak, Aditya P; Tiyaboonchai, Waree; Patankar, Swati; Madhusudhan, Basavaraj; Souto, Eliana B

    2010-11-01

    In the present work, curcuminoids-loaded lipid nanoparticles for parenteral administration were successfully prepared by a nanoemulsion technique employing high-speed homogenizer and ultrasonic probe. For the production of nanoparticles, trimyristin, tristerin and glyceryl monostearate were selected as solid lipids and medium chain triglyceride (MCT) as liquid lipid. Scanning electron microscopy (SEM) revealed the spherical nature of the particles with sizes ranging between 120 and 250 nm measured by photon correlation spectroscopy (PCS). The zeta potential of the particles ranged between -28 and -45 mV depending on the nature of the lipid matrix produced, which also influenced the entrapment efficiency (EE) and drug loading capacity (LC) found to be in the range of 80-94% and 1.62-3.27%, respectively. The LC increased reciprocally on increasing the amount of MCT as confirmed by differential scanning calorimetry (DSC). DSC analyses revealed that increasing imperfections within the lipid matrix allowed for increasing encapsulation parameters. Nanoparticles were further sterilized by filtration process which was found to be superior over autoclaving in preventing thermal degradation of thermo-sensitive curcuminoids. The in vivo pharmacodynamic activity revealed 2-fold increase in antimalarial activity of curcuminoids entrapped in lipid nanoparticles when compared to free curcuminoids at the tested dosage level.

  8. Calculation of optimum emulsifier mixtures for phase inversion emulsification*.

    PubMed

    Förster, T; Rybinski, W V; Tesmann, H; Wadle, A

    1994-04-01

    Synopsis The phase inversion emulsification is a convenient method of preparing fine-disperse and long-term stable oil-in-water emulsions, which are stabilized with nonionic emulsifiers. On the basis of EACN-values (equivalent alkane carbon numbers) the calculation of phase inversion in concentrates (CAPICO) is possible, which yields emulsifier and oil mixing ratios corresponding to a given phase inversion temperature (PIT). The CAPICO-method is illustrated for the example of a cosmetic oil-in-water lotion containing an oil mixture, glyceryl monostearate and a fatty alcohol ethoxylate. Of special interest is the influence of silicone oils on the PIT. At a constant emulsifier oil ratio the complete phase behaviour of this emulsion system is represented in a temperature/water content graph. Optimum emulsification results are obtained if during PIT emulsification a microemulsion or a lamellar phase is passed. The emulsions were characterized by particle sizing, and emulsion stability against sedimentation was evaluated by ultrasonic velocity changes. A fine-disperse and long-term stable oil-in-water emulsion was prepared by a time and energy-saving two-step hot-cold process.

  9. Hyperbranched polyglycerol-based lipids via oxyanionic polymerization: toward multifunctional stealth liposomes.

    PubMed

    Hofmann, Anna Maria; Wurm, Frederik; Hühn, Eva; Nawroth, Thomas; Langguth, Peter; Frey, Holger

    2010-03-01

    We describe the synthesis of linear-hyperbranched lipids for liposome preparation based on linear poly(ethylene glycol) (PEG) and hyperbranched polyglycerol (PG). Molecular weights were adjusted to values around 3000 g/mol with varying degrees of polymerization of the linear and the branched segments in analogy to PEG-based stealth lipids; polydispersities were generally low and below 1.3. The hydrophobic anchors were introduced into the lipid structures as initiators for the anionic polymerization of ethylene oxide and are either based on cholesterol or on different aliphatic glyceryl ethers. Complete incorporation of the apolar initiators was evidenced by MALDI-ToF analysis at all stages of the reaction. The linear-hyperbranched polyether lipid is incorporated as the polyfunctional shell in liposome formulations together with 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC). The resulting liposomes were subsequently characterized via dynamic light scattering (DLS) and small angle neutron scattering (SANS) as well as transmission electron microscopy (TEM), demonstrating the formation of unilamellar liposomes in the size range of 40 to 50 nm. PMID:20121134

  10. Optimization of matrix tablets controlled drug release using Elman dynamic neural networks and decision trees.

    PubMed

    Petrović, Jelena; Ibrić, Svetlana; Betz, Gabriele; Đurić, Zorica

    2012-05-30

    The main objective of the study was to develop artificial intelligence methods for optimization of drug release from matrix tablets regardless of the matrix type. Static and dynamic artificial neural networks of the same topology were developed to model dissolution profiles of different matrix tablets types (hydrophilic/lipid) using formulation composition, compression force used for tableting and tablets porosity and tensile strength as input data. Potential application of decision trees in discovering knowledge from experimental data was also investigated. Polyethylene oxide polymer and glyceryl palmitostearate were used as matrix forming materials for hydrophilic and lipid matrix tablets, respectively whereas selected model drugs were diclofenac sodium and caffeine. Matrix tablets were prepared by direct compression method and tested for in vitro dissolution profiles. Optimization of static and dynamic neural networks used for modeling of drug release was performed using Monte Carlo simulations or genetic algorithms optimizer. Decision trees were constructed following discretization of data. Calculated difference (f(1)) and similarity (f(2)) factors for predicted and experimentally obtained dissolution profiles of test matrix tablets formulations indicate that Elman dynamic neural networks as well as decision trees are capable of accurate predictions of both hydrophilic and lipid matrix tablets dissolution profiles. Elman neural networks were compared to most frequently used static network, Multi-layered perceptron, and superiority of Elman networks have been demonstrated. Developed methods allow simple, yet very precise way of drug release predictions for both hydrophilic and lipid matrix tablets having controlled drug release.

  11. Process and formulation variables in the preparation of wax microparticles by a melt dispersion technique. I. Oil-in-water technique for water-insoluble drugs.

