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Chromatographic Analysis (chromatographic + analysis)
Kinds of Chromatographic Analysis Selected AbstractsMetabolism of fluoranthene in different plant cell cultures and intact plantsENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 5 2000Marit Kolb Abstract The metabolism of fluoranthene was investigated in 11 cell cultures of different plant species using a [14C]-labeled standard. Most species metabolized less than 5% of fluoranthene to soluble metabolites and formed less than 5% nonextractable residues during the standardized 48-h test procedure. Higher metabolic rates were observed in lettuce (Lactuca sativa, 6%), wheat (Tricitum aestivum, 9%), and tomato (Lycopersicon esculentum, 15%). A special high metabolic rate of nearly 50% was determined for the rose species Paul's Scarlet. Chromatographic analysis of metabolites extracted from aseptically grown tomato plants proved that the metabolites detected in the cell cultures were also formed in the intact plants. Metabolites produced in tomato and rose cells from [14C]-fluoranthene were conjugated with glucose, glucuronic acid, and other cell components. After acid hydrolyses, the main metabolite of both species was 1-hydroxyfluoranthene as identified by gas chromatography,mass spectrometry and high-performance liquid chromatography with diode array detection. The second metabolite formed by both species was 8-hydroxy-fluoranthene. A third metabolite in tomatoes was 3-hydroxyfluoranthene. [source] Effect of stationary phase polarity on the retention of ionic liquid cations in reversed phase liquid chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 17 2006Sylwia Kowalska Abstract Chromatographic analysis of ionic liquids on different types of packings offers interesting possibility to determine their retention mechanism. As a consequence, the major interactions between stationary phase ligands and analyzed chemical entities can be defined. The main aim of this work was to analyze cations of ionic liquids on chemically bonded stationary phases with specific structural properties. The attempt to predict the main interactions between positive ions of ionic liquids and stationary phase ligands was undertaken. For that purpose, butyl, octyl, octadecyl, phenyl, aryl, mixed, alkylamide, and cholesterolic packings were chosen and applied to the analysis of six most commonly used ionic liquids' cations. Obtained results indicate mainly dispersive and ,,, type of interaction part in the retention mechanism of analyzed compounds. [source] Disruption of Maternal Behavior by Alcohol Intoxication in the Lactating Rat: A Behavioral and Metabolic AnalysisALCOHOLISM, Issue 8 2002Marta Yanina Pepino Background Preweanling rats exhibit clear behavioral signs of distress after interacting with an alcohol-intoxicated dam. Interestingly, behavioral reactivity of infants to the experience of alcohol in the nursing context decreases as a function of repeated alcohol administrations to the mother. In this study, maternal activities were examined when dams were exposed to repeated administrations of a subnarcoleptic alcohol dose. Maternal changes in alcohol metabolism were also analyzed as a function of repeated exposures to the drug. Methods During postpartum days 3, 5, 7, 9, 11, and 13, nursing dams received an intragastric administration of either 2.5 g/kg of alcohol or water. Maternal behaviors were evaluated (experiment 1). Blood alcohol levels (BALs) of the dams were determined on postpartum day 16 after all mothers received either an intragastric (experiment 2) or an intraperitoneal (experiment 3) dose of alcohol. The doses used (2.5 g/kg intragastrically and 1.5 g/kg intraperitoneally) were chosen because they promote similar peak BALs in dams naive to alcohol. Results Maternal behaviors were strongly affected by the state of intoxication. Nevertheless, these disruptions clearly subsided with progression of alcohol-related experiences (experiment 1). Chromatographic analysis of alcohol metabolism indicated the development of tolerance in dams that had prior experience with alcohol (experiment 2). Changes in BALs as a function of prior experience with alcohol seemed related to first-pass alcohol metabolism rather than hepatic oxidative processes of the drug (experiments 2 and 3). Conclusions When the dam first experiences a moderate state of alcohol intoxication, maternal behaviors are uniformly disrupted. Subsequent exposures to alcohol lead to maternal metabolic tolerance. In conjunction with previous studies, these data indicate that infantile reactivity to alcohol is dependent on how the members of the dam/pup dyad express or perceive ethanol's postabsorptive effects. [source] Chromatographic analysis of simple phenols in some species from the genus SalixPHYTOCHEMICAL ANALYSIS, Issue 5 2010Loretta Pob, ocka-Olech Abstract Introduction , Salicis Cortex, made from willow bark is a herbal remedy, which is standardised based on the content of salicin, a compound with analgesic