    PubMed

    Bodmeier, R; Wang, J; Bhagwatwar, H

    1992-01-01

    Ibuprofen-wax (carnauba, paraffin, beeswax, and the semisynthetic glyceryl esters--Gelucire 64/02 and Precirol ATO5) microparticles were prepared without organic solvents as an alternative to polymeric microparticles. In the melt dispersion technique, the drug-wax melt was emulsified into a heated aqueous phase followed by cooling to form the microparticles. The microparticles were characterized with respect to their drug loading, and morphological and release properties. They were spherical and non-agglomerated and drug loading close to 60 per cent were achieved. The more hydrophilic waxes (Gelucire 64/02 or Precirol ATO5) could be prepared without the use of surfactants. With the other waxes, increasing amounts of sodium lauryl sulphate in the external aqueous phase decreased the drug loading because of drug solubilization when compared to the polymeric stabilizer, poly(vinyl alcohol). The type of wax, the rate of cooling, and the temperature of the aqueous phase had no significant effect on the drug loading because of the low solubility of the drug in the external aqueous phase. The drug release was controlled by the hydrophobicity of the wax. Besides ibuprofen, other water-soluble drugs (ketoprofen, indomethacin, hydrocortisone) were also encapsulated by this method. The wax microparticles could be formulated into an aqueous sustained-release oral suspension dosage form. PMID:1613647

  12. Wax-incorporated emulsion gel beads of calcium pectinate for intragastric floating drug delivery.

    PubMed

    Sriamornsak, Pornsak; Asavapichayont, Panida; Nunthanid, Jurairat; Luangtana-Anan, Manee; Limmatvapirat, Sontaya; Piriyaprasarth, Suchada

    2008-01-01

    The purpose of this study was to prepare wax-incorporated pectin-based emulsion gel beads using a modified emulsion-gelation method. The waxes in pectin-olive oil mixtures containing a model drug, metronidazole, were hot-melted, homogenized and then extruded into calcium chloride solution. The beads formed were separated, washed with distilled water and dried for 12 h. The influence of various types and amounts of wax on floating and drug release behavior of emulsion gel beads of calcium pectinate was investigated. The drug-loaded gel beads were found to float on simulated gastric fluid if the sufficient amount of oil was used. Incorporation of wax into the emulsion gel beads affected the drug release. Water-soluble wax (i.e. polyethylene glycol) increased the drug release while other water-insoluble waxes (i.e. glyceryl monostearate, stearyl alcohol, carnauba wax, spermaceti wax and white wax) significantly retarded the drug release. Different waxes had a slight effect on the drug release. However, the increased amount of incorporated wax in the formulations significantly sustained the drug release while the beads remained floating. The results suggest that wax-incorporated emulsion gel beads could be used as a carrier for intragastric floating drug delivery. PMID:18459055

  13. Preparation and physicochemical properties of surfactant-free emulsions using electrolytic-reduction ion water containing lithium magnesium sodium silicate.

    PubMed

    Okajima, Masahiro; Wada, Yuko; Hosoya, Takashi; Hino, Fumio; Kitahara, Yoshiyasu; Shimokawa, Ken-ichi; Ishii, Fumiyoshi

    2013-04-01

    Surfactant-free emulsions by adding jojoba oil, squalane, olive oil, or glyceryl trioctanoate (medium chain fatty acid triglycerides, MCT) to electrolytic-reduction ion water containing lithium magnesium sodium silicate (GE-100) were prepared, and their physiochemical properties (thixotropy, zeta potential, and mean particle diameter) were evaluated. At an oil concentration of 10%, the zeta potential was ‒22.3 ‒ ‒26.8 mV, showing no marked differences among the emulsions of various types of oil, but the mean particle diameters in the olive oil emulsion (327 nm) and MCT emulsion (295 nm) were smaller than those in the other oil emulsions (452-471 nm). In addition, measurement of the hysteresis loop area of each type of emulsion revealed extremely high thixotropy of the emulsion containing MCT at a low concentration and the olive emulsion. Based on these results, since surfactants and antiseptic agents markedly damage sensitive skin tissue such as that with atopic dermatitis, surfactant- and antiseptic-free emulsions are expected to be new bases for drugs for external use. PMID:23715508

  14. Physicopharmaceutical characteristics of an oil-in-water emulsion-type ointment containing diclofenac sodium.

    PubMed

    Takamura, A; Ishii, F; Noro, S; Koishi, M

    1984-05-01

    The oil-in-water (o/w) emulsion-type ointment was prepared with food additives containing diclofenac sodium. The oil phase and the emulsifier used were 1,2,3- propanetriyl trioctanoate (caprylic acid glyceryl ester) and sugar wax, and sugar ester, respectively. The emulsion stability of the o/w emulsion-type ointment as well as the diclofenac sodium release profile were investigated and compared with those from conventional ointments. The emulsion stability was evaluated in terms of the viscosity of the emulsion product, the particle size distribution of oil droplets, and the zeta potential of the droplets. It was found that sugar esters have excellent properties as emulsifiers, based on the results of viscosity and zeta potential measurements. The in vitro release test revealed that the amount of diclofenac sodium released from o/w emulsion-type ointment was greater than from the hydrophilic and absorptive ointment. Accordingly, it was concluded that o/w emulsion-type bases are suitable for pharmaceutical use in ointment products. PMID:6737243

  15. Development and Evaluation of Taste Masked Granular Formulation of Satranidazole by Melt Granulation Technique

    PubMed Central

    Pawar, Harshal Ashok; Joshi, Pooja Rasiklal

    2014-01-01

    Drugs from nitroimidazole category are generally bitter in taste. Oral formulation with bitter taste is not palatable. Geriatrics and pediatrics patients usually suffer from swallowing difficulties. Many other patients in some disease conditions avoid swallowing tablets. Satranidazole is a new nitro-imidazole derivative with bitter taste and is available in market as film coated tablet. The purpose of this research was to mask the bitter taste of Satranidazole by coating complexation with low melting point wax and Eudragit EPO. Different types of wax (glyceryl monostearate, stearic acid and cetyl alcohol) were tried for taste masking. The drug to stearic acid ratio 1 : 2 was found to be optimum on the basis of taste evaluation and in vitro release. The formulated granules were found to possess good flow property. FTIR studies confirmed that there was no interaction between drug and excipients. Scanning Electron Microscopy of drug and the optimized batch of granules was performed. The in vitro release of drug from granules was compared with marketed tablet formulation. The taste masked granules of optimized batch showed 87.65% release of drug in 1 hr which is comparable to that of marketed tablet formulation. PMID:26556200

  16. Tolterodine Tartrate Proniosomal Gel Transdermal Delivery for Overactive Bladder

    PubMed Central

    Rajabalaya, Rajan; Leen, Guok; Chellian, Jestin; Chakravarthi, Srikumar; David, Sheba R.

    2016-01-01

    The goal of this study was to formulate and evaluate side effects of transdermal delivery of proniosomal gel compared to oral tolterodine tartrate (TT) for the treatment of overactive bladder (OAB). Proniosomal gels are surfactants, lipids and soy lecithin, prepared by coacervation phase separation. Formulations were analyzed for drug entrapment efficiency (EE), vesicle size, surface morphology, attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, in vitro skin permeation, and in vivo effects. The EE was 44.87%–91.68% and vesicle size was 253–845 nm for Span formulations and morphology showed a loose structure. The stability and skin irritancy test were also carried out for the optimized formulations. Span formulations with cholesterol-containing formulation S1 and glyceryl distearate as well as lecithin containing S3 formulation showed higher cumulative percent of permeation such as 42% and 35%, respectively. In the in vivo salivary secretion model, S1 proniosomal gel had faster recovery, less cholinergic side effect on the salivary gland compared with that of oral TT. Histologically, bladder of rats treated with the proniosomal gel formulation S1 showed morphological improvements greater than those treated with S3. This study demonstrates the potential of proniosomal vesicles for transdermal delivery of TT to treat OAB. PMID:27589789

  17. Extension of the LOPLS-AA Force Field for Alcohols, Esters, and Monoolein Bilayers and its Validation by Neutron Scattering Experiments.

    PubMed

    Pluhackova, Kristyna; Morhenn, Humphrey; Lautner, Lisa; Lohstroh, Wiebke; Nemkovski, Kirill S; Unruh, Tobias; Böckmann, Rainer A

    2015-12-10

    The recently presented LOPLS-AA all-atom force field for long hydrocarbon chains, based on the OPLS-AA force field, was extended to alcohols, esters, and glyceryl monooleate (GMO) lipids as a model lipid. Dihedral angles were fitted against high level ab initio calculations, and ester charges were increased to improve their hydration properties. Additionally, the ester Lennard-Jones parameters were readjusted to reproduce experimental liquid bulk properties, densities, and heats of vaporization. This extension enabled the setup of LOPLS-AA parameters for GMO molecules. The properties of the lipid force field were tested for the liquid-crystalline phase of a GMO bilayer. The obtained area per lipid for GMO is in good agreement with experiment. Additionally, the lipid dynamics on the subpicosecond to the nanosecond time scale is in excellent agreement with results from time-of-flight (TOF) quasielastic neutron scattering (QENS) experiments on a multilamellar monoolein system, enabling here for the first time the critical evaluation of the short-time dynamics obtained from a molecular dynamics simulation of a membrane system. PMID:26537654

  18. Production of hybrid lipid-based particles loaded with inorganic nanoparticles and active compounds for prolonged topical release.

    PubMed

    García-González, C A; Sampaio da Sousa, A R; Argemí, A; López Periago, A; Saurina, J; Duarte, C M M; Domingo, C

    2009-12-01

    The production of particulate hybrid carriers containing a glyceryl monostearate (Lumulse GMS-K), a waxy triglyceride (Cutina HR), silanized TiO(2) and caffeine were investigated with the aim of producing sunscreens with UV-radiation protection properties. Particles were obtained using the supercritical PGSS (Particles from Gas Saturated Solutions) technique. This method takes advantages of the lower melting temperatures of the lipids obtained from the dissolution of CO(2) in the bulk mixture. Experiments were performed at 13 MPa and 345 K, according to previous melting point measurements. Blends containing Lumulse GMS-K and Cutina HR lipids (50 wt%) were loaded with silanized TiO(2) and caffeine in percentile proportions of 6 and 4 wt%, respectively. The particles produced were characterized using several analytical techniques as follows: system crystallinity was checked by X-ray diffraction and differential scanning calorimetry, thermal stability by thermogravimetric analysis, and morphology by scanning and transmission electron microscopy. Further, the UV-shielding ability of TiO(2) after its dispersion in the lipidic matrix was assessed by solid UV-vis spectroscopy. Preliminary results indicated that caffeine-loaded solid lipid particles presented a two-step dissolution profile, with an initial burst of 60 wt% of the loaded active agent. Lipid blends loaded with TiO(2) and caffeine encompassed the UV-filter behavior of TiO(2) and the photoaging prevention properties of caffeine.

  19. A rheological and microstructural characterisation of bigels for cosmetic and pharmaceutical uses.

    PubMed

    Lupi, Francesca R; Shakeel, Ahmad; Greco, Valeria; Oliviero Rossi, Cesare; Baldino, Noemi; Gabriele, Domenico

    2016-12-01

    Bigels are biphasic systems formed by water-based hydrogels and oil-based organogels, mainly studied, in the last few years, for pharmaceutical and cosmetic application focused on the controlled delivery of both lipophilic and hydrophilic active agents. The rheological properties of bigels depend on both the amount and the rheological characteristics of single structured phases. Moreover, it can be expected that, at large fractions of one of the starting gels, systems more complex than oil-in-water or water-in-oil can be obtained, yielding bicontinuous or matrix-in-matrix arrangement. Model bigels were investigated from a microstructural (i.e. microscopy and electrical conductivity tests) and rheological point of view. The hydrogel was prepared by using a low-methoxyl pectin whereas the organogel was prepared by using olive oil and, as gelator, a mixture of glyceryl stearate and policosanol. Model bigels were obtained by increasing the amount of organogel mixed with the hydrogel, and microstructural characterisation evidenced an organogel-in-hydrogel behaviour for all investigated samples, even though at the highest organogel content a more complex structure seems to arise. A semi-empirical model, based on theoretical equations developed for suspensions of elastic spheres in elastic media, was proposed to relate bigel rheological properties to single phase properties and fractions.