and antiphlogistic properties. However, clinical trials suggest that other compounds also present in Salicis Cortex can contribute to the pharmacological effects. Objective , To characterise the composition of phenolic acids in the barks of different species and clones from the genus Salix by use of chromatographic methods,HPTLC and HPLC. Methodology , The phenolic acid composition was analysed by MGD (multiple gradient development),HPTLC technique. The separation was performed on HPTLC Diol plates with gradient elution using a mixture of chloroform:hexane:ethyl acetate with increasing concentration of ethyl acetate from 10 to 25%. Derivatisation with thymol reagent was employed for the first time for specific detection of phenolic acids containing methoxyl groups. Results , The presence of all phenolic acids previously reported in the genus Salix was confirmed, namely p -hydroxybenzoic, vanillic, cinnamic, p -coumaric, ferulic and caffeic acids. Furthermore, pyrocatechol as a constituent of willow bark was revealed. The highest concentration of this compound was observed in the S. purpurea bark (2.25,mg/g). Conclusion , The presence of a relatively high content of pyrocatechol in Salix species may raise doubts about the safe application of this herbal medicine. Copyright © 2010 John Wiley & Sons, Ltd. [source] Kinetics and products of the reactions of selected diols with the OH radicalINTERNATIONAL JOURNAL OF CHEMICAL KINETICS, Issue 5 2001Heidi L. Bethel Using a relative rate method, rate constants have been measured at 296 ± 2 K for the gas-phase reactions of OH radicals with 1,2-butanediol, 2,3-butanediol, 1,3-butanediol, and 2-methyl-2,4-pentanediol, with rate constants (in units of 10,12 cm3 molecule,1 s,1) of 27.0 ± 5.6, 23.6 ± 6.3, 33.2 ± 6.8, and 27.7 ± 6.1, respectively, where the error limits include the estimated overall uncertainty of ±20% in the rate constant for the reference compound. Gas chromatographic analyses showed the formation of 1-hydroxy-2-butanone from 1,2-butanediol, 3-hydroxy-2-butanone from 2,3-butanediol, 1-hydroxy-3-butanone from 1,3-butanediol, and 4-hydroxy-4-methyl-2-pentanone from 2-methyl-2,4-pentanediol, with formation yields of 0.66 ± 0.11, 0.89 ± 0.09, 0.50 ± 0.09, and 0.47 ± 0.09, respectively, where the indicated errors are the estimated overall uncertainties. Pathways for the formation of these products are presented, together with a comparison of the measured and estimated rate constants and product yields. © 2001 John Wiley & Sons, Inc. Int J Chem Kinet 33: 310,316, 2001 [source] Characterization of extracellular polymers synthesized by tropical intertidal biofilm bacteriaJOURNAL OF APPLIED MICROBIOLOGY, Issue 1 2007B.O. Ortega-Morales Abstract Aim:, This study was performed to determine the potential of tropical intertidal biofilm bacteria as a source of novel exopolymers (EPS). Methods and Results:, A screening procedure was implemented to detect EPS-producing biofilm bacteria. Isolates MC3B-10 and MC6B-22, identified respectively as a Microbacterium species and Bacillus species by 16S rDNA and cellular fatty acids analyses, produced different EPS, as evidenced by colorimetric and gas chromatographic analyses. The polymer produced by isolate MC3B-10 displays significant surfactant activity, and may chelate calcium as evidenced by spectroscopic analysis. Conclusions:, Polymer MC3B-10 appears to be a glycoprotein, while EPS MC6B-22 seems to be a true polysaccharide dominated by neutral sugars but with significant concentrations of uronic acids and hexosamines. EPS MC3B-10 possesses a higher surfactant activity than that of commercial surfactants, and given its anionic nature, may chelate cations thus proving useful in bioremediation. The chemical composition of polymer MC6B-22 suggests its potential biomedical application in tissue regeneration. Significance and Impact of the Study:, This is the first report of a Microbacterium species producing EPS with surfactant properties, which expands our knowledge of the micro-organisms capable of producing these biomolecules. Furthermore, this work shows that tropical intertidal environments are a nonpreviously recognized habitat for bioprospecting EPS-producing bacteria, and that these molecules might be involved in ecological roles protecting the cells against dessication. [source] Antibacterial factors in skin mucus of rabbitfishesJOURNAL OF FISH BIOLOGY, Issue 6 2001Y. Nagashima Aqueous extracts from the skin mucus of two species of rabbitfishes Siganus fuscescens and S. guttatus showed antibacterial activity against gram-negative bacteria. Stability tests and chromatographic analyses suggested that the S. fuscescens antibacterial factor is an acidic glycoprotein with a molecular mass of 400 kDa. [source] Enlarging the library of poly-(L -lysine citramide) polyelectrolytic drug carriersJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 20 2001Anne-Claude Couffin-Hoarau Abstract Poly-(L -lysine citramide) is a degradable drug carrier of the polyelectrolyte type that is composed of