  20. Effects of some lubricants and evaluation of compression parameters on directly compressible powders.

    PubMed

    Uğurlu, Timuçin; Halaçoğlu, Mekin Doğa

    2014-05-01

    The objective of this study was to investigate the effects of conventional lubricants including a new candidate lubricant "Hexagonal boron nitride (HBN)" on direct compression powders. Lubricants such as magnesium stearate, glyceryl behenate, stearic acid, talc and polyethylene glycol6000 were studied in this article. Tablets were manufactured on an instrumented tablet press with various lubricant concentrations. Bulk and tapped densities, and Carr's index parameters were calculated for powders. Tensile strength, cohesion index, lower punch ejection force and lubricant effectiveness values were investigated for tablets. The deformation mechanisms of tablets were studied during compression from the Heckel plots with or without lubricants. Powders formulated with MGST and HBN showed better flow properties based on Carr's index. MGST was found to be the most effective lubricant based on lubricant effectiveness for tablets. HBN was found very close to MGST with the same concentrations. Other lubricants showed less effectiveness than that of MGST and HBN. It is observed that an increase in the concentration of HBN leads to decreased tensile strength and cohesion index values because of its surface-covering property. Despite covering property, HBN had no significant effect on disintegration time. Based on the Heckel plots at the level of 1%, HBN showed the most pronounced plastic character.

  1. A five-year study of cosmetic reactions.

    PubMed

    Adams, R M; Maibach, H I

    1985-12-01

    During 64 months (1977 to 1983), twelve dermatologists from various sections of the United States studied a total of 713 patients with cosmetic dermatitis out of an estimated total of 13,216 patients with contact dermatitis. The number of patients seen for all causes during this period was 281,100. An important finding was that half of the patients or physicians were unaware that a cosmetic was responsible for their dermatitis. Skin care products, hair preparations (including colors), and facial makeup were responsible for the majority of the reactions. The most important objective was identification of causative ingredients. Eighty-seven percent of the subjects had patch tests. Fragrance, preservatives (Quaternium-15, formaldehyde, imidazolidinyl urea, and parabens), p-phenylenediamine, and glyceryl monothioglycolate were the most frequently identified allergic sensitizers, in that order. In addition to the clinical data, the study permitted assessment of the frequency of cosmetic reactions, although the data may not be entirely representative of the country at large because of the special interests of the dermatologists involved.

  2. Encapsulation of Cancer Therapeutic Agent Dacarbazine Using Nanostructured Lipid Carrier.

    PubMed

    Almoussalam, Musallam; Zhu, Huijun

    2016-01-01

    The only formula of dacarbazine (Dac) in clinical use is intravenous infusion, presenting a poor therapeutic profile due to the low dispersity of the drug in aqueous solution. To overcome this, a nanostructured lipid carrier (NLC) consisting of glyceryl palmitostearate and isopropyl myristate was developed to encapsulate Dac. NLCs with controlled size were achieved using high shear dispersion (HSD) following solidification of oil-in-water emulsion. The synthesis parameters, including surfactant concentration, the speed and time of HSD were optimized to achieve the smallest NLC with size, polydispersion index and zeta potential of 155 ± 10 nm, 0.2 ± 0.01, and -43.4 ± 2 mV, respectively. The optimal parameters were also employed for Dac-loaded NLC preparation. The resultant NLC loaded with Dac possessed size, polydispersion index and zeta potential of 190 ± 10 nm, 0.2 ± 0.01, and -43.5 ± 1.2 mV, respectively. The drug encapsulation efficiency and drug loading reached 98% and 14%, respectively. This is the first report on encapsulation of Dac using NLC, implying that NLC could be a new potential candidate as drug carrier to improve the therapeutic profile of Dac. PMID:27168058

  3. Extension of the LOPLS-AA Force Field for Alcohols, Esters, and Monoolein Bilayers and its Validation by Neutron Scattering Experiments.

    PubMed

    Pluhackova, Kristyna; Morhenn, Humphrey; Lautner, Lisa; Lohstroh, Wiebke; Nemkovski, Kirill S; Unruh, Tobias; Böckmann, Rainer A

    2015-12-10

    The recently presented LOPLS-AA all-atom force field for long hydrocarbon chains, based on the OPLS-AA force field, was extended to alcohols, esters, and glyceryl monooleate (GMO) lipids as a model lipid. Dihedral angles were fitted against high level ab initio calculations, and ester charges were increased to improve their hydration properties. Additionally, the ester Lennard-Jones parameters were readjusted to reproduce experimental liquid bulk properties, densities, and heats of vaporization. This extension enabled the setup of LOPLS-AA parameters for GMO molecules. The properties of the lipid force field were tested for the liquid-crystalline phase of a GMO bilayer. The obtained area per lipid for GMO is in good agreement with experiment. Additionally, the lipid dynamics on the subpicosecond to the nanosecond time scale is in excellent agreement with results from time-of-flight (TOF) quasielastic neutron scattering (QENS) experiments on a multilamellar monoolein system, enabling here for the first time the critical evaluation of the short-time dynamics obtained from a molecular dynamics simulation of a membrane system.