citric acid and L -lysine building blocks. In a previous work, poly-(L -lysine citramide) was synthesized by the interfacial polycondensation of ,-hydroxy acid protected citryl dichloride with COOH-protected lysine diamine. Because of head-to-head and head-to-tail and tail-to-tail linkages in the chains as well as various side reactions such as deprotection of the ,-hydroxy acid moieties and intramolecular imide ring formation, a very large family of degradable polyelectrolyte copolymers was obtained. All the members of this family hydrolytically degrade to the same end products. In this study, another route was explored based on the polycondensation of ,-hydroxy acid protected citric acid pentafluorophenyl diesters, namely, citrobenzal dipentafluorophenyl and citrochloral dipentafluorophenyl with N - N,-trimethylsilylated COOH-protected L -lysine. The resulting polymers were characterized by IR, NMR, and size exclusion chromatographic analyses. The resulting chain structures and repeat units were identified from these characterizations and are discussed as compared with characteristics exhibited by analogous polymers resulting from interfacial polycondensation. Differences observed at the intermediate stage involving protected polymers were largely erased during the final deprotection stage because of imide formation during final hydrolysis under the selected conditions. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 3475,3484, 2001 [source] The influence of malolactic fermentation and Oenococcus oeni strain on glycosidic aroma precursors and related volatile compounds of red wineJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 14 2006Maurizio Ugliano Abstract Free and glycosidically bound volatile compounds of red wine were measured after malolactic fermentation (MLF) with four different commercial starter cultures of Oenococcus oeni. MLF resulted in a significant decrease in the concentration of total glycosides, expressed as phenol-free glycosyl glucose. Gas chromatographic analyses of wine enzyme hydrolysates showed that the extent of hydrolysis of glycosides during MLF was dependent on both bacterial strain and chemical structure of the substrate. The highest decrease was observed for glycosidic precursors of primary terpene alcohols. Glycoside-related aroma compounds such as linalool, farnesol, and ,-damascenone were increased after MLF with all the bacterial strains tested. Two of the strains were also able to release significant amounts of vinylphenols during MLF. Copyright © 2006 Society of Chemical Industry [source] Determination of community structure through deconvolution of PLFA-FAME signature of mixed populationBIOTECHNOLOGY & BIOENGINEERING, Issue 3 2007Dipesh K. Dey Abstract Phospholipid fatty acids (PLFAs) as biomarkers are well established in the literature. A general method based on least square approximation (LSA) was developed for the estimation of community structure from the PLFA signature of a mixed population where biomarker PLFA signatures of the component species were known. Fatty acid methyl ester (FAME) standards were used as species analogs and mixture of the standards as representative of the mixed population. The PLFA/FAME signatures were analyzed by gas chromatographic separation, followed by detection in flame ionization detector (GC-FID). The PLFAs in the signature were quantified as relative weight percent of the total PLFA. The PLFA signatures were analyzed by the models to predict community structure of the mixture. The LSA model results were compared with the existing "functional group" approach. Both successfully predicted community structure of mixed population containing completely unrelated species with uncommon PLFAs. For slightest intersection in PLFA signatures of component species, the LSA model produced better results. This was mainly due to inability of the "functional group" approach to distinguish the relative amounts of the common PLFA coming from more than one species. The performance of the LSA model was influenced by errors in the chromatographic analyses. Suppression (or enhancement) of a component's PLFA signature in chromatographic analysis of the mixture, led to underestimation (or overestimation) of the component's proportion in the mixture by the model. In mixtures of closely related species with common PLFAs, the errors in the common components were adjusted across the species by the model. Biotechnol. Bioeng. 2007;96: 409,420. © 2006 Wiley Periodicals, Inc. [source] The role of ,-acidic and ,-basic chiral stationary phases in the high-performance liquid chromatographic enantioseparation of unusual ,-amino acidsCHIRALITY, Issue 3 2009István Ilisz Abstract The application of 3,5-dimethylphenyl-carbamoylated-,-cyclodextrin (Cyclobond I 2000 DMP) and 2,6-dinitro-4-trifluoromethylphenyl-ether-,-cyclodextrin-based (Cyclobond DNP) chiral stationary phases for the high-performance liquid chromatographic enantioseparation of unusual ,-amino acids is reported. The investigated amino acids were saturated or unsaturated alicyclic ,-3-homo-amino acids and bicyclic ,-amino acids. Prior to chromatographic analyses, all amino acids were transformed to N- 3,5-dinitrobenzoyl- or N -3,5-dimethylbenzoyl form to ensure a ,-acidic or ,-basic function and to enhance the ,-acidic-,-basic interactions between analytes and chiral selectors. Chromatographic results are given as retention, separation and resolution factors. The chromatographic conditions were varied to achieve optimal separation. The sequence of elution of the enantiomers was determined in some cases. Chirality, 2009. © 2008 Wiley-Liss, Inc. [source] Linear retention indices in gas chromatographic analysis: a reviewFLAVOUR AND FRAGRANCE JOURNAL, Issue 5 2008Barbara d'Acampora Zellner Abstract The main purpose of any chromatographic analysis is to resolve mixtures of compounds into less complex mixtures or ultimately into pure components. In addition to this function, the chromatographic system can provide retention data which serve as complementary information for the positive identification of resolved components. The need to express gas chromatographic retention data in a standardized system has long been recognized and retention index values presented to be a valuable parameter. Those values are mainly calculated by applying the equations proposed by Kováts, for isothermal analysis, and van den Dool and Kratz, for programmed gas chromatographic runs. In general, these indices denote the retention behaviour of the compounds of interest according to a uniform scale determined by a series of closely related standard substances. The use of retention indices in the flavour and fragrance field is well-documented, and they are widely applied for the comparison of results between laboratories, as well as to characterize stationary phases. Copyright © 2008 John Wiley & Sons, Ltd. [source] Bacterial synthesis of poly(hydroxybutyrate- co-hydroxyvalerate) using carbohydrate-rich mahua (Madhuca sp.) flowersJOURNAL OF APPLIED MICROBIOLOGY, Issue 1 2007P.K. Anil Kumar Abstract Aims:, The objective of the present work was to utilize an unrefined natural substrate namely mahua (Madhuca sp.) flowers, as a carbon source for the production of bacterial polyhydroxyalkanoate (PHA) copolymer by Bacillus sp-256. Methods and Results:, In the present work, three bacterial strains were tested for PHA production on mahua flower extract (to impart 20 g l,1 sugar) amongst which, Bacillus sp-256 produced higher concentration of PHA in its biomass (51%) compared with Rhizobium meliloti (31%) or Sphingomonas sp (22%). Biosynthesis of poly(hydroxybutyrate-co-hydroxyvalerate) , P(HB-co-HV) , of 90 : 10 mol% by Bacillus sp-256 was observed by gas chromatographic analysis of the polymer. Major component of the flower is sugars (57% on dry weight basis) and additionally it also contains proteins, vitamins, organic acids and essential oils. The bacterium utilized malic acid present in the substrate as a co-carbon source for the copolymer production. The flowers could be used in the form of aqueous extract or as whole flowers. PHA content of biomass (%) and yield (g l,1) in a 3·0-l stirred tank fermentor after 30 h of fermentation under constant pH (7) and dissolved oxygen content (40%) were 54% and 2·7 g l,1, respectively. Corresponding yields for control fermentation with sucrose as carbon source were 52% and 2·5 g l,1. The polymer was characterized by proton NMR. Conclusions:, Utilization of mahua flowers, a natural substrate for bacterial fermentation aimed at PHA production, had additional advantage, as the sugars and organic acids present in the flowers were metabolized by Bacillus sp-256 to synthesize P(HB-co-HV) copolymer. Significance and Impact of the Study:, Literature reports on utilization of suitable cheaper natural substrate for PHA copolymer production is scanty. Mahua flowers used in the present experiment is a cheaper carbon substrate compared with several commercial substrates and it is rich in main carbon as well as co-carbon sources that can be utilized by bacteria for PHA copolymer production. [source] Synthesis of 2-phenyl-3-hydroxyethanyl-1,3-oxazolidine and its application as latent curing agentsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2007Jun Gao Abstract A kind of new compound of 2-phenyl-3-hydroxyethanyl-1,3-oxazolidine was successfully synthesized by addition,condensation reaction of phenyl aldehyde and ,-hydroxylethanolamine and purified by vacuum distillation. Its purity was examined by gas chromatographic analysis. Its structure was confirmed by 13C NMR and FTIR. When this compound was added as a latent curing agent in single-component moisture-curable polyurethane system (SPU), bubbles of SPU formed during curing was obviously restrained, and the elongation at break of the cured SPU contained a certain content of 2-phenyl-3-hydroxyethanyl-1,3-oxazolidine was increased to 16 times when compared with that uncontained this oxazolidine derivative. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Hard-modelled trilinear decomposition (HTD) for an enhanced kinetic multicomponent analysisJOURNAL OF CHEMOMETRICS, Issue 5 2002Yorck-Michael Neuhold Abstract We present a novel approach for kinetic, spectral and chromatographic resolution of trilinear data sets acquired from slow chemical reaction processes via repeated chromatographic analysis with diode array detection. The method is based on fitting rate constants of distinct chemical model reactions (hard-modelled, integrated rate laws) by a Newton,Gauss,Levenberg/Marquardt (NGL/M) optimization in combination with principal component analysis (PCA) and/or evolving factor analysis (EFA), both known as powerful methods from bilinear data analysis. We call our method hard-modelled trilinear decomposition (HTD). Compared with classical bilinear hard-modelled kinetic data analysis, the additional chromatographic resolution leads to two major advantages: (1) the differentiation of indistinguishable rate laws, as they can occur in consecutive first-order reactions; and (2) the circumvention of many problems due to rank deficiencies in the kinetic concentration profiles. In this paper we present the theoretical background of the algorithm and discuss selected chemical rate laws. Copyright © 2002 John Wiley & Sons, Ltd. [source] Platelets are mitogenic for periosteum-derived cellsJOURNAL OF ORTHOPAEDIC RESEARCH, Issue 5 2003Reinhard Gruber Abstract The early stages of bone regeneration are associated with a high mitogenic activity of periosteal cells. Here we addressed the question of whether platelets that accumulate within the developing haematoma can account for this tissue response. Addition of platelets, platelet-released supernatants, platelet membranes, and microparticles to bovine periosteum-derived cells resulted in an increase in 3H-thymidine incorporation; lipid extracts had no effect. Platelet-released supernatants retained their activity after incubation at 56°C, but not at 100°C. Gel chromatographic analysis revealed the highest mitogenic activity at approximately 35 kD. Of the factors released from activated platelets, basic fibroblast growth factor (bFGF) and platelet-derived growth factor (PDGF) increased 3H-thymidine incorporation. The mitogenic activity of platelet-released supernatants was decreased by anti-PDGF, and anti-bFGF antibodies. Platelet-released supernatants increased the number of proliferating periosteum-derived cells as determined by the expression pattern of Ki67. Platelet-released supernatants also resulted in a stimulation of cell proliferation in periosteal explants. These results suggest that platelets have the potential to stimulate the mitogenic response of the periosteum during bone repair. © 2003 Orthopaedic Research Society. Published by Elsevier Science Ltd. All rights reserved. [source] Mechanistic studies of intramolecular CH insertion reaction of arylnitrenes: isotope effect, configurational purity and radical clock studiesJOURNAL OF PHYSICAL ORGANIC CHEMISTRY, Issue 1 2005Shigeru Murata Abstract In order to reveal the mechanism of the intramolecular CH insertion of arylnitrenes, three experiments were carried out: measurement of isotope effects, determination of the extent of configurational retention and radical clock studies. Irradiation of the deuterium-substituted azide 4 - d in an inert solvent exclusively afforded the indolines 5 - h and 5 - d, in which the kinetic isotope effect kH/kD on the intramolecular CH insertion of the nitrene was evaluated as 12.6,14.7 at room temperature. A chiral chromatographic analysis of the indoline 11 obtained from the optically active azide (S)- 6 revealed that the enantiomeric purity of the starting azide was almost completely lost during the intramolecular CH insertion of the photolytically generated nitrene (enantiomeric excess <10%). The thermolysis of the azide 7 at 180°C mainly gave a mixture of the cyclopropyl ring-opened products 20,22, together with the intramolecular CH insertion product with an intact cyclopropyl ring 19. On the basis of these observations, we concluded that the intramolecular CH insertion of the nitrene proceeds primarily by the hydrogen abstraction,recombination mechanism. We propose, however, a small contribution of the concerted mechanism to the intramolecular CH insertion, based on the solvent dependence of the isotope effect and the extent of the configurational retention. Copyright © 2004 John Wiley & Sons, Ltd. [source] Sol,gel microextraction phases for sample preconcentration in chromatographic analysisJOURNAL OF SEPARATION SCIENCE, JSS, Issue 19 2010Scott S. Segro Abstract Sol,gel technology provides a simple and reliable method for solid-phase microextraction (SPME) fiber preparation through in situ creation of surface-bonded organic,inorganic hybrid coatings characterized by enhanced thermal stability and solvent-resistance properties that are important for the coupling of SPME with GC and HPLC, respectively. The sol,gel coating technology has led to the development of an extensive array of sol,gel sorbent coatings for SPME. In