  4. Physicopharmaceutical characteristics of an oil-in-water emulsion-type ointment containing diclofenac sodium.

    PubMed

    Takamura, A; Ishii, F; Noro, S; Koishi, M

    1984-05-01

    The oil-in-water (o/w) emulsion-type ointment was prepared with food additives containing diclofenac sodium. The oil phase and the emulsifier used were 1,2,3- propanetriyl trioctanoate (caprylic acid glyceryl ester) and sugar wax, and sugar ester, respectively. The emulsion stability of the o/w emulsion-type ointment as well as the diclofenac sodium release profile were investigated and compared with those from conventional ointments. The emulsion stability was evaluated in terms of the viscosity of the emulsion product, the particle size distribution of oil droplets, and the zeta potential of the droplets. It was found that sugar esters have excellent properties as emulsifiers, based on the results of viscosity and zeta potential measurements. The in vitro release test revealed that the amount of diclofenac sodium released from o/w emulsion-type ointment was greater than from the hydrophilic and absorptive ointment. Accordingly, it was concluded that o/w emulsion-type bases are suitable for pharmaceutical use in ointment products.

  5. Wax-incorporated emulsion gel beads of calcium pectinate for intragastric floating drug delivery.

    PubMed

    Sriamornsak, Pornsak; Asavapichayont, Panida; Nunthanid, Jurairat; Luangtana-Anan, Manee; Limmatvapirat, Sontaya; Piriyaprasarth, Suchada

    2008-01-01

    The purpose of this study was to prepare wax-incorporated pectin-based emulsion gel beads using a modified emulsion-gelation method. The waxes in pectin-olive oil mixtures containing a model drug, metronidazole, were hot-melted, homogenized and then extruded into calcium chloride solution. The beads formed were separated, washed with distilled water and dried for 12 h. The influence of various types and amounts of wax on floating and drug release behavior of emulsion gel beads of calcium pectinate was investigated. The drug-loaded gel beads were found to float on simulated gastric fluid if the sufficient amount of oil was used. Incorporation of wax into the emulsion gel beads affected the drug release. Water-soluble wax (i.e. polyethylene glycol) increased the drug release while other water-insoluble waxes (i.e. glyceryl monostearate, stearyl alcohol, carnauba wax, spermaceti wax and white wax) significantly retarded the drug release. Different waxes had a slight effect on the drug release. However, the increased amount of incorporated wax in the formulations significantly sustained the drug release while the beads remained floating. The results suggest that wax-incorporated emulsion gel beads could be used as a carrier for intragastric floating drug delivery.

  6. Influence of Surfactant and Lipid Type on the Physicochemical Properties and Biocompatibility of Solid Lipid Nanoparticles

    PubMed Central

    Pizzol, Carine Dal; Filippin-Monteiro, Fabíola Branco; Restrepo, Jelver Alexander Sierra; Pittella, Frederico; Silva, Adny Henrique; de Souza, Paula Alves; de Campos, Angela Machado; Creczynski-Pasa, Tânia Beatriz

    2014-01-01

    Nine types of solid lipid nanoparticle (SLN) formulations were produced using tripalmitin (TPM), glyceryl monostearate (GM) or stearic acid (SA), stabilized with lecithin S75 and polysorbate 80. Formulations were prepared presenting PI values within 0.25 to 0.30, and the physicochemical properties, stability upon storage and biocompatibility were evaluated. The average particle size ranged from 116 to 306 nm, with a negative surface charge around −11 mV. SLN presented good stability up to 60 days. The SLN manufactured using SA could not be measured by DLS due to the reflective feature of this formulation. However, TEM images revealed that SA nanoparticles presented square/rod shapes with an approximate size of 100 nm. Regarding biocompatibility aspects, SA nanoparticles showed toxicity in fibroblasts, causing cell death, and produced high hemolytic rates, indicating toxicity to red blood cells. This finding might be related to lipid type, as well as, the shape of the nanoparticles. No morphological alterations and hemolytic effects were observed in cells incubated with SLN containing TPM and GM. The SLN containing TPM and GM showed long-term stability, suggesting good shelf-life. The results indicate high toxicity of SLN prepared with SA, and strongly suggest that the components of the formulation should be analyzed in combination rather than separately to avoid misinterpretation of the results. PMID:25141003

  7. Preparation and physicochemical properties of surfactant-free emulsions using electrolytic-reduction ion water containing lithium magnesium sodium silicate.

    PubMed

    Okajima, Masahiro; Wada, Yuko; Hosoya, Takashi; Hino, Fumio; Kitahara, Yoshiyasu; Shimokawa, Ken-ichi; Ishii, Fumiyoshi

    2013-04-01

    Surfactant-free emulsions by adding jojoba oil, squalane, olive oil, or glyceryl trioctanoate (medium chain fatty acid triglycerides, MCT) to electrolytic-reduction ion water containing lithium magnesium sodium silicate (GE-100) were prepared, and their physiochemical properties (thixotropy, zeta potential, and mean particle diameter) were evaluated. At an oil concentration of 10%, the zeta potential was ‒22.3 ‒ ‒26.8 mV, showing no marked differences among the emulsions of various types of oil, but the mean particle diameters in the olive oil emulsion (327 nm) and MCT emulsion (295 nm) were smaller than those in the other oil emulsions (452-471 nm). In addition, measurement of the hysteresis loop area of each type of emulsion revealed extremely high thixotropy of the emulsion containing MCT at a low concentration and the olive emulsion. Based on these results, since surfactants and antiseptic agents markedly damage sensitive skin tissue such as that with atopic dermatitis, surfactant- and antiseptic-free emulsions are expected to be new bases for drugs for external use.

  8. Process and formulation variables in the preparation of wax microparticles by a melt dispersion technique. I. Oil-in-water technique for water-insoluble drugs.

    PubMed

    Bodmeier, R; Wang, J; Bhagwatwar, H

    1992-01-01

    Ibuprofen-wax (carnauba, paraffin, beeswax, and the semisynthetic glyceryl esters--Gelucire 64/02 and Precirol ATO5) microparticles were prepared without organic solvents as an alternative to polymeric microparticles. In the melt dispersion technique, the drug-wax melt was emulsified into a heated aqueous phase followed by cooling to form the microparticles. The microparticles were characterized with respect to their drug loading, and morphological and release properties. They were spherical and non-agglomerated and drug loading close to 60 per cent were achieved. The more hydrophilic waxes (Gelucire 64/02 or Precirol ATO5) could be prepared without the use of surfactants. With the other waxes, increasing amounts of sodium lauryl sulphate in the external aqueous phase decreased the drug loading because of drug solubilization when compared to the polymeric stabilizer, poly(vinyl alcohol). The type of wax, the rate of cooling, and the temperature of the aqueous phase had no significant effect on the drug loading because of the low solubility of the drug in the external aqueous phase. The drug release was controlled by the hydrophobicity of the wax. Besides ibuprofen, other water-soluble drugs (ketoprofen, indomethacin, hydrocortisone) were also encapsulated by this method. The wax microparticles could be formulated into an aqueous sustained-release oral suspension dosage form.

  9. Vitamin A loaded solid lipid nanoparticles for topical use: occlusive properties and drug targeting to the upper skin.

    PubMed

    Jenning, V; Gysler, A; Schäfer-Korting, M; Gohla, S H

    2000-05-01

    To evaluate the potential use of solid lipid nanoparticles (SLN) in dermatology and cosmetics, glyceryl behenate SLN loaded with vitamin A (retinol and retinyl palmitate) and incorporated in a hydrogel and o/w-cream were tested with respect to their influence on drug penetration into porcine skin. Conventional formulations served for comparison. Excised full thickness skin was mounted in Franz diffusion cells and the formulations were applied for 6 and 24 h, respectively. Vitamin A concentrations in the skin tissue suggested a certain drug localizing effect. High retinol concentrations were found in the upper skin layers following SLN preparations, whereas the deeper regions showed only very low vitamin A levels. Because of a polymorphic transition of the lipid carrier with subsequent drug expulsion following the application to the skin, the drug localizing action appears to be limited for 6-24 h. Best results were obtained with retinol SLN incorporated in the oil-in-water (o/w) cream retarding drug expulsion. The penetration of the occlusion sensitive drug retinyl palmitate was even more influenced by SLN incorporation. Transepidermal water loss (TEWL) and the influence of drug free SLN on retinyl palmitate uptake exclude pronounced occlusive effects. Therefore enhanced retinyl palmitate uptake should derive from specific SLN effects and is not due to non-specific occlusive properties.

  10. Development and characterization of novel hydrogel containing antimicrobial drug for treatment of burns

    PubMed Central

    Thakkar, Vaishali; Korat, Vaishali; Baldaniya, Lalji; Gohel, Mukesh; Gandhi, Tejal; Patel, Nirav

    2016-01-01

    Introduction: The aim of burn management and therapy is fast healing and epithelisation to prevent infection. The present study is concerned with the development and characterization of a novel nanaoparticulate system; cubosomes, loaded with silver sulfadiazine (SSD) and Aloe vera for topical treatment of infected burns. Methods: Cubosome dispersions were formulated by an emulsification technique using different concentrations of a lipid phase Glyceryl Monooleate (GMO) and Poloxamer 407. The optimum formulae were incorporated in an aloe vera gel containing carbopol 934, to form cubosomal hydrogels (cubogels). The cubogels were characterized by in vitro release of SSD, rheological properties, pH, bioadhesion, Transmission Electron Microscopy and in-vivo Wound Healing Study. Results: The results show that the different concentration of GMO had significant effect on particle size, % EE and in vitro drug release. From the in-vitro drug release pattern and similarity factor (f2), it was concluded that batch CG3 (15% GMO and 1% P407) exhibited complete and controlled drug release within 12 hour (i.e. 98.25%), better bio adhesion and superior burn healing as compared to the marketed product. Conclusion: The in vivo burns healing study in rats revealed that the prepared optimized cubogel containing SSD and aloe vera has superior burns healing rate than cubogel with only SSD and marketed preparation so, it may be successfully used in the treatment of deep second degree burn.

  11. Sensitivity analysis of near-infrared functional lymphatic imaging

    NASA Astrophysics Data System (ADS)

    Weiler, Michael; Kassis, Timothy; Dixon, J. Brandon

    2012-06-01

    Near-infrared imaging of lymphatic drainage of injected indocyanine green (ICG) has emerged as a new technology for clinical imaging of lymphatic architecture and quantification of vessel function, yet the imaging capabilities of this approach have yet to be quantitatively characterized. We seek to quantify its capabilities as a diagnostic tool for lymphatic disease. Imaging is performed in a tissue phantom for sensitivity analysis and in hairless rats for in vivo testing. To demonstrate the efficacy of this imaging approach to quantifying immediate functional changes in lymphatics, we investigate the effects of a topically applied nitric oxide (NO) donor glyceryl trinitrate ointment. Premixing ICG with albumin induces greater fluorescence intensity, with the ideal concentration being 150 μg/mL ICG and 60 g/L albumin. ICG fluorescence can be detected at a concentration of 150 μg/mL as deep as 6 mm with our system, but spatial resolution deteriorates below 3 mm, skewing measurements of vessel geometry. NO treatment slows lymphatic transport, which is reflected in increased transport time, reduced packet frequency, reduced packet velocity, and reduced effective contraction length. NIR imaging may be an alternative to invasive procedures measuring lymphatic function in vivo in real time.

  12. Non-Invasive Vagus Nerve Stimulation as Treatment for Trigeminal Allodynia

    PubMed Central

    Oshinsky, Michael L.; Murphy, Angela L.; Hekierski, Hugh; Cooper, Marnie; Simon, Bruce J.