this article, sol,gel microextraction coatings are reviewed, with particular attention on their synthesis, characterization, and applications in conjunction with GC and HPLC analyses. In addition, the development of sol,gel-coated stir bars, their inherent advantages, and applications are discussed. Next, the development and applications of sol,gel capillary microextraction (CME) in hyphenation with GC and HPLC is extensively reviewed. The newly emerging germania- and titania-based sol,gel microextraction phases look promising, especially in terms of pH and hot solvent stability. Finally, sol,gel monolithic beds for CME are reviewed. Such monolithic beds are in a position to greatly improve the extracting capabilities and enhanced sensitivity in CME. [source] Solid phase microextraction-high performance liquid chromatographic determination of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in the presence of sodium dodecyl sulfate surfactantJOURNAL OF SEPARATION SCIENCE, JSS, Issue 12 2008Gaurav Abstract A simple and sensitive method has been developed using preconcentration technique solid phase microextraction (SPME) and analytical technique HPLC-UV for the determination of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) from the environmental samples. Aqueous solution of anionic surfactant SDS was used for the extraction of both nitramine high explosives, viz., HMX and RDX from soil samples which were subsequently sorbed on SPME fiber. The static desorption was carried out in the desorption chamber of the SPME-HPLC interface in the presence of mobile phase ACN/methanol/water (30:35:35) and the subsequent chromatographic analysis at a flow rate of 0.5 mL/min and detection at 230 nm. For this purpose, a C18, 5 ,m RP analytical column was used as a separation medium in this method. Several parameters relating to SPME, e.g., adsorption/desorption time, concentration of salt, stirring rate, etc., were optimized. The method was linear over the range of 20,400 ng/mL for HMX and RDX standards in the presence of surfactant in aqueous phase, respectively. The correlation coefficient (R2) for HMX and RDX are 0.9998 and 0.9982, respectively. With SPME, the detection limits (S/N = 3) in ng/mL are 0.05 and 0.1 for HMX and RDX, respectively in the presence of the SDS surfactant. The developed method has been applied successfully to the analysis of real environmental samples like bore well water, river water, and ground alluvial soil. [source] Sampling flower scent for chromatographic analysisJOURNAL OF SEPARATION SCIENCE, JSS, Issue 11 2008Elena E. Stashenko Abstract The analysis of flower volatiles requires special methods for their isolation with enrichment. Living flowers show a continuous change in their volatile profile that depends on intrinsic (genetic) and external (light, temperature, hydric stress) factors. Excised flowers suffer rapid deterioration and loss of volatiles. While industrial isolation methods for flower volatiles are well established, those at the laboratory-scale experience progressive development, in the search for higher sensitivity, reproducibility, and simplicity. This review covers the flower scent sampling methods most commonly employed during the last decade, and includes comments on their strengths and limitations. The strengths of headspace solid-phase microextraction (HS-SPME) for in vivo monitoring are emphasized with the examples of monitoring the circadian variation of Brugmansia suaveolens flower scent and of volatile aldehyde detection in flower scent using on-fiber derivatization. [source] A novel solid phase for selective separation of flavonoid compoundsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2007Yong-qing Xia Abstract A novel straightforward approach to selective separation for flavonoid compounds was reported. The solid phase material was prepared by copolymerization using allyl-bromide-modified chitosan as macromonomer, and ethylene glycol dimethacrylate as cross-linker. The material was evaluated by chromatographic analysis; it exhibited high selectivity separation for quercetin and its structural analogues using different mobile phases. The material could directly trap a specific class of compounds including quercetin and kaempferol from the hydrolyzate of Ginkgo biloba extract. These results demonstrated the possibility of direct extraction of certain constituents from herb using this material. [source] HPLC-DAD in identification and quantification of selected coumarins in crude extracts from plant cultures of Ammi majus and Ruta graveolensJOURNAL OF SEPARATION SCIENCE, JSS, Issue 14 2003Marian Kami Abstract This paper describes a method for the separation and determination of selected coumarins and furanocoumarins in the crude extracts from plant tissue cultures of Ammi majus hairy roots and Ruta graveolens cell suspensions, cultured in vitro, separately or together as co-cultures. The usefulness of the three main components of the eluent used in reversed-phase high performance liquid chromatographic analysis, namely: methanol (MeOH), acetonitrile (ACN), and tetrahydrofuran (THF), and different elution programs, was assessed. In the optimal analytical method a Lichrospher® RP-18e 5-,m column, a THF-MeOH elution gradient, and a UV/VIS DAD detector were used. Due to the presence of many different compounds in the investigated plant extracts, the use of a UV/VIS DAD detector was essential. Coumarins were identified by comparison of their UV spectra with those of the analytical standards, and characterization of peak purity. [source] Extraction of pure lycopene from industrial tomato by-products in water using a new high-pressure processJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 14 2008Daniele Naviglio Abstract BACKGROUND: Lycopene, a precursor of ,-carotene with a well-known antioxidant activity, contained in many natural products such as tomato (Lycopersicon esculentum Mill.), watermelon, red pepper and papaya, is usually recovered from natural vegetal sources using organic solvents and a purification step. In this paper an innovative process for the extraction of pure lycopene from tomato waste in water that uses the Naviglio® extractor and water as extracting phase is presented. RESULTS: Lycopene was obtained in the all- trans form at a very high grade of purity, not less than 98% (w/w), with an average recovery of 14% (w/w). The availability of high-purity trans -lycopene allowed measurement of the molar absorption coefficient. An alternative procedure for high-performance liquid chromatographic analysis using a phenyl-hexyl silicone phase as inverse phase and a linear gradient in water and acetonitrile is also described. CONCLUSIONS: The use of water as extracting phase considerably reduces the cost of the entire process when compared with the commonly used solvent-based procedure or with the newer supercritical extraction process of lycopene from tomato waste. Lycopene, not soluble in water, was recovered in a quasi-crystalline solid form and purified by solid-phase extraction using a small amount of organic solvent. Copyright © 2008 Society of Chemical Industry This article was published online on September 15, 2008. Errors in Figures 2 - 4 were subsequently identified. The publishers wish to apologise for these errors. This notice is included in the online and print versions to indicate that both have been corrected [September 19, 2008] [source] Analysis of pesticide residues by online reversed-phase liquid chromatography,gas chromatography in the oil from olives grown in an experimental plot.JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 12 2006Part II Abstract The effect of the pesticide dose used to control pests in olive trees and the date of treatment on the residues present in the oil were studied for four organophosphorus pesticides (diazinon, malathion, trichlorphon and chlorfenvinphos) and one organochlorine (endosulfan). Pesticide residue analysis was performed using online reversed-phase liquid chromatography,gas chromatography, using an automated through oven transfer adsorption desorption interface and selective detectors, such as nitrogen,phosphorus detector and electronic capture detector. A simple filtration step was necessary before the chromatographic analysis of samples. The obtained data were statistically analyzed and conclusions about olive pesticide treatments are presented. Copyright © 2006 Society of Chemical Industry [source] Time of flight mass spectrometry applied to the liquid chromatographic analysis of pesticides in water and foodMASS SPECTROMETRY REVIEWS, Issue 6 2006Sílvia Lacorte Abstract Liquid chromatography coupled to mass spectrometry (LC-MS) is an excellent technique to determine trace levels of polar and thermolabile pesticides and their degradation products in complex matrices. LC-MS can be equipped with several mass analyzers, each of which provides unique features capable to identify, quantify, and resolve ambiguities by selecting appropriate ionization and acquisition parameters. We discuss in this review the use of LC coupled to (quadrupole) time-of-flight mass spectrometry (LC-(Q)ToF-MS) to determine the presence of target and non-target pesticides in water and food. This technique is characterized by operating at a resolving power of 10,000 or more. Therefore, it gives accurate masses for both parent and fragment ions and enables the measurement of the elemental formula of a compound achieving compound identification. In addition, the combination of quadrupole-ToF permits tandem mass spectrometry, provides more structural information, and enhances selectivity. The purpose of this article is to provide an overview on the state of art and applicability of liquid chromatography time-of-flight mass spectrometry (LC-ToF-MS), and liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QToF-MS) for the analysis of pesticides in environmental matrices and food. The performance of such techniques is depicted in terms of accurate mass measurement, fragmentation, and selectivity. The final section is devoted to describing the applicability of LC-(Q)ToF-MS to routine analysis of pesticides in food matrices, indicating those operational conditions and criteria used to screen, quantify, and identify target and "suspected" pesticides and their degradation products in water, fruits, and vegetables. The potential and future trends as well as limitations of LC-(Q)ToF-MS for pesticide monitoring are highlighted. © 2006 Wiley Periodicals, Inc. [source] Photosensitized DNA Damage: The Case of Fluoroquinolones,PHOTOCHEMISTRY & PHOTOBIOLOGY, Issue 4 2009Virginie Lhiaubet-Vallet This review focuses on DNA damage photosensitized by the fluoroquinolone (FQ) antibacterial drugs. The in vivo evidence for photocarcinogenesis mediated by FQs is presented in the introduction. The different methods employed for detection of DNA-photodamage mediated by FQs are then summarized, including gel electrophoresis (with whole cells, with isolated DNA and with oligonucleotides) and chromatographic analysis (especially HPLC with electrochemical and MS/MS detection). The chemical mechanisms involved in the formation of the reported lesions are discussed on the basis of product studies and transient spectroscopic evidence. In general, the literature coverage is limited to the last decade, although some earlier citations are also included. [source] Gas chromatographic analysis of dimethyltryptamine and , -carboline alkaloids in ayahuasca, an amazonian psychoactive plant beveragePHYTOCHEMICAL ANALYSIS, Issue 2 2009Ana Paula Salum Pires Abstract Introduction Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N -dimethyltryptamine, whereas B. caapi contains substantial amounts of , -carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. Objective To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main , -carbolines found in ayahuasca preparations. Methodology The alkaloids were extracted by means of solid phase extraction (C18) and detected by gas chromatography with nitrogen/phosphorous detector. Results The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02,4.0 mg/mL (r2 > 0.99). The method was also precise (RSD < 10%). Conclusion A simple gas chromatographic method to determine the main alkaloids found in ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright © 2009 John Wiley & Sons, Ltd. [source] High-performance thin layer chromatographic analysis of anti-inflammatory triterpenoids from Boswellia serrata Roxb.PHYTOCHEMICAL ANALYSIS, Issue 6 2001K. Krohn Abstract A rapid and simple high-performance thin layer chromatographic (HPTLC) method was developed for the simultaneous quantitative estimation of the biologically active triterpenoids ,-boswellic acid, 3- O -acetyl-,-boswellic acid, 11-keto-,-boswellic acid and 3- O -acetyl-11-keto-,-boswellic acid from the gum resin of Boswellia serrata. The assay combines the isolation and separation of boswellic acid derivatives on silica gel 60F254 -HPTLC plates with spot visualisation and scanning at 250,nm. Methanol was found to be the most appropriate solvent for the exhaustive extraction of boswellic acid derivatives. Copyright © 2001 John Wiley & Sons, Ltd. [source] Micro-high-performance liquid chromatography/Fourier transform mass spectrometry with electron-capture dissociation for the analysis of protein enzymatic digestsRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 10 2002Walter Davidson Electron-capture dissociation (ECD) Fourier transform mass spectrometry (FTMS) employed to generate comprehensive sequence information for the chromatographic analysis of enzymatic protein digests is described. A pepsin digest of cytochrome c was separated by reversed-phase micro-high-performance liquid chromatography (µHPLC) and ionized ,on-line' by electrospray ionization (ESI). The ions thus formed were transferred to and trapped in the FTMS analyzer cell. Typically, no precursor ion isolation was performed. The trapped ions were subjected to a pulse of electrons to induce fragmentation. Mass spectra were acquired continuously to produce a three-dimensional LC/MS data set. The spectra were dominated by c and, to a lesser degree, z ions, which provided near complete sequence coverage. External calibration provided good mass accuracy and resolution, typical of FTMS. Thus,µHPLC/ECD,,,FTMS is shown to be a highly informative method for the analysis of enzymatic protein digests. Copyright © 2002 John Wiley & Sons, Ltd. [source] Chromatography of amino acids and short peptides.BIOMEDICAL CHROMATOGRAPHY, Issue 8 2007New advances Abstract The newest results in the application of various chromatographic methods (gas,liquid chromatography, liquid chromatographic techniques, electrically driven systems) for the separation and quantitative determination of amino acids and short peptides in pure state and in complicated matrices are compiled. The results are concisely described and critically evaluated. The future trends of the chromatographic analysis of amino acids and short peptides are briefly discussed. Copyright © 2007 John Wiley & Sons, Ltd. [source] | |||||||||||||||||||