    2014-01-01

    Implanted vagus nerve stimulation (VNS) has been used to treat seizures and depression. In this study, we explore the mechanism of action of non-invasive vagus nerve stimulation (nVNS) for the treatment of trigeminal allodynia. Rats were repeatedly infused with inflammatory mediators directly onto the dura, which leads to chronic trigeminal allodynia. nVNS for 2min decreases periorbital sensitivity in rats with periorbital trigeminal allodynia for up to 3.5hr after stimulation. Using microdialysis, we quantified levels of extracellular neurotransmitters in the trigeminal nucleus caudalis (TNC). Allodynic rats showed a 7.7±0.9 fold increase in extracellular glutamate in the TNC following i.p. administration of the chemical headache trigger, glyceryl trinitrate (GTN; 0.1mg/kg). Allodynic rats, which received nVNS, had only a 2.3±0.4 fold increase in extracellular glutamate following GTN similar to the response in control naive rats. When nVNS was delayed until 120min after GTN treatment, the high levels of glutamate in the TNC were reversed following nVNS. The nVNS stimulation parameters used in this study did not produce significant changes in blood pressure or heart rate. These data suggest that nVNS may be used to treat trigeminal allodynia. PMID:24530613

  13. Safranal-loaded solid lipid nanoparticles: evaluation of sunscreen and moisturizing potential for topical applications

    PubMed Central

    Khameneh, Bahman; Halimi, Vahid; Jaafari, Mahmoud Reza; Golmohammadzadeh, Shiva

    2015-01-01

    Objective(s): In the current study, sunscreen and moisturizing properties of solid lipid nanoparticle (SLN)-safranal formulations were evaluated. Materials and Methods: Series of SLN were prepared using glyceryl monostearate, Tween 80 and different amounts of safranal by high shear homogenization, and ultrasound and high-pressure homogenization (HPH) methods. SLN formulations were characterized for size, zeta potential, morphology, thermal properties, and encapsulation efficacy. The Sun Protection Factor (SPF) of the products was determined in vitro using transpore tape. The moisturizing activity of the products was also evaluated by corneometer. Results: The SPF of SLN-safranal formulations was increased when the amount of safranal increased. Mean particle size for all formulas was approximately 106 nm by probe sonication and 233 nm using HPH method. The encapsulation efficiency of safranal was around 70% for all SLN-safranal formulations. Conclusion: The results conclude that SLN-safranal formulations were found to be effective for topical delivery of safranal and succeeded in providing appropriate sunscreen properties. PMID:25810877

  14. Liquid crystalline phase as a probe for crystal engineering of lactose: carrier for pulmonary drug delivery.

    PubMed

    Patil, Sharvil S; Mahadik, Kakasaheb R; Paradkar, Anant R

    2015-02-20

    The current work was undertaken to assess suitability of liquid crystalline phase for engineering of lactose crystals and their utility as a carrier in dry powder inhalation formulations. Saturated lactose solution was poured in molten glyceryl monooleate which subsequently transformed into gel. The gel microstructure was analyzed by PPL microscopy and SAXS. Lactose particles recovered from gels after 48 h were analyzed for polymorphism using techniques such as FTIR, XRD, DSC and TGA. Particle size, morphology and aerosolisation properties of prepared lactose were analyzed using Anderson cascade impactor. In situ seeding followed by growth of lactose crystals took place in gels with cubic microstructure as revealed by PPL microscopy and SAXS. Elongated (size ∼ 71 μm) lactose particles with smooth surface containing mixture of α and β-lactose was recovered from gel, however percentage of α-lactose was more as compared to β-lactose. The aerosolisation parameters such as RD, ED, %FPF and % recovery of lactose recovered from gel (LPL) were found to be comparable to Respitose® ML001. Thus LC phase (cubic) can be used for engineering of lactose crystals so as to obtain particles with smooth surface, high elongation ratio and further they can be used as carrier in DPI formulations.

  15. Effect of side-chain structure of rigid polyimide dispersant on mechanical properties of single-walled carbon nanotube/cyanate ester composite.

    PubMed

    Yuan, Wei; Li, Weifeng; Mu, Yuguang; Chan-Park, Mary B

    2011-05-01

    Three kinds of polymer, polyimide without side-chain (PI), polyimide-graft-glyceryl 4-nonylphenyl ether (PI-GNE), and polyimide-graft-bisphenol A diglyceryl acrylate (PI-BDA), have been synthesized and used to disperse single-walled carbon nanotubes (SWNTs) and to improve the interfacial bonding between SWNTs and cyanate ester (CE) matrix. Visual observation, UV-vis-near-IR (UV-vis-NIR) spectra, and atomic force microscopy (AFM) images show that both PI-GNE and PI-BDA are highly effective at dispersing and debundling SWNTs in DMF, whereas PI is less effective. Interaction between SWNTs and PI, PI-GNE or PI-BDA was confirmed by computer simulation and Raman spectra. A series of CE-based composite films reinforced with different loadings of SWNTs, SWNTs/PI, SWNTs/PI-GNE and SWNTs/PI-BDA were prepared by solution casting. It was found that, because of the unique side-chain structure of PI-BDA, SWNTs/PI-BDA disperse better in CE matrix than do SWNTs/PI-GNE, SWNTs/PI, and SWNTs. As a result, SWNTs/PI-BDA/CE composites have the greatest improvement in mechanical properties of the materials tested. These results imply that the choice of side-chain on a dispersant is very important to the dispersion of SWNTs in matrix and the filler/matrix interfacial adhesion, which are two key requirements for achieving effective reinforcement. PMID:21526794

  16. Identification and specific blockade of two receptors for histamine in the cardiovascular system.

    PubMed

    Powell, J R; Brody, M J

    1976-01-01

    Histamine caused a fall in blood pressure in anesthetized dogs and cats which was only partially attenuated by mepyramine (pyrilamine), a histamine type H1-receptor antagonist. Further treatment with burimide or metiamide, type H2-receptor antagonists, caused nearly complete attenuation of the response to histamine. Burimamide alone had no effect on vasodilatation produced by histamine in the dog gracilis muscle whereas mepyramine alone caused a partial attenuation. An H2-receptor agonist, 4-methylhistamine and an H1-receptor agonist, 2-(2-pyridyl)ethylamine, both produced vasodilatation which was blocked by metiamide and mepyramine, respectively. Constriction of the saphenous vein produced by histamine was found to involve interaction with H1-receptors only. In the intact dog, histamine increased heart rate and decreased left ventricular dp/dt through direct effects. Mepyramine prevented the increase in heart rate but did not affect the chronotropic actions of isoproterenol and glyceryl trinitrate. H1-receptor blockade did not alter inotropic effects whereas subsequent H2-receptor blockade prevented the negative inotropic effect of histamine. It is concluded that both peripheral vascular and cardiac responses to histamine are mediated through activation of H1- and H2-histamine receptors.

  17. Clinical and therapeutic aspects of adrenoleukodystrophy and adrenomyeloneuropathy.

    PubMed

    Moser, H W

    1995-09-01

    Adrenoleukodystrophy (ALD) and its adult variant adrenomyeloneuropathy (AMN) are X-linked diseases in which a deficiency of lignoceroyl-CoA ligase, a peroxisomal enzyme needed for the degradation of very long chain fatty acids (VLCFA), has been reported. The responsible gene recently has been cloned; it codes for a peroxisomal membrane protein, ALDP, which is a member of the ABC (ATP binding cassette) transporter superfamily. Elevations in VLCFA, particularly C24 and C26, have proven useful in the diagnosis of the childhood, adolescent and adult cerebral forms and AMN. ALD and AMN commonly coexist in the same families; the same VLCFA elevations and gene mutations have been recognized in both ALD and AMN. This phenotypic heterogeneity suggests the influence of an autosomal modifier gene. Dietary manipulation using glyceryl trioleate-trieurucate oil (Lorenzo's oil) has been highly successful in lowering VLCFA, but not in affecting the rate of neurologic deterioration in symptomatic ALD boys or AMN adults. Dietary pretreatment of neurologically asymptomatic ALD patients may have some benefit and is advisable at the present time. Currently, we recommend bone marrow transplantation for those patients who show evidence of early cerebral involvement and for whom a well-matched donor is available. A drug therapy trial utilizing beta interferon and thalidomide is underway.

  18. Relationship between the size of nanoparticles and their adjuvant activity: Data from a study with an improved experimental design

    PubMed Central

    Li, Xinran; Sloat, Brian R.; Yanasarn, Nijaporn; Cui, Zhengrong

    2011-01-01

    There is a growing interest in identifying the relationship between the size of nanoparticles and their adjuvant activity, but the results from recent studies remain controversial. To address the controversy, it was thought that one should pay attention to the nanoparticle formulations to make sure that the antigen-loaded nanoparticles to be compared are not only different in particle size, but more importantly, as identical to each other as possible in all other formulation properties. In the present study, using ovalbumin (OVA) as a model antigen conjugated onto nanoparticles engineered from lecithin/glyceryl monostearate-in-water emulsions, we prepared OVA-nanoparticles of 230 nm and 708 nm. Before evaluating the immune responses induced by them in a mouse model, we made sure that: i) the sizes of the two OVA-nanoparticles did not extensively overlap, ii) the nanoparticles have similar zeta potentials and comparable antigen-loading, and iii) the nanoparticles did not aggregate when suspended in simulated biological media. We then showed that when subcutaneously injected into mice, the 230 nm OVA-conjugated nanoparticles induced stronger OVA-specific antibody and cellular immune responses than the 708 nm OVA-nanoparticles. Future studies attempting to correlate the size of nanoparticles and their adjuvant activities need to consider formulation parameters to ensure that the particles are different only in size and are stable before and after injection. PMID:21182941

  19. Preparation of solid lipid nanoparticles from W/O/W emulsions: preliminary studies on insulin encapsulation.

    PubMed

    Gallarate, Marina; Trotta, Michele; Battaglia, Luigi; Chirio, Daniela

    2009-08-01

    A method to produce solid lipid nanoparticles (SLN) from W/O/W multiple emulsions was developed applying the solvent-in-water emulsion-diffusion technique. Insulin was chosen as hydrophilic peptide drug to be dissolved in the acidic inner aqueous phase of multiple emulsions and to be consequently carried in SLN. Several partially water-miscible solvents with low toxicity were screened in order to optimize emulsions and SLN composition, after assessing that insulin did not undergo any chemical modification in the presence of the different solvents and under the production process conditions. SLN of spherical shape and with mean diameters in the 600-1200 nm range were obtained by simple water dilution of the W/O/W emulsion. Best results, in terms of SLN mean diameter and encapsulation efficiencies, were obtained using glyceryl monostearate as lipid matrix, butyl lactate as a solvent, and soy lecithin and Pluronic F68 as surfactants. Encapsulation efficiencies up to 40% of the loaded amount were obtained, owing to the actual multiplicity of the system; the use of multiple emulsion-derived SLN can be considered a useful strategy to encapsulate a hydrophilic drug in a lipid matrix.

  20. Solid lipid nanoparticles formed by solvent-in-water emulsion-diffusion technique: development and influence on insulin stability.

    PubMed

    Battaglia, Luigi; Trotta, Michele; Gallarate, Marina; Carlotti, M Eugenia; Zara, Gian Paolo; Bargoni, Alessandro

    2007-11-01

    Insulin-loaded solid lipid nanoparticles (SLN), obtained by the solvent-in-water emulsion-diffusion technique, were produced using isovaleric acid (IVA) as organic phase, glyceryl mono-stearate (GMS) as lipid, soy lecithin and sodium taurodeoxycholate (TDC) as emulsifiers. IVA, a partially water-miscible solvent with low toxicity, was used to dissolve both insulin and lipids. SLN of spherical shape were obtained by simple water dilution of the O/W emulsion. Analysis of SLN content after processing showed interesting encapsulation efficiency with respect to therapeutic doses; moreover, insulin did not undergo any chemical modification within the nanoparticles and most of it remained stable after incubation of the SLN with trypsin solution. The biological activity of insulin, i.e. the ability to decrease glycemia in rats, was not negatively influenced by the SLN production process, as after subcutaneous administration of insulin extracted from SLN to animals, the blood glucose levels were quite similar to those obtained after administration of a conventional insulin suspension. Consequently, SLN seem to have interesting possibilities as delivery systems for oral administration of insulin.